阅读说明：本技术 一种功能聚酯生产系统、生产方法及功能聚酯纤维 (Functional polyester production system, production method and functional polyester fiber ) 是由 邱志成 李鑫 王颖 李志勇 金剑 武术芳 王雪 刘玉来 张凯悦 于 2020-12-23 设计创作，主要内容包括：本发明公开了一种功能聚酯生产系统、生产方法及功能聚酯纤维,所述功能聚酯生产系统的聚酯低聚物连续制备系统包括设置在酯化系统和预缩聚系统之间的精确控制反应单元和混合单元,本发明提供的功能聚酯生产系统,可以连续制备得到功能粉体分散粒径小的功能聚酯低聚物,然后通过功能聚酯低聚物的缩聚反应,可获得功能粉体呈高度均匀分散的功能聚酯,制备得到的功能聚酯压滤值FPFPV不大于0.2bar/g,有利于改善功能聚酯的纺丝性能,适合用于生产高品质纤维和薄膜等产品。(The invention discloses a functional polyester production system, a production method and functional polyester fibers, wherein a polyester oligomer continuous preparation system of the functional polyester production system comprises an accurate control reaction unit and a mixing unit which are arranged between an esterification system and a pre-polycondensation system, the functional polyester production system provided by the invention can continuously prepare functional polyester oligomers with small dispersed particle sizes of functional powder, then functional polyester with highly and uniformly dispersed functional powder can be obtained through the polycondensation reaction of the functional polyester oligomers, the filter pressing value FPFPFPV of the prepared functional polyester is not more than 0.2bar/g, the spinning performance of the functional polyester is favorably improved, and the functional polyester continuous preparation system is suitable for producing products such as high-quality fibers, films and the like.)

1. A functional polyester production system, comprising:

the continuous preparation system comprises an esterification system, a pre-polycondensation system and a final polycondensation system which are connected in sequence, the continuous preparation system for the functional polyester oligomer comprises an accurate control reaction unit and a mixing unit which are arranged between the esterification system and the pre-polycondensation system, an outlet of the esterification system is connected with an inlet of the accurate control reaction unit and an inlet of the mixing unit respectively, and an outlet of the accurate control reaction unit is connected with an inlet of the mixing unit.

2. The functional polyester production system according to claim 1, wherein:

the precise control reaction unit comprises a horizontal reaction kettle, at least two cavities are arranged in the kettle body of the horizontal reaction kettle, and a stirrer and at least two ultrasonic vibrators are arranged in each cavity;

the mixing unit comprises a dynamic mixer.

3. The functional polyester production system according to claim 2, wherein:

the bottom of the horizontal reaction kettle body is provided with at least one partition plate to separate the inner space of the horizontal reaction kettle body into the cavity, and the bottom of the partition plate is provided with a non-return diversion hole for the unidirectional flow of reaction materials.

4. The functional polyester production system according to claim 2 or 3, wherein:

heating devices communicated with the heat medium pipeline are arranged in each cavity of the horizontal reaction kettle, and the heating temperature of the heating devices in each cavity is independently controlled by a flow regulating valve arranged on the heat medium pipeline;

preferably, the heating means comprises a heating medium jacket and a heating coil.

5. A production method for producing a functional polyester using the production system as set forth in any one of claims 1 to 4, comprising the steps of:

s1, carrying out esterification reaction on the raw material of the polyester oligomer to obtain the polyester oligomer;

s2, mixing part of the polyester oligomer prepared in the step S1 with the functional powder slurry, and heating and volatilizing to prepare a functional powder condensation compound;

s3, mixing the residual part of polyester oligomer prepared in the step S1 with the functional powder condensation compound prepared in the step S2 to prepare functional polyester oligomer;

s4, carrying out pre-polycondensation reaction and final polycondensation reaction on the functional polyester oligomer prepared in the step S3 to prepare functional polyester;

the step S2 occurs in the precisely controlled reaction unit of the functional polyester oligomer continuous production system, and the step S3 occurs in the mixing unit of the functional polyester oligomer continuous production system.

6. The process for producing functional polyester according to claim 5, wherein:

in the step S3, the hydroxyl value of the functional powder condensate is controlled to be not higher than 350mgKOH/g, the average particle diameter of the functional powder in the functional powder condensate is not higher than 1000nm, and the content of the functional powder in the functional powder condensate is 4.7-20%.

7. The process for producing a functional polyester according to claim 5, wherein:

the heating temperature of the reaction unit is accurately controlled to be 200-250 ℃;

and in the step S2, ultrasonic treatment is carried out on part of the polyester oligomer and the functional powder slurry, wherein the ultrasonic treatment time is 30-120 min.

8. The process for producing a functional polyester according to claim 5, wherein:

the intrinsic viscosity of the functional polyester prepared in the step S4 is 0.5-1.2 dL/g, and the filter pressing value FPFPV is not more than 0.2 bar/g.

9. A functional polyester fiber spun from a functional polyester produced by the functional polyester production system according to any one of claims 1 to 4 or the functional polyester produced by the functional polyester production method according to any one of claims 5 to 8.

10. The functional polyester fiber according to claim 9, wherein:

the functional polyester fiber has a breaking strength of 2.6-8.4 cN/dtex and an elongation at break of 17-67%.

Technical Field

The invention belongs to the technical field of high polymer material synthesis, and particularly relates to a functional polyester production system, a production method and functional polyester fibers.

Background

At present, the preparation method of functional polyester fiber mainly adopts a master batch method, firstly, functional powder and carrier resin are melted and mixed to obtain functional master batches with high functional powder content, and then, functional master batch melt and polyester melt for spinning are uniformly mixed to obtain the functional polyester fiber through a spinning process. In the process of preparing the functional polyester fiber by the master batch method, the dispersion of the functional powder in the high-viscosity polyester melt is mainly realized by the mechanical shearing force provided by the mixing equipment, so that the high-uniform dispersion of the functional powder in the polyester melt is difficult to realize, the spinning performance of the prepared functional polyester melt is poor, and the fine denier or superfine denier functional polyester fiber is difficult to spin.

The present invention has been made in view of this situation.

Disclosure of Invention

The functional polyester production system provided by the invention can continuously prepare functional polyester oligomer with small dispersed particle size of functional powder and produce functional polyester with highly uniformly dispersed functional powder.

In order to solve the technical problems, the invention adopts the technical scheme that:

a first object of the present invention is to provide a production system of functional polyester, comprising: the continuous preparation system comprises an esterification system, a pre-polycondensation system and a final polycondensation system which are connected in sequence, the continuous preparation system for the functional polyester oligomer comprises an accurate control reaction unit and a mixing unit which are arranged between the esterification system and the pre-polycondensation system, an outlet of the esterification system is connected with an inlet of the accurate control reaction unit and an inlet of the mixing unit respectively, and an outlet of the accurate control reaction unit is connected with an inlet of the mixing unit.

The further scheme of the invention is as follows: the precise control reaction unit comprises a horizontal reaction kettle, at least two cavities are arranged in the kettle body of the horizontal reaction kettle, and a stirrer 3 and at least two ultrasonic vibrators 5 are arranged in each cavity; the mixing unit comprises a dynamic mixer.

In the above scheme, the precise control reaction unit and the mixing unit are added between the existing esterification system and the pre-polycondensation system, the ultrasonic vibration rod is arranged inside the horizontal reaction kettle of the precise control reaction unit, the ultrasonic vibration rod can uniformly generate ultrasonic waves at 360 degrees, and the output of the energy is not influenced by load changes such as liquid level, temperature difference and the like. Ultrasonic waves are generated by ultrasonic vibration rods arranged in each cavity and act on a polyester oligomer melt to initiate a cavitation effect, local high temperature, high pressure, strong shock waves, microjet and the like are generated, the function among functional powder particles can be greatly weakened, the agglomeration of the functional powder particles can be effectively reduced, the deposition of the functional powder in each cavity of a reaction kettle is avoided, and the high uniform dispersion of the functional powder in the polyester oligomer is realized, so that the obtained functional polyester has a highly uniform structure, and is suitable for producing high-quality fibers and film products.

Preferably, the mixing unit comprises a dynamic mixer including, but not limited to, a shear pump, a screw extruder, a planetary gear dynamic mixer, a dynamic mixer of the dynamic and static ring gear type, or a dynamic mixer of the ball and socket type.

In the scheme, the functional powder slurry is efficiently and uniformly mixed in the polyester oligomer in a dynamic mixing mode so as to achieve nearly homogeneous physical blending, and the functional powder slurry is prevented from being directly added into an esterification reaction kettle to cause the coagulation of functional powder due to the high-temperature gasification of ethylene glycol, so that the functional polyester with uniform structure is prepared.

Preferably, the agitator includes, but is not limited to, a flap opening turbine agitator, a flap disk turbine agitator, a propeller agitator, a flap paddle agitator, a triangular reciprocating rotary agitator.

Preferably, the stirrer comprises two stirring blades arranged along the height direction of the reaction kettle body, and the two stirring blades are mutually meshed.

As an embodiment of the invention, the ultrasonic vibrator can adopt an ultrasonic vibration rod, the ultrasonic vibration rod is inserted from the bottom of the horizontal reaction kettle, and the height of the ultrasonic vibration rod is 1/4-1/2 of the height of the kettle body of the horizontal reaction kettle.

As an embodiment of the invention, at least one partition plate 2 is arranged at the bottom of the horizontal reaction kettle body 1 to partition the internal space of the horizontal reaction kettle body into the chambers, and the partition plate is provided with a non-return flow guide hole 4 for the unidirectional flow of the reaction materials.

Preferably, the height of the partition is 1/2-3/4 of the height of the kettle body of the horizontal reaction kettle.

As an embodiment of the present invention, the reaction kettle body is provided with a material inlet 11 and a material outlet 12, the material inlet is located at the lower part or the bottom of one side of the reaction kettle body, and the material outlet is located at the lower part or the bottom of the other side of the reaction kettle body.

After entering the reaction kettle from a material inlet arranged at the lower part or the bottom of one side of the reaction kettle, the material flows through the cavities in sequence through the non-return flow-guiding holes arranged on the partition plate for the unidirectional flow of the reaction material, and finally flows out from a material outlet arranged at the lower part or the bottom of the other side of the reaction kettle. The multi-cavity structure of the horizontal reaction kettle can obviously reduce the back mixing degree of materials and reduce the side reaction of the materials caused by long-time stay in the reaction kettle.

As an embodiment of the invention, each chamber of the horizontal reaction kettle is internally provided with a heating device communicated with a heat medium pipeline, and the heating temperature of the heating device in each chamber is independently controlled by a flow regulating valve arranged on the heat medium pipeline;

preferably, the heating means comprises a heating medium jacket 6 and a heating coil 7.

Specifically, the horizontal reaction kettle is an ultrasonic reaction kettle with a built-in heat medium pipeline, and the heat medium pipeline comprises at least two heat medium inlet pipelines 8 and a heat medium outlet pipeline 9.

Through setting up heat medium jacket and heating coil in each cavity of reation kettle, heat medium jacket and heating coil sharing heat medium inlet line, heat medium outlet line, and heating device's heating temperature is by setting up the flow control valve independent control on different heat medium outlet line in each cavity, make reation kettle possess substep accurate control's function, the opening size through adjusting flow control valve can the independent control heat medium jacket and the heating coil's heating temperature, and then control each cavity material temperature and regulate and control the reaction degree of material stage by stage.

Preferably, the ultrasonic vibration rod is arranged between the heating coil and the partition plate or between the heating coil and the inner wall of the reaction kettle body.

As an embodiment of the invention, each chamber of the reaction kettle is provided with 2 retractable modifier injection distributors 13.

2 telescopic modifier injection distributors are arranged in each cavity of the reaction kettle, so that the reaction kettle has the function of adding modifiers at different reaction stages; and the functional powder slurry is also injected into the precisely controlled reaction unit on line through a modifier injection distributor. Wherein 2 telescopic modifier injection distributors are used for one, one modifier injection distributor extends below the liquid level of the material to work in the operation process of the reaction kettle, and the other modifier injection distributor contracts above the liquid level of the material for standby. Once the material blocks the working modifier injection distributor, the modifier injection distributor can be retracted and detached for dredging, and the spare modifier injection distributor extends below the liquid level of the material for use.

Further, a gas phase outlet 14 is arranged at the top of the reaction kettle body, and a reaction kettle pressure regulating valve 16 is arranged on a gas phase pipeline connecting the gas phase outlet and the steam separation condenser 15.

The second purpose of the invention provides a functional polyester production system, which comprises the following steps:

s1, carrying out esterification reaction on the raw material of the polyester oligomer to obtain the polyester oligomer;

s2, mixing part of the polyester oligomer prepared in the step S1 with the functional powder slurry, and heating and volatilizing to prepare a functional powder condensation compound;

s3, mixing the residual part of polyester oligomer prepared in the step S1 with the functional powder condensation compound prepared in the step S2 to prepare functional polyester oligomer;

s4, carrying out pre-polycondensation reaction and final polycondensation reaction on the functional polyester oligomer prepared in the step S3 to prepare functional polyester;

the step S2 occurs in the precisely controlled reaction unit of the functional polyester oligomer continuous production system, and the step S3 occurs in the mixing unit of the functional polyester oligomer continuous production system.

In the functional polyester production method, functional powder slurry is prepared by grinding functional powder and dihydric alcohol which are used as raw materials in a functional powder slurry preparation system formed by connecting 1-5 grinding machines in series.

The average particle size of the functional powder in the functional powder slurry obtained by continuous preparation can be regulated and controlled by regulating the number of the grinding machines connected in series and the particle size of the grinding medium in the grinding machine.

The dihydric alcohol includes, but is not limited to, ethylene glycol, propylene glycol, butylene glycol, hexylene glycol, methyl propylene glycol, neopentyl glycol, diethylene glycol, or triethylene glycol. The functional powder is powder with functions of coloring, radiation protection, antibiosis, electric conduction, heat conduction, far infrared, flame retardance, negative ion, fluorescence or magnetism, and the functional powder comprises but is not limited to one or more of the following substances: carbon black, pigment brown 3, pigment blue 5, pigment blue 15:1, pigment blue 15:3, pigment blue 15:4, pigment blue 15:6, pigment blue 16, pigment blue 28, pigment blue 29, pigment blue 60, pigment violet 19, pigment violet 23, pigment violet 29, pigment red 101, pigment red 102, pigment red 108, pigment red 112, pigment red 122, pigment red 146, pigment red 149, pigment red 170, pigment red 171, pigment red 172, pigment red 175, pigment red 176, pigment red 177, pigment red 178, pigment red 179, pigment red 185, pigment red 202, pigment red 207, pigment red 208, pigment red 214, pigment red 241, pigment red 242, pigment red 254, pigment red 255, pigment red 263, pigment red 264, pigment red 272, pigment yellow 6, pigment yellow 13, pigment yellow 14, pigment yellow 17, pigment yellow 21, pigment yellow 37, pigment yellow 77, pigment yellow 74, pigment yellow 81, pigment yellow, Pigment yellow 97, pigment yellow 107, pigment yellow 110, pigment yellow 120, pigment yellow 129, pigment yellow 138, pigment yellow 139, pigment yellow 147, pigment yellow 148, pigment yellow 150, pigment yellow 151, pigment yellow 155, pigment yellow 168, pigment yellow 174, pigment yellow 180, pigment yellow 187, pigment yellow 192, pigment yellow 195, pigment yellow 196, pigment yellow 197, pigment orange 34, pigment orange 36, pigment orange 43, pigment orange 61, pigment orange 64, pigment orange 68, pigment orange 70, pigment orange 73, pigment green 5, pigment green 7, pigment green 36, pigment green 50 yellow green luminescent powder (ZnS: Cu), long-lasting phosphor (SrMgAl4O8: Eu2+ Dy 3), sky blue luminescent powder (Sr2MgSi2O7), orange luminescent powder (Y2O2S: Eu.Mg: Ti), yellow green luminescent powder (SrAl2O4: Eu.Dy), blue green luminescent powder (Sr4A14O 5: Eu.5: Eu.Y), orange yellow luminescent powder (Y2O 2: Eu.2: Eu.16: Ge: 64), aerogel luminescent powder (Eu: 64: Eu.M.M.I.I), silica: Eu.I.I.I.I.I.I.I.I.I.I.II), Eu, Eu.II, Silver oxide, silver-loaded zeolite, silver-loaded titanium dioxide, zinc-doped titanium dioxide, copper-doped titanium dioxide, silver-loaded zinc oxide, zinc-doped copper oxide, copper-doped zinc oxide, cuprous oxide, zinc oxide, aluminum oxide, titanium dioxide, silicon dioxide, graphene, carbon nanotubes, aluminum nitride, boron nitride, silicon carbide, graphite, bamboo charcoal, coffee carbon, zirconium carbide, zirconium oxide, titanium carbide, hafnium carbide, tourmaline, opal, bizarite, layered double hydroxide, mica, jade, magnesium hydroxide, zinc borate, ferroferric oxide or tin antimony oxide, indium tin oxide, aluminum-doped zinc oxide.

Preferably, the average particle size of the functional powder in the functional powder slurry is controlled to be not higher than 1000 nm; further preferably, the average particle size of the functional powder in the functional powder slurry is controlled to be not higher than 400 nm; more preferably, the average particle diameter of the functional powder in the functional powder slurry is controlled to be not more than 200 nm.

The average particle size is controlled within the range, so that the functional powder can be highly uniformly dispersed in the functional polyester prepared in the subsequent process.

In the functional polyester production method, one or more of raw materials of terephthalic acid slurry, copolymerization modified monomer slurry and polyester waste for preparing polyester oligomer are mixed, wherein the terephthalic acid slurry is prepared from terephthalic acid and dihydric alcohol according to the molar ratio of 1.05-2.0, the copolymerization modified monomer slurry is composed of a melt of copolymerization modified monomer or a mixture of copolymerization modified monomer and dihydric alcohol, and the polyester waste is polyester bottle waste and production leftovers, polyester film waste and production leftovers, polyester textile waste and production leftovers and/or polyester fiber production leftovers.

The molar ratio of the alcohol acid in the terephthalic acid slurry is controlled to be 1.05-2.0, the terephthalic acid has good pulping property, the terephthalic acid slurry within the range of the molar ratio of the alcohol acid is input into an esterification system, the air lift of the esterification system is within a proper range, the esterification reaction is favorably and stably carried out, the condensation reflux quantity of the ethylene glycol during the esterification reaction is small, and the reaction energy consumption is favorably saved.

Co-modifying monomers include, but are not limited to: isophthalic acid, adipic acid, neopentyl glycol, diethylene glycol, polyethylene glycol, sorbitol, polyamide, polyethylene glycol adipate, diethylene glycol isophthalate-5-sulfonate sodium, diethylene glycol isophthalate-5-sulfonate lithium, diethylene glycol isophthalate-5-sulfonate potassium, diethylene glycol 2-carboxyethylphenylphosphinate, diethylene glycol [ (6-oxo-6H-dibenzo [ c, e ] [1,2] oxyphosphate-6-yl) methyl ] succinate, dipropylene glycol isophthalate-5-sulfonate sodium, dipropylene glycol isophthalate-5-sulfonate lithium, dipropylene glycol isophthalate-5-sulfonate potassium, dipropylene glycol 2-carboxyethylphenylphosphinate, sorbitol, polyamide, polyethylene glycol adipate, diethylene glycol isophthalate-5-sulfonate sodium, dipropylene glycol 2-carboxyethylphenylphosphinate, sorbitol, Dipropylene glycol [ (6-oxo-6H-dibenzo [ c, e ] [1,2] oxaphosphorin-6-yl) methyl ] succinate, dibutylene isophthalate-5-sulfonate sodium, dibutylene isophthalate-5-sulfonate lithium, dibutylene isophthalate-5-sulfonate potassium, dibutylene 2-carboxyethylphenylphosphinate, dibutylene [ (6-oxo-6H-dibenzo [ c, e ] [1,2] oxaphosphorin-6-yl) methyl ] succinate.

In one embodiment of the present invention, in step S3, the hydroxyl value of the functional powder condensate is controlled to be not higher than 350mgKOH/g, the average particle diameter of the functional powder in the functional powder condensate is controlled to be not higher than 1000nm, and the content of the functional powder in the functional powder condensate is controlled to be 4.7% to 20%.

The functional powder content in the functional powder condensation compound is controlled within the range, so that the functional polyester with highly uniformly dispersed functional powder can be prepared; the hydroxyl value of the functional powder condensation compound is controlled within the range, the generation amount of the by-product dihydric alcohol is small in the polycondensation reaction process, and the reduction of the production operation stability caused by the obvious increase of the evaporation amount of the dihydric alcohol when the functional powder condensation compound is injected into an accurately controlled reaction unit is avoided.

As an embodiment of the invention, the heating temperature of the reaction unit is accurately controlled to be 200-250 ℃;

and in the step S2, ultrasonic treatment is carried out on part of the polyester oligomer and the functional powder slurry, wherein the ultrasonic treatment time is 30-120 min.

The ultrasonic wave generated by the ultrasonic vibrating rod generates sound wave cavitation between the polyester oligomer melt and the functional powder to cause the formation, growth and explosion compression of bubbles in the polyester oligomer melt, the reaction temperature of the reaction unit is accurately controlled within the range, and the phenomenon that the vapor pressure of the bubbles in the polyester oligomer melt is increased due to overhigh temperature can be prevented, so that the buffering action force is increased for the bubble explosion process to cause the cavitation to be weakened. The functional polyester condensation compound with more dispersed functional powder can be prepared by utilizing the reaction temperature condition.

Because the precise control reaction unit adopts the combined action of the ultrasonic vibrating bar and the stirrer, the functional powder particles in the functional powder slurry can be dispersed more uniformly in the functional polyester condensation compound; the cavitation of the ultrasonic wave can improve the volatilization speed of the polycondensation byproduct glycol, promote the polycondensation reaction, shorten the reaction time of the functional polyester condensation compound which enables the reaction to reach a specific hydroxyl value, improve the reaction efficiency and reduce the production cost; in addition, the control reaction is carried out according to the conditions, the agglomeration of functional powder particles can be effectively reduced, and the functional polyester with a more uniform structure can be produced by using the functional polyester condensate prepared under the reaction time conditions.

In one embodiment of the present invention, the ultrasonic vibrator has a frequency of 20 to 80kHz and a power of 500 to 3000W.

The ultrasonic wave cavitation that the ultrasonic wave that ultrasonic vibration stick produced produces between polyester oligomer melt and functional powder leads to the formation, growth and the blasting compression of bubble in the polyester oligomer melt, with the power control of ultrasonic vibration stick in above-mentioned within range, can prevent to lead to the ultrasonic wave intensity increase in the unit area because of ultrasonic power is too big, make the bubble quantity that produces in the polyester oligomer melt too saturated, the ultrasonic wave can take place the scattering attenuation between a large amount of bubbles, leads to the cavitation effect to weaken. The functional polyester condensation compound with more dispersed functional powder can be prepared by utilizing the reaction conditions of the ultrasonic vibrating rod.

As an embodiment of the invention, the intrinsic viscosity of the functional polyester prepared in the step S4 is 0.5-1.2 dL/g, and the filter pressing value FPFPV is not more than 0.2 bar/g.

The intrinsic viscosity and the filter pressing value are controlled within the ranges, so that the functional powder can be highly and uniformly dispersed in the polyester matrix, and the prepared functional polyester is suitable for preparing products such as high-quality films, fibers and the like.

Preferably, the reaction temperature of the esterification system is 230-290 ℃, the reaction temperature of the pre-polycondensation system is 240-295 ℃, and the reaction temperature of the final polycondensation system is 250-300 ℃.

The third purpose of the invention is to provide a functional polyester fiber spun by the functional polyester prepared by the functional polyester production system and the functional polyester production method.

Preferably, the functional polyester fiber comprises one or more of dope-dyed, antibacterial, radiation-proof, antistatic, fluorescent, far-infrared, heat-conducting or negative-ion functional polyester fiber.

Preferably, the functional polyester molecule is copolyester with cationic dye dyeable, hydrophilic, cotton-like, flame retardant, low melting point or high shrinkage functions.

Preferably, the functional polyester molecule is polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate.

In one embodiment of the present invention, the functional polyester fiber has a breaking strength of 2.6 to 8.4cN/dtex and an elongation at break of 17 to 67%.

After adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects:

the functional polyester production system provided by the invention can continuously prepare the functional polyester oligomer with small dispersed particle size of the functional powder, then the functional polyester with highly uniform dispersed functional powder can be obtained through the polycondensation reaction of the functional polyester oligomer, the filter pressing value FPFPV of the prepared functional polyester is not more than 0.2bar/g, the spinning performance of the functional polyester is favorably improved, and the functional polyester production system is suitable for producing products such as high-quality fibers, films and the like.

The production method of the functional polyester provided by the invention can realize highly uniform dispersion of functional powder in the functional polyester, effectively reduce agglomeration of the powder in the preparation process of the functional polyester fiber, improve the spinning performance of the functional polyester, shorten the reaction time, improve the production efficiency of the functional polyester and reduce the cost.

The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.

Drawings

The accompanying drawings, which are included to provide a further understanding of the invention, are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without limiting the invention to the right. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:

FIG. 1 is a schematic structural diagram of an ultrasonic reaction kettle body in a functional polyester production system according to the present invention;

FIG. 2 is a side view of an ultrasonic reactor vessel in the functional polyester production system of the present invention;

FIG. 3 is a process flow diagram of a process for producing functional polyester according to the present invention.

In the figure: 1. an ultrasonic reaction kettle body; 2. a partition plate; 3. a stirrer; 4. a non-return flow guide hole; 5. an ultrasonic vibrator; 6. a heating medium jacket; 7. a heating coil; 8. a heating medium inlet pipeline; 9. a heating medium outlet pipeline; 10. a flow regulating valve; 11. a material inlet; 12. a material outlet; 13. a syringe dispenser; 14. a gas phase outlet; 15. a steam separation condenser; 16. a pressure regulating valve.

It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.

As shown in fig. 1 and 2, the present invention provides a functional polyester production system comprising: the system comprises a polyester main production system and a functional polyester oligomer continuous preparation system, wherein the polyester main production system comprises an esterification system, a pre-polycondensation system and a final polycondensation system which are connected in sequence, and the functional polyester oligomer continuous preparation system comprises an accurate control reaction unit and a mixing unit which are arranged between the esterification system and the pre-polycondensation system; the accurate control reaction unit includes horizontal reation kettle, horizontal reation kettle specifically is ultrasonic reaction cauldron, 1 bottom of the ultrasonic reaction cauldron body be provided with an at least baffle 2 in order with the internal space of the ultrasonic reaction cauldron body 1 separates into two at least cavities, the non return water conservancy diversion hole 4 that supplies the one-way flow of reaction material is seted up to the bottom of baffle 2, is equipped with agitator 3 and two at least ultrasonic vibrator 5 in each cavity.

All be equipped with in each cavity with heat medium pipe connection's heat medium jacket 6 and heating coil 7, the heat medium pipe connection includes two at least heat medium inlet line 8 and heat medium outlet line 9, the heating temperature of heat medium jacket 6 and heating coil 7 in each cavity is by setting up flow control valve 10 independent control on different heat medium outlet line 9.

The ultrasonic reaction kettle body 1 is provided with a material inlet 11 and a material outlet 12, the material inlet 11 is located at the lower part of one side of the reaction kettle body, and the material outlet 12 is located at the bottom of the other side of the reaction kettle body. The top of the ultrasonic reaction kettle body 1 is provided with a gas phase outlet 14, and a gas phase pipeline connecting the gas phase outlet with the steam separation condenser 15 is provided with a reaction kettle pressure regulating valve 16.

Each chamber of the reaction kettle is provided with 2 telescopic modifier injection distributors 13.

Examples 1 to 18 below all used the production system of the above-mentioned functional polyester to prepare functional polyester.

Example 1

In this example, the steps for preparing the functional polyester are as follows:

s1: terephthalic acid, ethylene glycol and a catalyst ethylene glycol antimony with the addition of 500ppm of the weight of the terephthalic acid are blended to prepare terephthalic acid slurry with the molar ratio of alcohol to acid of 2.0, and the terephthalic acid slurry is continuously and uniformly conveyed to an esterification reaction system consisting of a vertical reaction kettle at the flow rate of 366kg/h for esterification reaction, wherein the reaction temperature of the esterification reaction kettle is 290 ℃. When the acid value of the polyester oligomer reached 50mgKOH/g, it was continuously and stably withdrawn from the esterification reaction vessel at a flow rate of 271kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing a polyester oligomer from an esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to a step-by-step accurate control ultrasonic reaction kettle at a flow rate of 79.8kg/h, 2 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, the height of each partition plate is 1/2 of the height of the reaction kettle body, and a flap opening turbine type stirrer is arranged in each chamber; 4 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1500W.

The ethylene glycol-based functional powder pre-dispersion slurry with the carbon black concentration of 20 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding mills in series at a flow rate of 37.5kg/h, and the functional powder slurry with the carbon black average particle size of 174nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 37.5kg/h into a first chamber of a stepwise accurately controlled ultrasonic reaction kettle to be uniformly mixed with polyester oligomer from an esterification system, then sequentially removing excessive ethylene glycol through a second chamber and a third chamber of the stepwise accurately controlled ultrasonic reaction kettle to obtain a functional powder condensation compound, and accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 220 ℃, the temperature of the second chamber to be 240 ℃, the temperature of the third chamber to be 250 ℃ step by step and the total reaction time to be 90 min. When the hydroxyl value of the functional powder condensation compound reaches 135mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the ultrasonic reaction kettle in a step-by-step accurate control manner at the flow rate of 83.3kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 9 wt%, and the average particle size is 253 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 191.2kg/h, feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together, and uniformly mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical pre-polycondensation reaction kettle, wherein the temperature of reactants in the pre-polycondensation reaction kettle is 295 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.30dL/g, the functional polyester is obtained by continuously and stably extracting the functional polyester prepolymer from the pre-polycondensation reaction kettle through a prepolymer pump and conveying the functional polyester prepolymer to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 290 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.67dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the stock solution colored black polyester fiber with the substrate being polyethylene terephthalate, wherein the filter pressing value FPFPV of the functional polyester is 0.028 bar/g. The dope-dyed black polyester fiber had a single-fiber fineness of 0.58dtex, a breaking strength of 3.2cN/dtex, and an elongation at break of 33%.

Example 2

In this example, the steps for preparing the functional polyester are as follows:

s1, continuously and uniformly conveying terephthalic acid slurry with the molar ratio of 1.13 to alcohol acid, which is prepared by blending terephthalic acid and ethylene glycol, to an esterification reaction system consisting of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle at the flow rate of 300kg/h for esterification reaction, wherein the reaction temperature of the first esterification reaction kettle is 260 ℃, and the reaction temperature of the second esterification reaction kettle is 265 ℃. The catalyst glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the second esterification reaction kettle at the flow rate of 5.4 kg/h. When the acid value of the polyester oligomer reached 15mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 261kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing a polyester oligomer from an esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to a step-by-step accurate control ultrasonic reaction kettle at a flow rate of 57.8kg/h, 2 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, the height of each partition plate is 1/2 of the height of the reaction kettle body, and a flap opening turbine type stirrer is arranged in each chamber; 4 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1500W.

The ethylene glycol-based functional powder pre-dispersion slurry with pigment blue 15:3 concentration of 40 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 15kg/h, and the functional powder slurry with the carbon black average particle size of 142nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 15kg/h into a first chamber of a stepwise accurately controlled ultrasonic reaction kettle, uniformly mixing the functional powder slurry with a polyester oligomer from an esterification system, then sequentially removing excessive ethylene glycol through a second chamber and a third chamber of the stepwise accurately controlled ultrasonic reaction kettle to obtain a functional powder condensation compound, and accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 220 ℃, the temperature of the second chamber to be 230 ℃, the temperature of the third chamber to be 250 ℃ step by step, wherein the total reaction time is 90 min. When the hydroxyl value of the functional powder condensation compound reaches 226mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 68.7kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 8.7 wt%, and the average particle size is 214 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 203.2kg/h, and feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a horizontal second pre-polycondensation reaction kettle, wherein the temperature of reactants of the first pre-polycondensation reaction kettle is 270 ℃, and the temperature of reactants of the second pre-polycondensation reaction kettle is 275 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.35dL/g, the functional polyester is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction, and the functional polyester is obtained. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 280 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.65dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the stock solution colored blue polyester fiber with the substrate being polyethylene terephthalate, wherein the filter pressing value FPFPV of the functional polyester is 0.021 bar/g. The dope-dyed blue polyester fiber had a single-fiber fineness of 0.77dtex, a breaking strength of 4.0cN/dtex, and an elongation at break of 32%.

Example 3

In this example, the steps for preparing the functional polyester are as follows:

s1, continuously and uniformly conveying terephthalic acid slurry with the molar ratio of 1.13 of alcohol acid, which is prepared by blending terephthalic acid and ethylene glycol, to an esterification reaction system consisting of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle at a flow rate of 302kg/h for esterification reaction, wherein the reaction temperature of the first esterification reaction kettle is 260 ℃, and the reaction temperature of the second esterification reaction kettle is 265 ℃. The catalyst glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the second esterification reaction kettle at the flow rate of 5.4 kg/h. When the acid value of the polyester oligomer reached 15mgKOH/g, the polyester oligomer was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 263kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 75.5kg/h, 2 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, and the height of each partition plate is 1/2 of the height of the reaction kettle body; a hinge opening turbine type stirrer is arranged in each chamber; 2 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, and the frequency of each ultrasonic vibration rod is 20kHz and the power of each ultrasonic vibration rod is 3000W.

The ethylene glycol-based functional powder pre-dispersion slurry with the carbon black concentration of 20 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding mills in series at the flow rate of 22.5kg/h, and the functional powder slurry with the carbon black average particle size of 174nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system into a first chamber of a stepped accurately-controlled ultrasonic reaction kettle at a flow rate of 22.5kg/h to be uniformly mixed with polyester oligomer from an esterification system, then sequentially removing excessive ethylene glycol through a second chamber and a third chamber of the stepped accurately-controlled ultrasonic reaction kettle to obtain a functional powder condensation compound, and accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 220 ℃, the temperature of the second chamber to be 230 ℃, the temperature of the third chamber to be 250 ℃ step by step, wherein the total reaction time is 90 min. When the hydroxyl value of the functional powder condensation compound reaches 127mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 80.7kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, the content of the functional powder in the functional powder condensation compound is 5.6 wt%, and the average particle size is 209 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 187.5kg/h, and feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer. The pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a vertical second pre-polycondensation reaction kettle, wherein the temperature of the reactant of the first pre-polycondensation reaction kettle is 270 ℃, and the temperature of the reactant of the second pre-polycondensation reaction kettle is 275 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.16dL/g, the functional polyester prepolymer is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle and a horizontal liquid phase tackifying kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 280 ℃, and the reaction temperature of the liquid phase tackifying reaction kettle is 295 ℃.

When the intrinsic viscosity of the functional polyester tackifying compound reaches 1.00dL/g, the functional polyester tackifying melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the dope-dyed black polyester fiber with the base body made of polyethylene terephthalate, wherein the filter pressing value FPFPV of the functional polyester is 0.026 bar/g. The dope-dyed black polyester fiber had a single-filament fineness of 2.86dtex, a breaking strength of 8.4cN/dtex, and an elongation at break of 17%

Example 4

In this example, the steps for preparing the functional polyester are as follows:

s1, continuously and uniformly conveying terephthalic acid slurry with the molar ratio of 1.13 to alcohol acid, which is prepared by blending terephthalic acid and ethylene glycol, to an esterification reaction system consisting of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle at the flow rate of 295kg/h for esterification reaction, wherein the reaction temperature of the first esterification reaction kettle is 260 ℃, and the reaction temperature of the second esterification reaction kettle is 265 ℃. The catalyst glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the second esterification reaction kettle at the flow rate of 5.4 kg/h. When the acid value of the polyester oligomer reached 15mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 257kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 52.3kg/h, 3 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 4 chambers, the height of each partition plate is 1/2 of the height of the reaction kettle body, and a push type stirrer is arranged in each chamber; 8 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/4 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 500W.

The ethylene glycol-based functional powder pre-dispersion slurry with the delustering agent titanium dioxide concentration of 30 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 33.3kg/h, and the functional powder slurry with the carbon black average particle size of 320nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 33.3kg/h into a second chamber of an ultrasonic reaction kettle, accurately controlling the second chamber to be uniformly mixed with polyester oligomer from a first chamber step by step, and then, sequentially and accurately controlling a third chamber and a fourth chamber of the ultrasonic reaction kettle step by step to remove excessive glycol to obtain a functional powder condensation compound, wherein the temperature of the first chamber of the ultrasonic reaction kettle is accurately controlled step by step to be 230 ℃, the temperature of the second chamber is 200 ℃, the temperature of the third chamber is 230 ℃, the temperature of the fourth chamber is 240 ℃, and the total reaction time is 120 min. When the hydroxyl value of the functional powder condensation compound reaches 214mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the fourth chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 66.7kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, the content of the functional powder in the functional powder condensation compound is 15 wt%, and the average particle size is 394 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 204.7kg/h, and feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a ball-and-socket dynamic mixer.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a horizontal second pre-polycondensation reaction kettle, wherein the temperature of reactants of the first pre-polycondensation reaction kettle is 270 ℃, and the temperature of reactants of the second pre-polycondensation reaction kettle is 275 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.35dL/g, the functional polyester is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction, and the functional polyester is obtained. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 280 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.67dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the full-dull polyester fiber with the substrate being polyethylene terephthalate, wherein the filter pressing value FPFPV of the functional polyester is 0.050 bar/g. The full-dull polyester fiber had a single-fiber fineness of 1.54dtex, a breaking strength of 3.2cN/dtex, and an elongation at break of 25%.

Example 5

In this example, the steps for preparing the functional polyester are as follows:

s1, the polyester oligomer raw material is composed of terephthalic acid slurry and hydrophilic copolymerization modified monomer polyethylene glycol slurry, wherein the terephthalic acid slurry is prepared by blending terephthalic acid and ethylene glycol according to the molar ratio of 1.15 to alcohol acid, and the hydrophilic copolymerization modified monomer polyethylene glycol slurry is prepared by melting polyethylene glycol at 80 ℃. The esterification reaction system consists of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle, wherein terephthalic acid slurry is continuously and uniformly conveyed to the vertical first esterification reaction kettle at a flow rate of 278kg/h, hydrophilic copolymerization modified monomer polyethylene glycol slurry is continuously and uniformly injected into the vertical second esterification reaction kettle at a flow rate of 12.5kg/h, and catalyst ethylene glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the vertical second esterification reaction kettle at a flow rate of 5.4 kg/h. The reaction temperature of the first esterification reaction kettle is 260 ℃, and the reaction temperature of the second esterification reaction kettle is 255 ℃. When the acid value of the polyester oligomer reached 25mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 256kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the ultrasonic reaction kettle with the flow rate of 62.7kg/h, the ultrasonic reaction kettle body is accurately controlled step by step, 2 partition plates are arranged in the ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, the height of each partition plate is 1/2 of the height of the reaction kettle body, a flap opening turbine type stirrer is arranged in each chamber, 4 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1500W.

The ethylene glycol-based functional powder pre-dispersion slurry with the carbon black concentration of 20 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 25kg/h, and the functional powder slurry with the carbon black average particle size of 174nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 25kg/h into a first chamber of a step-by-step accurately controlled ultrasonic reaction kettle and uniformly mixing with a polyester oligomer from an esterification system, and then sequentially removing excessive ethylene glycol through a second chamber and a third chamber of the step-by-step accurately controlled ultrasonic reaction kettle to obtain a functional powder condensation product, wherein a high-shear mixer is a high-shear pump, the temperature of the first chamber of the ultrasonic reaction kettle is accurately controlled in steps to be 220 ℃, the temperature of the second chamber is controlled to be 240 ℃, the temperature of the third chamber is controlled to be 250 ℃, and the total reaction time is 90 min. When the hydroxyl value of the functional powder condensation compound reaches 228mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 71.4kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 7 wt%, and the average particle size is 242 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 191.2kg/h, feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together, and uniformly mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer. The pre-polycondensation reaction system consists of a vertical pre-polycondensation reaction kettle, wherein the reactant temperature of the pre-polycondensation reaction kettle is 270 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.30dL/g, the functional polyester prepolymer is continuously and stably extracted from the pre-polycondensation reaction kettle through a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 275 ℃.

When the intrinsic viscosity of the functional polyester tackifying compound reaches 0.72dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the stock solution coloring black hydrophilic polyester fiber with the matrix being hydrophilic copolyester, wherein the filter pressing value FPFPFPV of the functional polyester is 0.031 bar/g. The monofilament fineness of the dope-dyed black hydrophilic polyester fiber is 1.54dtex, the breaking strength is 3.2cN/dtex, and the elongation at break is 34%.

Example 6

In this example, the steps for preparing the functional polyester are as follows:

s1, the polyester oligomer raw material slurry is composed of terephthalic acid slurry and low-melting point copolymerization modified monomer isophthalic acid slurry, wherein the terephthalic acid slurry is prepared by blending terephthalic acid and ethylene glycol according to the molar ratio of 1.12 of alcohol acid, and the low-melting point copolymerization modified monomer isophthalic acid slurry is prepared by blending isophthalic acid and ethylene glycol according to the molar ratio of 1.12 of alcohol acid. The terephthalic acid slurry is continuously and uniformly conveyed to a first esterification reaction kettle of an esterification reaction system consisting of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle at the flow rate of 178kg/h and the flow rate of 119kg/h simultaneously to carry out esterification reaction, wherein the reaction temperature of the first esterification reaction kettle is 260 ℃, and the reaction temperature of the second esterification reaction kettle is 265 ℃. The catalyst glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the second esterification reaction kettle at the flow rate of 5.4 kg/h. When the acid value of the polyester oligomer reached 15mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 259kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the ultrasonic reaction kettle with the flow rate of 45.4kg/h, the ultrasonic reaction kettle body is accurately controlled step by step, 1 partition plate is arranged in the ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 2 chambers, the height of the partition plate is 3/4 of the height of the reaction kettle body, a flap disc turbine type stirrer is arranged in each chamber, 4 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1500W.

The ethylene glycol-based functional powder pre-dispersion slurry with the carbon black concentration of 20 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 25kg/h, and the functional powder slurry with the carbon black average particle size of 174nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 12.5kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, and then removing excessive glycol through a second chamber of the ultrasonic reaction kettle, so as to obtain a functional powder condensation compound, wherein a high-shear mixer is a grinder, the temperature of the first chamber of the ultrasonic reaction kettle is accurately controlled to be 230 ℃, the temperature of the second chamber is controlled to be 250 ℃, and the total reaction time is 100 min. When the hydroxyl value of the functional powder condensation compound reaches 108mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the second chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 53.4kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 14 wt%, and the average particle size is 331 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 213.6kg/h, and feeding the polyester oligomer and a functional powder condensation compound from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a dynamic and static ring gear type dynamic mixer.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a vertical second pre-polycondensation reaction kettle, wherein the temperature of reactants of the first pre-polycondensation reaction kettle is 265 ℃, and the temperature of reactants of the second pre-polycondensation reaction kettle is 270 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.22dL/g, the functional polyester prepolymer is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 275 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.70dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the stock solution colored red low-melting-point polyester fiber with the matrix being low-melting-point copolyester, wherein the filter pressing value FPFPV of the functional polyester is 0.113 bar/g. The filament number of the dope-dyed red low-melting-point polyester fiber is 3.47dtex, the breaking strength is 2.6cN/dtex, and the elongation at break is 67%.

Example 7

In this example, the steps for preparing the functional polyester are as follows:

s1, terephthalic acid slurry which is prepared by terephthalic acid and butanediol and has the molar ratio of 1.12 of alcohol acid is continuously and uniformly conveyed to an esterification reaction system consisting of a vertical esterification reaction kettle at a flow rate of 294kg/h for esterification reaction, and the reaction temperature of the esterification reaction kettle is 240 ℃. The catalyst tetrabutyl titanate solution with the concentration of 20 wt% is continuously and evenly injected into the vertical esterification reaction kettle at the flow rate of 3.5 kg/h. When the acid value of the polyester oligomer reached 13mgKOH/g, it was continuously and stably withdrawn from the esterification reaction vessel at a flow rate of 259kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 45.4kg/h, 2 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, and the height of each partition plate is 3/4 of the height of the reaction kettle body; a push type stirrer is arranged in each chamber; 4 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1500W.

Butanediol-based functional powder pre-dispersion slurry with a heat conducting agent aluminum nitride concentration of 30 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 25kg/h, and the functional powder slurry with the carbon black average particle size of 50nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 25kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, then sequentially and accurately controlling a second chamber and a third chamber of the ultrasonic reaction kettle step by step to remove excessive butanediol to obtain a functional powder condensation compound, accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle step by step to be 210 ℃, the temperature of the second chamber to be 230 ℃, the temperature of the third chamber to be 240 ℃, and controlling the total reaction time to be 90 min. When the hydroxyl value of the functional powder condensation compound reaches 98mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 54.3kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, the content of the functional powder in the functional powder condensation compound is 13.8 wt%, and the average particle size is 103 nm.

Delivering the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 213.6kg/h, feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together, and uniformly mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical pre-polycondensation reaction kettle, wherein the reactant temperature of the pre-polycondensation reaction kettle is 240 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.50dL/g, the functional polyester prepolymer is continuously and stably extracted from the pre-polycondensation reaction kettle through a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 260 ℃.

When the intrinsic viscosity of the functional polyester reaches 1.20dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the heat-conducting polyester fiber with the substrate being polybutylene terephthalate, wherein the filter pressing value FPFPV of the functional polyester is 0.014 bar/g. The heat-conducting fiber has a filament number of 3.47dtex, a breaking strength of 3.4cN/dtex, and an elongation at break of 29%.

Example 8

In this example, the steps for preparing the functional polyester are as follows:

s1, continuously and uniformly conveying terephthalic acid slurry with the molar ratio of 1.4 to the alcohol acid prepared by terephthalic acid and propylene glycol at a flow rate of 327kg/h to an esterification reaction system consisting of a vertical first esterification reaction kettle and a horizontal second esterification reaction kettle for esterification reaction, wherein the reaction temperature of the first esterification reaction kettle is 235 ℃, and the reaction temperature of the second esterification reaction kettle is 240 ℃. A10 wt% solution of tetraisopropyl titanate as a catalyst was continuously and uniformly injected into the second esterification reaction vessel at a flow rate of 1.2 kg/h. When the acid value of the polyester oligomer reached 10mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 285kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 54.2kg/h, wherein 1 partition plate is arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 2 chambers, and the height of the partition plate is 3/4 of the height of the reaction kettle body; a flap disc turbine type stirrer is arranged in each chamber; 12 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 40kHz, and the power of each ultrasonic vibration rod is 500W.

Propylene glycol-based functional powder pre-dispersion slurry with the fluorescent agent long afterglow phosphor (SrMgAl4O8: Eu2+ Dy3+) concentration of 11 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at the flow rate of 30kg/h, and the functional powder slurry with the carbon black average particle size of 742nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 30kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, removing excessive propylene glycol through a second chamber of the ultrasonic reaction kettle, obtaining a functional powder condensation compound, accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 200 ℃, the temperature of the second chamber to be 220 ℃ step by step, and controlling the total reaction time to be 40 min. When the hydroxyl value of the functional powder condensation compound reaches 350mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the second chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 67.3kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 5.0 wt%, and the average particle diameter is 856 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 230.8kg/h, and feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical pre-polycondensation reaction kettle, wherein the reactant temperature of the pre-polycondensation reaction kettle is 255 ℃. When the inherent viscosity of the prepolymer reaches 0.5dL/g, the prepolymer is continuously and stably extracted from the pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 260 ℃.

When the intrinsic viscosity of the final polymer reaches 0.95dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the fluorescent polyester fiber with the substrate being polytrimethylene terephthalate, wherein the filter pressing value FPFPFPV of the functional polyester is 0.162 bar/g. The fluorescent polyester fiber has a filament fineness of 3.47dtex, a breaking strength of 2.6cN/dtex, and an elongation at break of 32%.

Example 9

In this example, the steps for preparing the functional polyester are as follows:

s1, terephthalic acid slurry with the molar ratio of 2.0 of alcohol acid, which is prepared by blending terephthalic acid, ethylene glycol and a catalyst of ethylene glycol antimony with the addition of 500ppm of the weight of the terephthalic acid, is continuously and uniformly conveyed to an esterification reaction system consisting of a vertical esterification reaction kettle at a flow rate of 322kg/h for esterification reaction, wherein the reaction temperature of the esterification reaction kettle is 290 ℃. When the acid value of the polyester oligomer reached 40mgKOH/g, the polyester oligomer was continuously and stably withdrawn from the esterification reaction vessel at a flow rate of 260kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 64.9kg/h, 2 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, and the height of each partition plate is 1/2 of the height of the reaction kettle body; a hinge opening turbine type stirrer is arranged in each chamber; 4 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1500W.

The ethylene glycol based functional powder pre-dispersion slurry with the zirconium carbide concentration of 20 wt% as a far infrared agent is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 33.75kg/h, and the functional powder slurry with the carbon black average particle size of 112nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 33.75kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, then sequentially removing excessive ethylene glycol through a second chamber and a third chamber of the ultrasonic reaction kettle, so as to obtain a functional powder condensation compound, accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 210 ℃, the temperature of the second chamber to be 220 ℃, the temperature of the third chamber to be 230 ℃ step by step, and controlling the total reaction time to be 90 min. When the hydroxyl value of the functional powder condensation compound reaches 288mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 80.6kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, the content of the functional powder in the functional powder condensation compound is 8.4 wt%, and the average particle size is 254 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 195.1kg/h, and feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical pre-polycondensation reaction kettle, wherein the reactant temperature of the pre-polycondensation reaction kettle is 290 ℃. When the inherent viscosity of the prepolymer reaches 0.30dL/g, the prepolymer is continuously and stably extracted from the pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 285 ℃.

When the intrinsic viscosity of the final polymer reaches 0.50dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the far infrared polyester fiber with the substrate being polyethylene terephthalate, wherein the filter pressing value FPFPFPV of the functional polyester is 0.033 bar/g. The far-infrared polyester fiber has a single fiber fineness of 1.54dtex, a breaking strength of 3.1cN/dtex, and an elongation at break of 28%.

Example 10

In this example, the steps for preparing the functional polyester are as follows:

s1, continuously and uniformly conveying terephthalic acid slurry with the molar ratio of 1.05 to alcohol acid, which is prepared by blending terephthalic acid and ethylene glycol, to an esterification reaction system consisting of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle at a flow rate of 298kg/h for esterification reaction, wherein the reaction temperature of the first esterification reaction kettle is 270 ℃, and the reaction temperature of the second esterification reaction kettle is 280 ℃. The catalyst glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the second esterification reaction kettle at the flow rate of 5.4 kg/h. When the acid value of the polyester oligomer reached 20mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 259kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 49.7kg/h, 2 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, and the height of each partition plate is 1/2 of the height of the reaction kettle body; a hinge opening turbine type stirrer is arranged in each chamber; 4 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1500W.

The ethylene glycol-based functional powder pre-dispersion slurry with the anti-ultraviolet radiation agent zinc oxide concentration of 11 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 25kg/h, and the functional powder slurry with the carbon black average particle size of 340nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 25kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, and then, sequentially and accurately controlling a second chamber and a third chamber of the ultrasonic reaction kettle step by step to remove excessive glycol to obtain a functional powder condensation compound, wherein the temperature of the first chamber of the ultrasonic reaction kettle is accurately controlled step by step to be 220 ℃, the temperature of the second chamber is 230 ℃, the temperature of the third chamber is 240 ℃, and the total reaction time is 90 min. When the hydroxyl value of the functional powder condensation compound reaches 239mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the ultrasonic reaction kettle in a step-by-step accurate control manner at the flow rate of 57.7kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 4.7 wt%, and the average particle size is 376 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 209.3kg/h, and feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a horizontal second pre-polycondensation reaction kettle, wherein the temperature of the reactant of the first pre-polycondensation reaction kettle is 275 ℃, and the temperature of the reactant of the second pre-polycondensation reaction kettle is 280 ℃. When the inherent viscosity of the prepolymer reaches 0.38dL/g, the prepolymer is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 285 ℃.

When the intrinsic viscosity of the final polymer reaches 0.62dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the radiation-proof polyester fiber with the substrate being polyethylene terephthalate, wherein the filter pressing value FPFPV of the functional polyester is 0.064 bar/g. The single filament number of the radiation-proof polyester fiber is 2.31dtex, the breaking strength is 3.5cN/dtex, and the elongation at break is 30%.

Example 11

In this example, the steps for preparing the functional polyester are as follows:

s1, continuously and uniformly conveying terephthalic acid slurry with the molar ratio of 1.05 to alcohol acid, which is prepared by blending terephthalic acid and ethylene glycol, to an esterification reaction system consisting of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle at the flow rate of 286kg/h for esterification reaction, wherein the reaction temperature of the first esterification reaction kettle is 270 ℃, and the reaction temperature of the second esterification reaction kettle is 280 ℃. The catalyst glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the second esterification reaction kettle at the flow rate of 5.4 kg/h. When the acid value of the polyester oligomer reached 25mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 248.7kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 48.3kg/h, 4 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 5 chambers, and the height of each partition plate is 1/2 of the height of the reaction kettle body; a triangular reciprocating rotary stirrer is arranged in each chamber; 2 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 2000W.

Ethylene glycol-based functional powder pre-dispersion slurry with a conductive agent of tin antimony oxide concentration of 30 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 41.7kg/h, and the functional powder slurry with the carbon black average particle size of 68nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system, accurately controlling the second chamber of an ultrasonic reaction kettle step by step and uniformly mixing the functional powder slurry with polyester oligomer from the first chamber, then sequentially and accurately controlling the third chamber, the fourth chamber and the fifth chamber of the ultrasonic reaction kettle step by step to remove excessive glycol to obtain a functional powder condensation compound, and accurately controlling the first chamber temperature of the ultrasonic reaction kettle step by step to be 240 ℃, the second chamber temperature to be 200 ℃, the third chamber temperature to be 220 ℃, the fourth chamber temperature to be 240 ℃, the fifth chamber temperature to be 250 ℃ and the total reaction time to be 50 min. When the hydroxyl value of the functional powder condensation compound reaches 141mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the fifth chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 62.6kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 20 wt%, and the average particle diameter is 182 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 200.4kg/h, and feeding the polyester oligomer and a functional powder condensation compound from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a grinder.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a horizontal second pre-polycondensation reaction kettle, wherein the temperature of reactants of the first pre-polycondensation reaction kettle is 280 ℃, and the temperature of reactants of the second pre-polycondensation reaction kettle is 285 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.50dL/g, the functional polyester prepolymer is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle and a horizontal liquid phase tackifying kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 290 ℃, and the reaction temperature of the liquid phase tackifying kettle is 300 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.80dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the antistatic polyester fiber with the polyethylene terephthalate as the matrix, wherein the filter pressing value FPFPV of the functional polyester is 0.015 bar/g. The antistatic polyester fiber has a filament number of 3.47dtex, a breaking strength of 3.4cN/dtex, and an elongation at break of 26%.

Example 12

In this example, the steps for preparing the functional polyester are as follows:

s1, continuously and uniformly conveying terephthalic acid slurry with the molar ratio of 1.12 to alkyd, which is prepared by blending terephthalic acid and butanediol, to an esterification reaction system consisting of a vertical esterification reaction kettle at a flow rate of 297kg/h for esterification reaction, wherein the reaction temperature of the esterification reaction kettle is 240 ℃. The catalyst tetrabutyl titanate solution with the concentration of 20 wt% is continuously and evenly injected into the vertical esterification reaction kettle at the flow rate of 3.5 kg/h. When the acid value of the polyester oligomer reached 13mgKOH/g, it was continuously and stably withdrawn from the esterification reaction vessel at a flow rate of 262kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 61.5kg/h, wherein 1 partition plate is arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 2 chambers, and the height of the partition plate is 3/4 of the height of the reaction kettle body; a flap disc turbine type stirrer is arranged in each chamber; 12 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 80kHz, and the power of each ultrasonic vibration rod is 500W.

Butanediol-based functional powder pre-dispersion slurry with a negative ion generator tourmaline concentration of 30 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 16.7kg/h, and the functional powder slurry with the carbon black average particle size of 254nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 16.7kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, removing excessive butanediol through a second chamber of the ultrasonic reaction kettle, obtaining a functional powder condensation compound, accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 230 ℃, the temperature of the second chamber to be 240 ℃ step by step and controlling the total reaction time to be 60 min. When the hydroxyl value of the functional powder condensation compound reaches 98mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the second chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 54.3kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, the content of the functional powder in the functional powder condensation compound is 9.2 wt%, and the average particle size is 353 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 200.5kg/h, and feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer; the pre-polycondensation reaction system consists of a vertical pre-polycondensation reaction kettle, wherein the reactant temperature of the pre-polycondensation reaction kettle is 250 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.40dL/g, the functional polyester prepolymer is continuously and stably extracted from the pre-polycondensation reaction kettle through a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation reaction system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 250 ℃.

When the intrinsic viscosity of the functional polyester reaches 1.00dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the negative ion polyester fiber with the substrate being polybutylene terephthalate, wherein the filter pressing value FPFPV of the functional polyester is 0.071 bar/g. The anion fiber had a single fiber fineness of 3.47dtex, a breaking strength of 2.8cN/dtex, and an elongation at break of 33%.

Example 13

In this example, the steps for preparing the functional polyester are as follows:

s1, the raw material slurry of the polyester oligomer slurry is composed of terephthalic acid slurry and high-shrinkage copolymerization modified monomer neopentyl glycol slurry, wherein the terephthalic acid slurry is prepared by blending terephthalic acid and ethylene glycol according to the molar ratio of alcohol acid of 1.05, and the high-shrinkage copolymerization modified monomer neopentyl glycol slurry is prepared by blending neopentyl glycol and ethylene glycol according to the weight ratio of 8: 2. The esterification system comprises a first esterification reaction kettle of an esterification system consisting of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle, wherein the first esterification reaction kettle is used for carrying out esterification reaction, terephthalic acid slurry is used at the flow rate of 292kg/h, and high-shrinkage copolymerization modified monomer neopentyl glycol slurry is simultaneously and continuously and uniformly conveyed at the flow rate of 13.2 kg/h. The reaction temperature of the first esterification reaction kettle is 260 ℃, and the reaction temperature of the second esterification reaction kettle is 265 ℃. The catalyst glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the second esterification reaction kettle at the flow rate of 5.4 kg/h. When the acid value of the polyester oligomer reached 15mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 266kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 58.9kg/h, wherein 1 partition plate is arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 2 chambers, and the height of the partition plate is 3/4 of the height of the reaction kettle body; a hinge opening turbine type stirrer is arranged in each chamber; 8 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 40kHz, and the power of each ultrasonic vibration rod is 1000W.

The ethylene glycol-based functional powder pre-dispersion slurry with the pigment yellow 147 concentration of 40 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 15.2kg/h, and the functional powder slurry with the carbon black average particle size of 246nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 15.2kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, removing excessive glycol through a second chamber of the ultrasonic reaction kettle, obtaining a functional powder condensation compound, accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 220 ℃, the temperature of the second chamber to be 240 ℃ step by step and controlling the total reaction time to be 60 min. When the hydroxyl value of the functional powder condensation compound reaches 158mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the second chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 67.6kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 9 wt%, and the average particle size is 376 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 207.1kg/h, and feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer. The pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a vertical second pre-polycondensation reaction kettle, wherein the temperature of reactants of the first pre-polycondensation reaction kettle is 265 ℃, and the temperature of reactants of the second pre-polycondensation reaction kettle is 270 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.20dL/g, the functional polyester prepolymer is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 275 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.72dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the stock solution colored yellow high-shrinkage polyester fiber with the substrate of high-shrinkage copolyester, wherein the filter pressing value FPFPV of the functional polyester is 0.102 bar/g. The dope-colored yellow high-shrinkage polyester fiber has a single filament number of 3.47dtex, a breaking strength of 3.0cN/dtex, and an elongation at break of 32%.

Example 14

In this example, the steps for preparing the functional polyester are as follows:

s1, the raw material slurry of the polyester oligomer slurry and the polyester oligomer comprises terephthalic acid slurry and cationic dye dyeable copolymerization modified monomer diethylene glycol isophthalate-5-sodium sulfonate slurry, wherein the terephthalic acid slurry is prepared by blending terephthalic acid and ethylene glycol according to the molar ratio of alcohol to acid of 1.15, and the cationic dye dyeable copolymerization modified monomer diethylene glycol isophthalate-5-sodium sulfonate slurry is prepared by blending diethylene glycol isophthalate-5-sodium sulfonate and ethylene glycol according to the weight ratio of 4: 6. The esterification reaction system consists of a vertical first esterification reaction kettle and a horizontal three-chamber structure second esterification reaction kettle, wherein terephthalic acid slurry is continuously and uniformly conveyed to the vertical first esterification reaction kettle at the flow rate of 293kg/h, cationic dye dyeable copolymerization modified monomer diethylene glycol isophthalate-5-sodium sulfonate slurry is continuously and uniformly injected into a second chamber of the horizontal second esterification reaction kettle at the flow rate of 14.5kg/h, and a catalyst ethylene glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into a third chamber of the horizontal second esterification reaction kettle at the flow rate of 5.4 kg/h. The reaction temperature of the first esterification reaction kettle is 260 ℃, the reaction temperature of the first chamber of the horizontal second esterification reaction kettle is 230 ℃, the reaction temperature of the second chamber is 220 ℃ and the reaction temperature of the third chamber is 240 ℃. When the acid value of the polyester oligomer reached 10mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 290kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 50.9kg/h, 2 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, and the height of each partition plate is 1/2 of the height of the reaction kettle body; a flap disc turbine type stirrer is arranged in each chamber; 4 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1500W.

The ethylene glycol-based functional powder pre-dispersion slurry with the antibacterial agent cuprous oxide concentration of 13 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 25kg/h, and the functional powder slurry with the carbon black average particle size of 84nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 25kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, and then, sequentially and accurately controlling a second chamber and a third chamber of the ultrasonic reaction kettle step by step to remove excessive glycol to obtain a functional powder condensation compound, wherein the temperature of the first chamber of the ultrasonic reaction kettle is accurately controlled to be 220 ℃, the temperature of the second chamber is 230 ℃, the temperature of the third chamber is 250 ℃ step by step, and the total reaction time is 90 min. When the hydroxyl value of the functional powder condensation compound reaches 226mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the ultrasonic reaction kettle in a step-by-step accurate control mode at the flow rate of 57.7kg/h through a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 5.6 wt%, and the average particle size is 197 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 239.1kg/h, and feeding the polyester oligomer and a functional powder condensation compound from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer. The pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a vertical second pre-polycondensation reaction kettle, wherein the temperature of the reactant of the first pre-polycondensation reaction kettle is 270 ℃, and the temperature of the reactant of the second pre-polycondensation reaction kettle is 275 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.10dL/g, the functional polyester prepolymer is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 280 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.58dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the antibacterial cationic dye dyeable polyester fiber with the substrate of cationic dye dyeable copolyester, wherein the filter pressing value FPFPFPV of the functional polyester is 0.012 bar/g. The monofilament titer of the antibacterial cationic dye dyeable polyester fiber is 1.16dtex, the breaking strength is 3.3cN/dtex, and the elongation at break is 34%.

Example 15

In this example, the steps for preparing the functional polyester are as follows:

and S1, the polyester oligomer raw material slurry is composed of terephthalic acid slurry and dispersed dye normal-pressure dyeable copolymerization modified monomer diethylene glycol adipate slurry, wherein the terephthalic acid slurry is prepared by blending terephthalic acid and ethylene glycol according to the alcohol acid molar ratio of 1.08, and the dispersed dye normal-pressure dyeable copolymerization modified monomer diethylene glycol adipate slurry is prepared by blending diethylene glycol adipate and ethylene glycol according to the weight ratio of 6: 4. The esterification reaction system consists of a vertical first esterification reaction kettle and a horizontal three-chamber structure second esterification reaction kettle, wherein terephthalic acid slurry is continuously and uniformly conveyed to the vertical first esterification reaction kettle at the flow rate of 275kg/h, the disperse dye normal-pressure dyeable copolymerization modified monomer diethylene glycol adipate slurry is continuously and uniformly injected into the second chamber of the horizontal second esterification reaction kettle at the flow rate of 42kg/h, and the catalyst ethylene glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the third chamber of the horizontal second esterification reaction kettle at the flow rate of 5.4 kg/h. The reaction temperature of the first esterification reaction kettle is 260 ℃, the reaction temperature of the first chamber of the horizontal second esterification reaction kettle is 250 ℃, the reaction temperature of the second chamber is 230 ℃ and the reaction temperature of the third chamber is 250 ℃. When the acid value of the polyester oligomer reached 15mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 281kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 60.5kg/h, 2 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, and the height of each partition plate is 1/2 of the height of the reaction kettle body; a hinge opening turbine type stirrer is arranged in each chamber; 4 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1500W.

The ethylene glycol-based functional powder pre-dispersion slurry with the aerogel concentration of 10 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding mills in series at a flow rate of 37.5kg/h, and the functional powder slurry with the carbon black average particle size of 382nm is prepared by grinding and enters the functional powder slurry.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 37.5kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, then sequentially removing excessive glycol through a second chamber and a third chamber of the ultrasonic reaction kettle, so as to obtain a functional powder condensation compound, accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 210 ℃, the temperature of the second chamber to be 230 ℃, the temperature of the third chamber to be 240 ℃ step by step, and controlling the total reaction time to be 90 min. When the hydroxyl value of the functional powder condensation compound reaches 165mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the ultrasonic reaction kettle in a step-by-step accurate control mode at the flow rate of 62.5kg/h through a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flowmeter, wherein the content of functional powder in the functional powder condensation compound is 6 wt%, and the average particle size is 498 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 220.5kg/h, and feeding the polyester oligomer and a functional powder condensate from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer. The pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a vertical second pre-polycondensation reaction kettle, wherein the temperature of the reactant of the first pre-polycondensation reaction kettle is 270 ℃, and the temperature of the reactant of the second pre-polycondensation reaction kettle is 275 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.19dL/g, the functional polyester prepolymer is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 280 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.68dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the ultraviolet radiation resistant disperse dye normal pressure dyeable polyester fiber with the matrix of disperse dye normal pressure dyeable copolyester, wherein the filter pressing value FPFPV of the functional polyester is 0.136 bar/g. The ultraviolet radiation resistant disperse dye is capable of being dyed in normal pressure, and has the filament number of 3.47dtex, the breaking strength of 3.3cN/dtex, and the elongation at break of 32%.

Example 16

In this example, the steps for preparing the functional polyester are as follows:

s1, the polyester oligomer raw material pulp is composed of terephthalic acid pulp and cotton-like copolymerization modified monomer polyamide pulp, wherein the terephthalic acid pulp is prepared by blending terephthalic acid and ethylene glycol according to the molar ratio of alkyd being 1.12, and the cotton-like copolymerization modified monomer polyamide pulp is prepared by melting polyamide at 230 ℃. The esterification reaction system consists of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle, wherein the terephthalic acid slurry is continuously and uniformly conveyed to the vertical first esterification reaction kettle at a flow rate of 270kg/h, the cotton-like copolymerization modified monomer polyamide slurry is continuously and uniformly injected into the vertical second esterification kettle at a flow rate of 25kg/h, and the catalyst ethylene glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the vertical second esterification kettle at a flow rate of 5.4 kg/h. The reaction temperature of the first esterification reaction kettle is 260 ℃ and the reaction temperature of the second esterification reaction kettle is 265 ℃. When the acid value of the polyester oligomer reached 15mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 260kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 47.8kg/h, wherein 1 partition plate is arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 2 chambers, and the height of the partition plate is 3/4 of the height of the reaction kettle body; a hinge opening turbine type stirrer is arranged in each chamber; 8 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1000W.

The ethylene glycol-based functional powder pre-dispersion slurry with the concentration of 30 wt% of copper and zinc oxide doped in the antibacterial agent is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at the flow rate of 16.7kg/h, and the functional powder slurry with the average carbon black particle size of 99nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 16.7kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, removing excessive glycol through a second chamber of the ultrasonic reaction kettle, obtaining a functional powder condensation compound, accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 220 ℃, the temperature of the second chamber to be 230 ℃ step by step, and controlling the total reaction time to be 60 min. When the hydroxyl value of the functional powder condensation compound reaches 226mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the second chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 57.3kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, wherein the content of the functional powder in the functional powder condensation compound is 8.7 wt%, and the average particle size is 244 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 212kg/h, and feeding the polyester oligomer and a functional powder condensation compound from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a high-shear pump.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer. The pre-polycondensation reaction system consists of a vertical first pre-polycondensation reaction kettle and a vertical second pre-polycondensation reaction kettle, wherein the temperature of the reactant of the first pre-polycondensation reaction kettle is 260 ℃, and the temperature of the reactant of the second pre-polycondensation reaction kettle is 265 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.20dL/g, the functional polyester prepolymer is continuously and stably extracted from the second pre-polycondensation reaction kettle by a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 270 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.70dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the antibacterial cotton-like polyester fiber with the substrate being cotton-like copolyester, wherein the filter pressing value FPFPV of the functional polyester is 0.033 bar/g. The monofilament titer of the antibacterial cotton-like polyester fiber is 1.16dtex, the breaking strength is 3.2cN/dtex, and the elongation at break is 28%.

Example 17

In this example, the steps for preparing the functional polyester are as follows:

s1, continuously and uniformly conveying the polyester bottle flake waste and alcoholysis ethylene glycol to an esterification system composed of an esterification hydrolysis reaction kettle in 249kg/h and 24kg/h respectively, wherein the esterification hydrolysis reaction kettle is composed of a horizontal esterification hydrolysis reaction kettle which is provided with a stirrer with two stirring paddles meshed with each other in parallel. The reaction temperature of the esterification hydrolysis reaction kettle was 270 ℃. When the hydroxyl value of the alcoholysis product of the polyester waste reaches 160mgKOH/g, the alcoholysis product is continuously and stably extracted from the esterification reaction kettle at a flow rate of 273kg/h by an oligomer conveying and metering device consisting of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 44.4kg/h, wherein 1 partition plate is arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 2 chambers, the height of the partition plate is 3/4 of the height of the reaction kettle body, and a flap opening turbine type stirrer is arranged in each chamber; 8 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1000W.

The ethylene glycol-based functional powder pre-dispersion slurry with the antibacterial agent graphene concentration of 20 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 12.5kg/h, and the functional powder slurry with the carbon black average particle size of 1000nm is prepared by grinding.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 12.5kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, removing excessive glycol through a second chamber of the ultrasonic reaction kettle, obtaining a functional powder condensation compound, accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 210 ℃, the temperature of the second chamber to be 230 ℃ step by step, and controlling the total reaction time to be 50 min. When the hydroxyl value of the functional powder condensation compound reaches 350mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the second chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 50kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, the content of the functional powder in the functional powder condensation compound is 5.0 wt%, and the average particle size is 1000 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 228.6kg/h, and feeding the polyester oligomer and a functional powder condensation compound from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a grinder.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer. The pre-polycondensation reaction system consists of a vertical pre-polycondensation reaction kettle, wherein the reactant temperature of the pre-polycondensation reaction kettle is 270 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.22dL/g, the functional polyester prepolymer is continuously and stably extracted from the pre-polycondensation reaction kettle through a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 275 ℃.

When the intrinsic viscosity of the functional polyester reaches 0.67dL/g, the functional polyester melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the antibacterial regenerated polyester fiber, wherein the filter pressing value FPFPV of the functional polyester is 0.2 bar/g. The antibacterial regenerated polyester fiber has the filament number of 3.47dtex, the breaking strength of 3.2cN/dtex and the elongation at break of 26 percent.

Example 18

In this example, the steps for preparing the functional polyester are as follows:

s1, the polyester oligomer raw material is composed of terephthalic acid slurry and flame-retardant copolymerization modified monomer 2-carboxyethyl phenyl diethylene glycol hypophosphite slurry, wherein the terephthalic acid slurry is prepared by blending terephthalic acid and ethylene glycol according to the molar ratio of alcohol to acid of 1.12, and the flame-retardant copolymerization modified monomer 2-carboxyethyl phenyl diethylene glycol hypophosphite slurry is prepared by blending 2-carboxyethyl phenyl diethylene glycol hypophosphite and ethylene glycol according to the weight ratio of 4: 6. The esterification reaction system consists of a vertical first esterification reaction kettle and a vertical second esterification reaction kettle, wherein terephthalic acid slurry is continuously and uniformly conveyed to the vertical first esterification reaction kettle of the esterification system at the flow rate of 284kg/h, flame-retardant copolymerization modified monomer 2-carboxyethyl phenyl diethylene glycol hypophosphite slurry is continuously and uniformly injected into the vertical second esterification reaction kettle at the flow rate of 37.5kg/h, and catalyst ethylene glycol antimony solution with the concentration of 2 wt% is continuously and uniformly injected into the vertical second esterification reaction kettle at the flow rate of 5.4 kg/h. The reaction temperature of the first esterification reaction kettle is 260 ℃, and the reaction temperature of the second esterification reaction kettle is 270 ℃. When the acid value of the polyester oligomer reached 10mgKOH/g, it was continuously and stably withdrawn from the second esterification reaction vessel at a flow rate of 284kg/h by an oligomer transfer metering device composed of an oligomer pump and an oligomer flow meter.

S2, dividing the polyester oligomer from the esterification system into two strands, wherein one strand of the polyester oligomer is conveyed to the step-by-step accurate control ultrasonic reaction kettle at a flow rate of 87.5kg/h, 2 partition plates are arranged in the step-by-step accurate control ultrasonic reaction kettle body to divide the inner space of the reaction kettle into 3 chambers, and the height of each partition plate is 1/2 of the height of the reaction kettle body; a hinge opening turbine type stirrer is arranged in each chamber; 8 ultrasonic vibration rods are arranged in each chamber, the length of each ultrasonic vibration rod is 1/2 of the height of the reaction kettle body, the frequency of each ultrasonic vibration rod is 20kHz, and the power of each ultrasonic vibration rod is 1000W.

The ethylene glycol-based functional powder pre-dispersion slurry with the far infrared agent titanium carbide concentration of 22 wt% is continuously and uniformly conveyed to a functional powder slurry preparation system formed by connecting 3 grinding machines in series at a flow rate of 18.75kg/h, and the functional powder slurry with the carbon black average particle size of 135nm is prepared by grinding and enters the functional powder slurry.

Injecting functional powder slurry from a functional powder slurry preparation system at a flow rate of 18.75kg/h into a first chamber of an ultrasonic reaction kettle, accurately controlling the first chamber to be uniformly mixed with polyester oligomer from an esterification system step by step, then sequentially removing excessive ethylene glycol through a second chamber and a third chamber of the ultrasonic reaction kettle, so as to obtain a functional powder condensation compound, accurately controlling the temperature of the first chamber of the ultrasonic reaction kettle to be 220 ℃, the temperature of the second chamber to be 230 ℃, the temperature of the third chamber to be 240 ℃ step by step, and controlling the total reaction time to be 30 min. When the hydroxyl value of the functional powder condensation compound reaches 167mgKOH/g, the functional powder condensation compound is continuously and stably extracted from the third chamber of the step-by-step accurate control ultrasonic reaction kettle at the flow rate of 82.7kg/h by a functional powder condensation compound metering and conveying unit consisting of a conveying pump and a flow meter, the content of the functional powder in the functional powder condensation compound is 5.0 wt%, and the average particle diameter is 257 nm.

And conveying the other strand of polyester oligomer from the esterification system to an inlet pipeline of a dynamic mixer at a flow rate of 196.5kg/h, and feeding the polyester oligomer and a functional powder condensation compound from the step-by-step accurate control ultrasonic reaction kettle into the dynamic mixer together for uniform mixing to obtain the functional powder oligomer, wherein the dynamic mixer is a planetary gear dynamic mixer.

S3, carrying out pre-polycondensation reaction on the functional polyester oligomer prepared in the step S2 to obtain a functional polyester prepolymer. The pre-polycondensation reaction system consists of a vertical pre-polycondensation reaction kettle, wherein the reactant temperature of the pre-polycondensation reaction kettle is 270 ℃. When the intrinsic viscosity of the functional polyester prepolymer reaches 0.18dL/g, the functional polyester prepolymer is continuously and stably extracted from the pre-polycondensation reaction kettle through a prepolymer pump and is conveyed to a final polycondensation system for final polycondensation reaction. The final polycondensation system consists of a horizontal final polycondensation reaction kettle and a horizontal liquid phase tackifying kettle, wherein the reaction temperature of the final polycondensation reaction kettle is 275 ℃, and the temperature of the liquid phase tackifying reaction kettle is 285 ℃.

When the intrinsic viscosity of the functional polyester tackifying compound reaches 0.78dL/g, the functional polyester tackifying melt is directly conveyed to a spinning position through a melt pipeline for spinning to prepare the far infrared flame-retardant polyester fiber with the flame-retardant copolyester as the matrix, wherein the filter pressing value FPFPV of the functional polyester is 0.039 bar/g. The far infrared flame-retardant polyester fiber has the filament number of 1.54dtex, the breaking strength of 3.8cN/dtex and the elongation at break of 35 percent.

Comparative example 1

The polyester melt with the intrinsic viscosity of 0.67dL/g is continuously and stably extracted from the final polycondensation reaction kettle at the flow rate of 225kg/h through a melt discharge pump and conveyed to a dynamic mixer through a melt pipeline. The functional master batch melt with the carbon black concentration of 30 wt% is injected into a dynamic mixer through a single screw extruder at the flow rate of 25 kg/h. And (3) uniformly mixing the polyester melt and the functional master batch melt by a dynamic mixer to obtain a functional polyester melt, and directly conveying the functional polyester melt to a spinning position for spinning through a melt pipeline to obtain the stock solution colored black polyester fiber, wherein the filter pressing value FPFPFPV of the functional polyester is 0.363 bar/g.

The dope-dyed black polyester fiber had a single-fiber fineness of 0.58dtex, a breaking strength of 2.2cN/dtex, and an elongation at break of 17%.

Experimental example 1

The functional polyester and the functional fiber products prepared in the above examples 1 to 18 and comparative example 1 were subjected to the related performance test, and the related performance of the test was as follows:

(1) average particle size (mum) of functional powder in functional polyester oligomer, test method: dissolving functional polyester oligomer in good solvent hexafluoroisopropanol, and then testing the particle size of functional powder by using a dynamic light scattering particle size analyzer;

(2) hydroxyl value (mgKOH/g) of functional polyester oligomer, test method: reference HG/T2709-95;

(3) functional polyester intrinsic viscosity (dL/g), test method: refer to GB/T14190-.

(4) Functional polyester filter pressure value fpfpfpv (bar/g), defined as the increase in pressure per gram of functional powder, test method: comprises a single screw extruder with the length-diameter ratio of phi 25mm multiplied by 25D, a melt metering pump with the volume of 1.2cc, a melt pressure sensor and a filter screen with the area S of 3.8cm²The four layers of combined filter screens of 60-100-; the filter pressing performance test process conditions are as follows: the melt temperature is 295 ℃, the pressure set value before the melt metering pump is 6.5MPa, and the metering flow of the melt metering pump is 38 g/min; 500g of polyester polyethylene terephthalate is extruded out from a filter pressing performance tester, and the balance pressure is recorded as the initial pressure P_sThen, 4000g of functional polyester is extruded out of the filter-pressing performance tester, 500g of polyester polyethylene terephthalate is extruded out of the filter-pressing performance tester, and the balance pressure is recorded as the termination pressure P_tAnd finally according to the formula FPFPFPV ═ P_t-P_s)/m_cCalculating to obtain a filter pressing value FPFPV, wherein in the formula, the FPFPV is the filter pressing value and has the unit of bar/g; p_sIs the initial pressure in bar; p_tFor the end pressure, the unit is bar; m is_cThe unit of the mass of the functional powder in the test sample is g.

(5) The linear density (dtex) of the functional polyester fiber is tested by the following method: reference GB/T14343-;

(6) the functional polyester fiber breaking strength (cN/dtex) is tested by the following method: reference GB/T14344-2008;

(7) functional polyester fiber elongation at break (%), test method: refer to GB/T14344-.

The results of the above tests for each property are shown in tables 1 and 2.

TABLE 1

TABLE 2

As can be seen from the data in tables 1 and 2, the filter pressing values FPFPFPV of the functional polyester prepared by the functional polyester production method are not higher than 0.2bar/g, and compared with the functional polyester prepared by the master batch method, the functional polyester prepared by the functional polyester production method has lower filter pressing values, and the functional polyester prepared by the functional polyester production method has higher dispersion uniformity of functional powder.

The addition amount of the carbon black used for preparing the functional polyester in the inventive example 1 and the comparative example 1 is the same, however, the carbon black in the example 1 is added to the polyester oligomer in the form of the continuously prepared functional powder condensation compound and then subjected to polycondensation reaction to obtain the functional polyester, and the carbon black in the comparative example 1 is added to the polyester melt prepared in the final polycondensation reaction in the form of the master batch to obtain the functional polyester. In the method of comparative example 1, when the functional polyester is prepared, the functional powder is difficult to highly and uniformly disperse in the high-viscosity polyester melt, and the spinning performance of the prepared functional polyester melt is poor.

The functional powder in the functional powder slurry realizes superfine dispersion in a dihydric alcohol carrier. Injecting the functional powder slurry into an ultrasonic reaction kettle which is accurately controlled step by step, realizing the rapid dispersion of the functional powder in the low-viscosity polyester oligomer through the synergy of the strong cavitation effect of ultrasonic waves and the mechanical stirring shearing effect, and then evaporating and removing excessive dihydric alcohol which is used as a slurry carrier and enters the reaction kettle by adjusting the reaction temperature of each chamber of the ultrasonic reaction kettle which is accurately controlled step by step to prepare the functional polyester oligomer with small dispersed particle size of the functional powder. The functional polyester can realize highly uniform dispersion of carbon black in a polyester matrix and effectively reduce agglomeration of carbon black particles in the preparation process of the functional polyester.

The filter pressing value FPFPFPV of the functional polyester in the example 1 is 0.028bar/g, the filter pressing value FPV of the functional polyester in the comparative example 1 is 0.0363bar/g, the carbon black is more uniformly dispersed in the example 1, and the filter pressing value of the functional polyester is lower, so that the prepared functional polyester fiber has more uniform structure and more excellent mechanical property, for example, the functional polyester fiber prepared in the example 1 has the breaking strength of 3.2cN/dtex, and the functional polyester fiber prepared in the comparative example 1 has the breaking strength of only 2.2cN/dtex, wherein the functional polyester fiber is prepared by adopting the same carbon black adding amount to prepare the functional polyester fiber with the same linear density.

Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.