阅读说明：本技术 一种聚醚醚酮细纱的制备方法及聚醚醚酮细纱 (Preparation method of polyether-ether-ketone spun yarn and polyether-ether-ketone spun yarn ) 是由 吴镝 于 2021-08-16 设计创作，主要内容包括：本发明提供了一种聚醚醚酮细纱的制备方法及聚醚醚酮细纱,其中,所述聚醚醚酮细纱的制备方法包括步骤：将制备好的混合料放入长径比大于或等于40的双螺杆挤出机中进行挤出共混、挤出以及拉伸,从而得到粗纱；所述混合料的组分包括：熔指为10～35g/10min的98份至102份的聚醚醚酮树脂、3份至12份的增强填料以及辅助剂；将所述粗纱在150℃至280℃的条件下进行二次热拉伸,从而得到细纱；所述二次热拉伸的长度为所述粗纱的1倍至3倍。本发明解决了聚醚醚酮细纱在加工过程中不仅容易出现机械力造成的纤维断裂、还容易出现毛丝及断头的现象、并需要降低剪切粘度的问题。(The invention provides a preparation method of polyether-ether-ketone spun yarn and the polyether-ether-ketone spun yarn, wherein the preparation method of the polyether-ether-ketone spun yarn comprises the following steps: putting the prepared mixture into a double-screw extruder with the length-diameter ratio of more than or equal to 40 for extrusion blending, extrusion and stretching, thereby obtaining rough yarns; the components of the mixture comprise: the melt index is 98 to 102 parts of polyether-ether-ketone resin, 3 to 12 parts of reinforcing filler and auxiliary agent, and the weight is 10 to 35g/10 min; carrying out secondary hot stretching on the rough yarn at the temperature of 150-280 ℃ to obtain a spun yarn; the length of the secondary hot stretching is 1 to 3 times that of the roving. The invention solves the problems that the PEEK spun yarn is easy to have fiber breakage caused by mechanical force, broken filaments and broken ends and needs to reduce the shearing viscosity in the processing process.)

1. A preparation method of polyether-ether-ketone spun yarn is characterized by comprising the following steps:

putting the prepared mixture into a double-screw extruder with the length-diameter ratio of more than or equal to 40 for extrusion blending, extrusion and stretching, thereby obtaining rough yarns; the components of the mixture comprise: the melt index is 98 to 102 parts of polyether-ether-ketone resin, 3 to 12 parts of reinforcing filler and auxiliary agent, and the weight is 10 to 35g/10 min;

carrying out secondary hot stretching on the rough yarn at the temperature of 150-280 ℃ to obtain a spun yarn; the length of the secondary hot stretching is 1 to 3 times that of the roving.

2. The method of preparing a polyetheretherketone yarn according to claim 1 wherein the extruder is divided into 9 heating zones, wherein the 8 th heating zone is equipped with a vacuum devolatilization device having a vacuum of 0.03Mpa to 0.07 Mpa; the length-diameter ratio of a spray hole of a spinneret plate in the extruder is 3: 1; the primary draw ratio of the crude fiber is 8 to 12; the roving has a linear density of 220dtex to 250 dtex.

3. The method of making a polyetheretherketone yarn of claim 1 wherein the spun yarn is drawn from the roving by at least 2 hot roll pulls and multiple pulls.

4. The method of preparing a polyetheretherketone yarn according to claim 2 wherein the 9 segments have a temperature of 280 ± 1.5 ℃, 320 ± 1.5 ℃, 350 ± 1.5 ℃, 365 ± 1.5 ℃, 375 ± 1.5 ℃, 380 ± 1.5 ℃ in sequence.

5. The process for the preparation of yarns of polyetheretherketone according to any of claims 1 to 4 wherein the adjuvant is between 3 and 12 parts of diphenylsulfone.

6. The process for the preparation of yarns of polyetheretherketone according to any of claims 1 to 4 wherein the adjuvant is 2.8 to 3.2 parts WakePELLET S lubricity aid.

7. The method of preparing a polyetheretherketone yarn according to any of claims 1 to 3 wherein the adjuvant is dibenzothiophene in an amount of 2.8 to 3.2 parts.

8. The process for preparing a polyetheretherketone yarn according to any of claims 1 to 3 wherein the adjuvant is 2.8 to 3.2 parts of triphenylphosphine.

9. The method for preparing polyetheretherketone spun yarn according to any of claims 1 to 4, further comprising the steps after obtaining the spun yarn: and detecting the breaking strength, the breaking elongation and the surface resistance of the spun yarn.

10. Polyether ether ketone spun yarn produced by the method for producing polyether ether ketone spun yarn according to any one of claims 1 to 9.

Technical Field

The invention belongs to the technical field of polyether-ether-ketone spinning, and particularly relates to a preparation method of polyether-ether-ketone spun yarns and the polyether-ether-ketone spun yarns.

Background

The polyether-ether-ketone fiber is a thermoplastic fiber with a molecular main chain containing phenylene ether-ketone chain links, and because the molecular chain of the polyether-ether-ketone contains rigid benzene rings, flexible ether bonds and carbonyl groups for improving intermolecular force, and the molecular chain segment structure is regular, the polyether-ether-ketone fiber has excellent performances of high temperature resistance, good flame retardance, solvent resistance, good wear resistance and insulation, radiation resistance and the like.

With the intensive research on the spinning process, the spinning equipment and the fiber performance of the polyether-ether-ketone fiber, the polyether-ether-ketone spinning gradually matures in industrial production, and the traditional polyether-ether-ketone spinning is mainly formed by uniformly mixing polyether-ether-ketone and a reinforcing filler and then carrying out corresponding process treatment.

In the traditional polyether-ether-ketone spinning, the material viscosity of polyether-ether-ketone is high at the processing temperature, and the dispersion effect of the reinforcing filler in polyether-ether-ketone is poor, so that the problems of fiber breakage caused by mechanical force, broken filaments and broken ends easily occurring in the processing process and the need of reducing the shear viscosity are solved.

Disclosure of Invention

The technical problem to be solved by the invention is how to provide a preparation method of a polyether-ether-ketone spun yarn, so as to solve the problems that the traditional polyether-ether-ketone spun yarn is easy to cause fiber breakage caused by mechanical force in the processing process, the phenomena of broken filaments and broken ends are easy to occur, and the shearing viscosity needs to be reduced.

In order to solve the technical problem, the invention provides a preparation method of polyether-ether-ketone spun yarn, which comprises the following steps:

putting the prepared mixture into a double-screw extruder with the length-diameter ratio of more than or equal to 40 for extrusion blending, extrusion and stretching, thereby obtaining rough yarns; the components of the mixture comprise: the melt index is 98 to 102 parts of polyether-ether-ketone resin, 3 to 12 parts of reinforcing filler and auxiliary agent, and the weight is 10 to 35g/10 min;

carrying out secondary hot stretching on the rough yarn at the temperature of 150-280 ℃ to obtain a spun yarn; the length of the secondary hot stretching is 1 to 3 times that of the roving.

Further, the extruder is divided into 9 heating sections, wherein the 8 th heating section is provided with a vacuum devolatilization device with the vacuum degree of 0.03MPa to 0.07 MPa; the length-diameter ratio of a spray hole of a spinneret plate in the extruder is 3: 1; the primary draw ratio of the crude fiber is 8 to 12; the roving has a linear density of 220dtex to 250 dtex.

Further, the spun yarn is obtained by drawing the roving through at least 2 groups of hot rollers and drawing and stretching for multiple times.

Further, the temperature of the 9 segments is 280 + -1.5 ℃, 320 + -1.5 ℃, 350 + -1.5 ℃, 365 + -1.5 ℃, 375 + -1.5 ℃, 380 + -1.5 ℃ and 380 + -1.5 ℃ in sequence.

Still further, the adjuvant is 3 to 12 parts of diphenyl sulfone.

Further, the adjuvant is 2.8 parts to 3.2 parts watt-gramsPELLET S lubricity aid.

Further, the adjuvant is dibenzothiophene in an amount of 2.8 parts to 3.2 parts.

Still further, the adjuvant is 2.8 parts to 3.2 parts of triphenylphosphine.

Further, the method further comprises the following steps after the spun yarn is obtained: and detecting the breaking strength, the breaking elongation and the surface resistance of the spun yarn.

The invention also provides the polyether-ether-ketone spun yarn prepared by the preparation method.

Compared with the prior art, the prepared mixture is firstly put into a double-screw extruder with the length-diameter ratio of more than or equal to 40 for blending, extruding and stretching, so that the roving is obtained; and the components defining the mix include: the melt index is 98 to 102 parts of polyether-ether-ketone resin, 3 to 12 parts of reinforcing filler and auxiliary agent, and the weight is 10 to 35g/10 min; finally, performing secondary hot stretching on the roving at the temperature of 150-280 ℃, namely performing traction and stretching for multiple times through at least 2 groups of hot rollers to obtain spun yarn; wherein the length of the secondary hot drawing is 1 to 3 times that of the roving. Therefore, the viscosity of the material can be reduced at the processing temperature of the polyether-ether-ketone, and the dispersion effect of the reinforcing filler in the polyether-ether-ketone is improved, so that the problems that the fiber is easy to break due to mechanical force, broken filaments and broken ends are easy to occur in the processing process, and the shearing viscosity needs to be reduced are solved.

Drawings

In order to make the content of the invention clearer, the drawings needed to be used in the description of the embodiments will be briefly described below, it being clear that the drawings in the following description are only some embodiments of the invention, and that other drawings can be derived by a person skilled in the art without inventive effort, wherein:

fig. 1 is a schematic flow step diagram of a preparation method of a polyetheretherketone spun yarn provided by an embodiment of the present invention.

Fig. 2 is a schematic flow step diagram of another preparation method of polyetheretherketone spun yarn according to an embodiment of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The embodiment of the invention provides a preparation method of polyether-ether-ketone spun yarn, which comprises the following steps as shown in the attached drawing 1:

s101, placing the prepared mixture into a double-screw extruder with the length-diameter ratio of more than or equal to 40 to perform blending, extrusion and stretching, so that the roving is obtained.

Specifically, the components of the mixture comprise: the melt index is 98 to 102 parts of polyether ether ketone resin (also called PEEK resin) with the weight ratio of 10 to 35g/10min, 3 to 12 parts of reinforcing filler (also called CTN) and auxiliary agent, and the parts are parts by weight. Wherein, the share of the parts is selected according to actual requirements.

Specifically, the prepared mixture is formed by uniformly mixing the polyether-ether-ketone resin, the reinforcing filler and the auxiliary agent, and can be mixed by adopting a dry method or a wet method.

Specifically, the adjuvant is 3 to 12 partsOf diphenyl sulfone, 2 to 5 parts of WakeAny one of PELLET S lubricant additive, 2 to 5 parts of dibenzothiophene and 2 to 5 parts of triphenylphosphine. Wherein, the share of the parts is selected according to actual requirements.

In this example, the polyetheretherketone resin is 100 parts, the melt index is 20g/10min, the reinforcing filler is 5 parts, and the auxiliary agent is 10 parts of diphenylsulfone.

In this example, the twin screw extruder has a length to diameter ratio of 40. Of course, 42, 44, 46, etc. may also be selected according to actual requirements.

Specifically, the diameter of the screw in the extruder is 16mm to 22 mm. Of course, according to actual requirements, adaptive adjustment can be performed.

Specifically, the screw speed in the extruder is 148rpm to 152rpm, the feeding rate is 258g/h to 302g/h, the temperature of a melt pump and a die is 370 ℃ to 415 ℃, the flow rate of the melt pump is 258g/h to 300g/h, the specification of a spinneret plate is 12 x 0.5mm spray holes, and the length-diameter ratio of the spray holes is 3: 1. The data of each structure in the extruder can be selected according to actual requirements.

In this example, the screw speed was 150rpm, the feed rate was 290g/h, the melt pump and die temperature was 380 ℃ and the melt pump flow was 290 g/h.

Specifically, the extruder was divided into 9 heating zones, wherein the 8 th heating zone was configured with vacuum devolatilization at a vacuum of 0.03Mpa to 0.07 Mpa. Wherein, the vacuum degree is adjusted according to actual requirements.

Specifically, the temperature of the 9 heating sections is 280 plus or minus 1.5 ℃, 320 plus or minus 1.5 ℃, 350 plus or minus 1.5 ℃, 365 plus or minus 1.5 ℃, 375 plus or minus 1.5 ℃, 380 plus or minus 1.5 ℃ in sequence. Of course, the temperature of each zone can also be adjusted according to different conditions and the selection of the auxiliary agent.

If the adjuvant is diphenyl sulfone or WakeWhen the PELLET S lubricating additive is used, the temperature of the 9 heating sections is 280 ℃, 320 ℃, 350 ℃, 365 ℃, 375 ℃, 380 ℃ and 380 ℃ in sequence. Of course, the temperatures of the 9 heating sections can also be adaptively adjusted according to actual requirements.

If the adjuvant is dibenzothiophene or triphenylphosphine, the temperatures of the 9 heating sections are 280 ℃, 320 ℃, 350 ℃, 375 ℃, 380 ℃ in sequence. Of course, the temperatures of the 9 heating sections can also be adaptively adjusted according to actual requirements.

In this embodiment, the 8 th heating section is provided with a vacuum devolatilizer having a vacuum degree of 0.05 Mpa.

Specifically, after the mixture enters the 9 heating sections to obtain devolatilized materials, the flow rate is stabilized through the melt pump, and then the mixture is stretched through an extruder to obtain the roving.

Specifically, the roving has a primary draw ratio of 8 to 12 and a linear density of 220dtex to 250 dtex. Of course, various data in the roving can be selected according to actual requirements.

In this example, the roving had a primary draw ratio of 10 and a density of 245 dtex.

S102, performing secondary hot stretching on the rough yarn at the temperature of 150-280 ℃ to obtain the spun yarn.

The roving and the spun yarn may be referred to as a fiber.

Specifically, the length of the fine yarn obtained by the secondary hot stretching is 1 to 3 times that of the roving.

Specifically, the spun yarn is obtained by drawing the roving through at least 2 groups of hot rollers and drawing and stretching for multiple times. The number of groups drawn by the hot roller is set according to actual requirements, and the number of times of drawing and stretching is also set according to actual requirements, and is not particularly limited herein.

In this embodiment, the length of the filament yarn is 3 times that of the roving yarn, and of course, the length of the filament yarn may be 1.8 times, 2 times, 2.5 times, 2.9 times, and the like according to actual requirements.

Specifically, the temperature adjustment of the secondary hot stretching can be selected according to actual requirements.

In this example, the secondary hot stretching was performed at 160 ℃; or at 260 ℃.

Further, as shown in fig. 2, after step S102, step S103 may be added, and the step S103 is to detect the breaking strength, the breaking elongation and the surface resistance of the spun yarn. Thereby providing qualified basis for the obtained spun yarn.

Specifically, the integrity of the spun yarn after the secondary hot stretching can be detected, so that a qualified basis can be better provided for the obtained spun yarn.

In the embodiment, the prepared mixture is put into a double-screw extruder with the length-diameter ratio of more than or equal to 40 for blending, extruding and stretching, so that roving is obtained; and the components defining the mix include: the melt index is 98 to 102 parts of polyether-ether-ketone resin, 3 to 12 parts of reinforcing filler and auxiliary agent, and the weight is 10 to 35g/10 min; dividing the extruder into 9 sections, wherein the 8 th section is provided with vacuum devolatilization with the vacuum degree of 0.03MPa to 0.07 MPa; finally, performing secondary hot stretching on the roving at the temperature of 150-280 ℃, namely performing traction and stretching for multiple times through at least 2 groups of hot rollers to obtain spun yarn; wherein the length of the secondary hot drawing is 1 to 3 times that of the roving. Therefore, the viscosity of the material can be reduced at the processing temperature of the polyether-ether-ketone, and the dispersion effect of the reinforcing filler in the polyether-ether-ketone is improved, so that the problems that the fiber is easy to break due to mechanical force, broken filaments and broken ends are easy to occur in the processing process, and the shearing viscosity needs to be reduced are solved.

The invention also provides another embodiment, which provides the polyether-ether-ketone spun yarn prepared by the preparation method of the polyether-ether-ketone spun yarn.

In order to better embody the advantageous effects of the present invention, comparative experiments will be conducted below through four prior art comparative examples and five specific examples of the present invention.

Comparative example 1

Step one, 100 parts of PEEK resin with a melt index of 20g/10min and 10 parts of CTN are uniformly mixed to form a mixture, and then the mixture is put into an extruder to be blended, extruded and stretched to obtain rough yarns, wherein the rotation speed of a screw in the extruder is 150rpm, the feeding rate is 290g/h, the temperature of a melt pump and a die is 380 ℃, the flow rate of the melt pump is 290g/h, the specification of a spinneret plate is 12 x 0.5mm, the extruder is divided into 9 heating zones, the temperatures of the 9 heating zones are respectively 280 ℃, 320 ℃, 350 ℃, 375 ℃, 380 ℃ and 380 ℃, the primary stretching ratio of the rough yarns is 10, and the linear density is 245 dtex.

Step two, carrying out secondary hot stretching on the rough yarn at the temperature of 160 ℃ to obtain spun yarn; the length of the secondary hot stretching is 3 times of that of the roving.

And detecting the breaking strength, the breaking elongation, the surface resistance and the integrity of the secondary hot stretching of the spun yarn.

Comparative example No. two

The CNT part was modified by 5 parts, and the rest of the procedure, process and conditions were the same as in comparative example one.

Comparative example No. three

The CNT part was modified to 2 parts and the remaining steps, processes and conditions were the same as in comparative example one.

Comparative example No. four

The temperature condition of the secondary hot stretching in the second step was modified to 260 ℃, and the remaining steps, processes and conditions were the same as those of the first comparative example.

Example one

Step one, 100 parts of PEEK resin with a melt index of 20g/10min, 5 parts of CTN and 10 parts of diphenyl sulfone are uniformly mixed to form a mixture, and then the mixture is put into an extruder to be extruded, blended, extruded and stretched to obtain the rough yarn, wherein the rotation speed of a screw in the extruder is 150rpm, the feeding rate is 290g/h, the temperature of a melt pump and a die is 380 ℃, the flow rate of the melt pump is 290g/h, the specification of a spinneret plate is 12 x 0.5mm spray holes, the length-diameter ratio of the spray holes is 3:1, the extruder is divided into 9 heating sections, the 8 th heating section is provided with vacuum devolatilization with the vacuum degree of 0.05Mpa, the temperatures of the 9 sections are respectively 280 ℃, 320 ℃, 350 ℃, 365 ℃, 375 ℃, 380 ℃ and 380 ℃, the primary stretching ratio of the rough yarn is 10, and the linear density is 245 dtex.

Step two, carrying out secondary hot stretching on the rough yarn at the temperature of 160 ℃ to obtain spun yarn; the length of the secondary hot stretching is 3 times of that of the roving.

And detecting the breaking strength, the breaking elongation, the surface resistance and the integrity of the secondary hot stretching of the spun yarn.

Example two

The temperature condition of the secondary hot stretching in the second step is modified to 260 ℃, and the rest steps, processes and conditions are the same as those of the first embodiment.

EXAMPLE III

Modifying 10 parts of diphenyl sulfone to 3 parts of wattThe PELLET S lubricant additive, the rest steps, process and conditions are the same as the first embodiment.

Example four

The steps, processes and conditions were the same as in example one except that 10 parts of diphenyl sulfone was changed to 3 parts of dibenzothiophene and the temperatures of the 9 heating zones were changed to 280 ℃, 320 ℃, 350 ℃, 375 ℃, 380 ℃ and 380 ℃.

EXAMPLE five

The same procedures, processes and conditions as in example one were followed except that 10 parts of diphenylsulfone was changed to 3 parts of triphenylphosphine and the temperatures of the 9 heating zones were changed to 280 ℃, 320 ℃, 350 ℃, 375 ℃, 380 ℃ and 380 ℃.

By comparing four prior art comparative examples with five specific examples of the invention, the following comparative tables can be derived:

as can be seen from the comparative table, the five embodiments of the present invention have better effects than the four comparative examples of the prior art in breaking strength, breaking elongation, surface resistance and integrity of the secondary hot-drawn fiber, and therefore, it can be concluded that the spun yarn prepared by the method for preparing polyetheretherketone spun yarn of the present invention has excellent properties compared to the prior art.

The above examples are merely illustrative for clearly illustrating the present invention and are not intended to limit the embodiments; the scope of the present invention includes, but is not limited to, the above embodiments, and all equivalent changes in the shape and structure according to the present invention are included in the scope of the present invention.