阅读说明：本技术 一种原位聚合着色石墨烯改性聚酰胺-6切片的生产装置及工艺 (Production device and process for in-situ polymerization coloring graphene modified polyamide-6 slice ) 是由 封其都 陈建新 陈亮 严栋 王冬晟 于 2021-01-28 设计创作，主要内容包括：本发明公开了一种原位聚合着色石墨烯改性聚酰胺-6切片的生产装置及工艺,包括：原料储罐、静态混合器、精对苯二甲酸配制罐、改性剂配制罐、石墨烯配制罐、着色剂配制罐,动态混合器等；本发明采用原位聚合的方法直接制得石墨烯改性聚酰胺-6有色切片,制得的切片可直接纺丝而得到客户所需要的功能型色丝,由于着色剂的粒径为纳米级,所以使得纺丝组件使用周期延长,一般能使用3-6个月,从而大大降低了纺丝的生产成本,通过加入经过处理的石墨烯后使得聚酰胺着色切片具有了抗菌、强度高、远红外等多种功能。(The invention discloses a device and a process for producing in-situ polymerized colored graphene modified polyamide-6 slices, which comprise the following steps: a raw material storage tank, a static mixer, a purified terephthalic acid preparation tank, a modifier preparation tank, a graphene preparation tank, a colorant preparation tank, a dynamic mixer and the like; the graphene modified polyamide-6 colored chip is directly prepared by adopting an in-situ polymerization method, the prepared chip can be directly spun to obtain functional colored filaments required by customers, the service life of a spinning component is prolonged due to the nanoscale particle size of the colorant, the spinning component can be generally used for 3-6 months, the production cost of spinning is greatly reduced, and the polyamide colored chip has multiple functions of antibiosis, high strength, far infrared and the like after the treated graphene is added.)

1. The utility model provides a production device of in situ polymerization colouring graphite alkene modified polyamide-6 section, includes raw materials storage tank (1), its characterized in that: the device is characterized by further comprising a preparation system, a reaction system and a mixing bin (18), wherein the raw material storage tank (1), the preparation system, the reaction system and the mixing bin (18) are communicated in sequence.

2. The in-situ polymerization production device for the colored graphene modified polyamide-6 chip as claimed in claim 1, wherein: the preparation system comprises a refined terephthalic acid preparation tank (3), a modifier preparation tank (4), a graphene preparation tank (5) and a colorant preparation tank (6), wherein the bottoms of the refined terephthalic acid preparation tank (3), the modifier preparation tank (4), the graphene preparation tank (5) and the colorant preparation tank (6) are communicated with a static mixer (2), and the static mixer (2) is communicated with a dynamic mixer (7).

3. The in-situ polymerization production device for the colored graphene modified polyamide-6 chip as claimed in claim 1, wherein: the reaction system comprises a front pressurizing polymerizer (8), a rear polymerizing reactor (9), a casting belt underwater pelletizing system (10), a pre-extraction water tank (11), an extraction tower (12), a drying tower (13) and a mixing bin (14), wherein the static mixer (2) is arranged on the dynamic mixer (7), the front pressurizing polymerizer (8) is arranged on the rear polymerizing reactor (9), the casting belt underwater pelletizing system (10), the pre-extraction water tank (11), the extraction tower (12), the drying tower (13) and the mixing bin (14) are sequentially communicated.

4. A production process of in-situ polymerized colored graphene modified polyamide-6 slices is characterized by comprising the following steps: the method comprises the following steps:

step 1: firstly, dissolving and mixing purified terephthalic acid and caprolactam in a purified terephthalic acid preparation tank (3) according to a certain proportion;

step 2: dissolving and mixing a modifier and caprolactam in a modifier preparation tank (4) according to a certain proportion;

and step 3: dispersing, grinding and mixing water, caprolactam, graphene and a graphene dispersion viscosity reducer in a graphene preparation tank (5) according to a certain proportion;

and 4, step 4: dispersing, grinding and mixing water, caprolactam, a coloring agent and a coloring agent dispersing agent in a coloring agent preparation tank (6) according to a certain proportion;

and 5: the caprolactam liquid in the raw material storage tank (1) is quantitatively pumped into a static mixer (2) through a pump, a pneumatic regulating valve and a mass flow meter, the caprolactam raw material liquid and the solution in each preparation tank pass through the static mixer (2) according to a certain proportion and are pumped into a dynamic mixer (7), and the caprolactam raw material liquid and the solution in each preparation tank are mixed by the dynamic mixer (7) and then are pumped into a front pressurizing polymerizer (8);

step 6: carrying out in-situ polymerization on the mixed solution, firstly carrying out hydrolytic ring opening and preliminary addition polymerization reaction by a front pressure polymerizer (8), wherein the temperature is 270-300 ℃, the pressure is 0.1-1.2 Mpa, stirring the mixed solution by a stirrer at the top of the front pressure polymerizer (8), preventing the coloring agent and the graphene from generating an agglomeration reaction, simultaneously further uniformly mixing the coloring agent, the graphene and caprolactam, conveying the generated initial polymer into a rear polymerization reactor (9) for addition polymerization and chain balance reaction, and carrying out normal pressure or micro negative pressure on the rear polymerization reactor (9) at the upper section of 270-300 ℃, at the lower section of 245-260 ℃ to generate a polyamide-6 polymer melt;

and 7: carrying out belt casting underwater pelletizing on the polyamide-6 polymer melt to obtain initial polyamide-6 graphene colored chips through a belt casting underwater pelletizing system (10);

and 8: putting the initial polyamide-6 graphene colored chips into a pre-extraction water tank (11), performing pre-extraction treatment by using water, conveying the treated initial polyamide-6 graphene chips and pre-extraction water into an extraction tower (12) through a slurry pump together for extraction, extracting the initial polyamide-6 graphene colored chips containing monomers and oligomers in the extraction tower (12) by using extraction water in countercurrent contact with the initial polyamide-6 graphene colored chips, wherein the temperature of the extraction water is 95-125 ℃, so as to obtain the extracted polyamide-6 graphene colored chips, and discharging the extraction water containing the monomers and the oligomers into the pre-extraction water tank from the top of the extraction tower;

and step 9: dehydrating the extracted polyamide-6 graphene colored slices, and then circularly drying in a drying tower (13) by using nitrogen to obtain polyamide-6 graphene colored dry slices; finally, the mixture is conveyed into a mixing bin (14) through nitrogen.

5. The production process of the in-situ polymerized colored graphene modified polyamide-6 chip as claimed in claim 4, wherein: in the steps 1 to 8: 100 parts of caprolactam, 2-25 parts of water, 0.05-0.5 part of purified terephthalic acid, 0.1-0.2 part of modifier, 0.8-28 parts of colorant, 0.16-5.6 parts of colorant dispersant, 0.1-2 parts of graphene and 0.0002-0.004 part of graphene dispersion viscosity reducer.

6. The production process of the in-situ polymerized colored graphene modified polyamide-6 chip as claimed in claim 4, wherein: in the step 4: the particle size of the colorant is 100-300 nanometers.

7. The production process of the in-situ polymerized colored graphene modified polyamide-6 chip as claimed in claim 4, wherein: in the step 3: the particle size of the graphene is 600-900 nanometers.

8. The production process of the in-situ polymerized colored graphene modified polyamide-6 chip as claimed in claim 4, wherein: in the step 6: the molecular weight of the initial polymer is 8800-10000, and the molecular weight of the polyamide-6 polymer melt is 9800-15100.

9. The production process of the in-situ polymerized colored graphene modified polyamide-6 chip as claimed in claim 4, wherein: in the step 8: the viscosity of the in-situ polymerized colored graphene modified polyamide-6 slice is 2.0-2.8.

Technical Field

The invention relates to the technical field of polyamide-6 slice preparation, in particular to a device and a process for producing in-situ polymerized and colored graphene modified polyamide-6 slices.

Background

The polyamide has excellent comprehensive properties of excellent electrical insulation performance, good alkali resistance and corrosion resistance, excellent mechanical properties, easy forming and processing and the like. The color yarn manufactured at home and abroad at present is mainly prepared by blending polyamide chips and color master batches before spinning and then spinning to obtain the color yarn, or by spinning the polyamide chips and then dyeing and finishing through the subsequent procedures. However, the problems and disadvantages of these two conventional manufacturing methods are as follows:

1. the addition of the coloring agent in the color master batch has micron-sized grain diameter, so that the spinning assembly has short period and poor spinnability, and is easy to float and break.

2. The blending uniformity of the color master batches is poor, and the spun silk has color difference.

3. In the dyeing and finishing process, a large amount of water and dye are needed, and waste water with extremely high chemical oxygen demand is discharged, so that the dyeing and finishing process has great pollution.

In the invention, the in-situ polymerization coloring is carried out by adding the caprolactam and the in-situ polymerization coloring into a polymerization kettle for polymerization reaction before polymerization reaction, thus solving the problems of the two traditional methods and ensuring the color fastness of the prepared slices to be high. In addition, the polyamide colored slice has multiple functions of antibiosis, high strength, far infrared and the like after the processed graphene is added.

Disclosure of Invention

The invention aims to provide a production device and a production process for in-situ polymerization coloring graphene modified polyamide-6 slices, the prepared slices have high color fastness, spun yarns have uniform color and luster, no color difference and high color fastness, and the polyamide coloring slices have multiple functions of antibiosis, high strength, far infrared and the like after the processed graphene is added, so that the problems in the background technology are solved.

In order to achieve the purpose, the invention provides the following technical scheme: the production device for the in-situ polymerization coloring graphene modified polyamide-6 slices comprises a raw material storage tank, a preparation system, a reaction system and a mixing bin, wherein the raw material storage tank, the preparation system, the reaction system and the mixing bin are communicated in sequence.

The preparation system comprises a purified terephthalic acid preparation tank, a modifier preparation tank, a graphene preparation tank and a colorant preparation tank, wherein the bottoms of the purified terephthalic acid preparation tank, the modifier preparation tank, the graphene preparation tank and the colorant preparation tank are communicated with a static mixer, and the static mixer is communicated with a dynamic mixer.

The reaction system comprises a front pressurizing polymerizer, a rear polymerizing reactor, a casting belt underwater pelletizing system, a pre-extraction water tank, an extraction tower, a drying tower and a mixing bin, wherein the static mixer, the dynamic mixer, the front pressurizing polymerizer, the rear polymerizing reactor, the casting belt underwater pelletizing system, the pre-extraction water tank, the extraction tower, the drying tower and the mixing bin are sequentially communicated.

A production process of in-situ polymerized colored graphene modified polyamide-6 slices comprises the following steps:

step 1: firstly, dissolving and mixing purified terephthalic acid and caprolactam in a purified terephthalic acid preparation tank according to a certain proportion;

step 2: dissolving and mixing a modifier and caprolactam in a modifier preparation tank according to a certain proportion;

and step 3: dispersing, grinding and mixing water, caprolactam, graphene and a graphene dispersion viscosity reducer in a graphene preparation tank according to a certain proportion;

and 4, step 4: dispersing, grinding and mixing water, caprolactam, a coloring agent and a coloring agent dispersing agent in a coloring agent preparation tank according to a certain proportion;

and 5: the caprolactam liquid in the raw material storage tank is quantitatively pumped into a static mixer through a pump, a starting regulating valve and a mass flow meter, the caprolactam raw material liquid and the solution in each preparation tank are pumped into a dynamic mixer through the static mixer according to a certain proportion, and the caprolactam raw material liquid and the solution in each preparation tank are mixed by the dynamic mixer and then pumped into a front pressurizing polymerizer;

step 6: carrying out in-situ polymerization on the mixed solution, firstly carrying out hydrolytic ring opening and preliminary polyaddition reaction by a front pressure polymerizer at the temperature of 270-300 ℃ and the pressure of 0.1-1.2 Mpa, stirring the mixed solution by a stirrer at the top of the front pressure polymerizer to prevent the aggregation reaction of the coloring agent and the graphene, simultaneously further uniformly mixing the pigment, the graphene and the caprolactam, conveying the generated initial polymer into a rear polymerization reactor for polyaddition and chain balance reaction, and carrying out normal pressure or micro negative pressure on the rear polymerization reactor 9 at the temperature of 270-300 ℃ at the upper section and 245-260 ℃ at the lower section to generate a polyamide-6 polymer melt;

and 7: carrying out belt casting underwater pelletizing on the polyamide-6 polymer melt to obtain initial polyamide-6 graphene colored chips;

and 8: putting the initial polyamide-6 graphene colored chips into a pre-extraction water tank, performing pre-extraction treatment by using water, conveying the treated initial polyamide-6 graphene chips and pre-extraction water into an extraction tower through a slurry pump for extraction, extracting the initial polyamide-6 graphene colored chips containing monomers and oligomers in the extraction tower by using extraction water in countercurrent contact with the initial polyamide-6 graphene colored chips to obtain extracted polyamide-6 graphene colored chips, and discharging the extraction water containing the monomers and the oligomers into the pre-extraction water tank from the top of the extraction tower;

and step 9: dehydrating the extracted polyamide-6 graphene colored slices, and then circularly drying in a drying tower by using nitrogen to obtain polyamide-6 graphene colored dry slices; and finally conveying the mixture to a mixing bin through nitrogen.

Wherein, in the step 1 to the step 8: 100 parts of caprolactam, 2-25 parts of water, 0.05-0.5 part of purified terephthalic acid, 0.1-0.2 part of modifier, 0.8-28 parts of colorant, 0.16-5.6 parts of colorant dispersant, 0.1-2 parts of graphene and 0.0002-0.004 part of graphene dispersion viscosity reducer.

Wherein, in the step 4: the particle size of the colorant is 100-300 nanometers.

Wherein, in the step 3: the particle size of the graphene is 600-900 nanometers.

Wherein, in the step 6: the molecular weight of the initial polymer is 8800-10000, and the molecular weight of the polyamide-6 polymer melt is 9800-15100.

Wherein, in the step 8: the viscosity of the in-situ polymerized colored graphene modified polyamide-6 slice is 2.0-2.8.

Compared with the prior art, the invention has the following beneficial effects: the in-situ polymerization colored graphene modified polyamide-6 slice is directly prepared by adopting an in-situ polymerization method, the prepared slice can be directly spun to obtain functional color silk required by customers, and the product has the following advantages:

1. the colorant and graphene are highly milled, dispersed, and a dispersant is employed to prevent re-agglomeration of the colorant. The grain size of the colorant is controlled to be 100-300 nanometers, and the grain size of the graphene is 600-900 nanometers.

2. The graphene dispersion viscosity reducer and the colorant dispersant used in the product are high temperature resistant, do not participate in polymerization reaction, do not influence subsequent spinning procedures, and have good spinnability.

3. Because the grain diameter of the coloring agent and the grain diameter of the graphene are both nano-scale, the service cycle of the spinning assembly is prolonged, and the spinning assembly can be used for 3-6 months generally, so that the production cost of spinning is greatly reduced.

4. The color of the silk spun by the colored slice is uniform and has no color difference.

5. Solves the problems of spinning by using bright slices and re-dyeing in the subsequent process, thereby solving the environmental protection problem and having no pollution.

6. The product has high color fastness.

7. The polyamide slice has multiple functions of antibiosis, high strength, far infrared and the like.

Drawings

FIG. 1 is a schematic view of the structure of a production apparatus of the present invention.

In the figure: 1. a raw material storage tank; 2. a static mixer; 3. a purified terephthalic acid preparation tank; 4. a modifier preparation tank; 5. preparing a graphene preparation tank; 6. a colorant preparation tank; 7. a dynamic mixer; 8. a pre-pressure polymerizer; 9. a post-polymerization reactor; 10. a belt casting underwater pelletizing system; 11. a pre-extraction water tank; 12. an extraction tower; 13. a drying tower; 14. a mixing bunker.

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.

Referring to fig. 1, the present invention provides a technical solution: the production device for the in-situ polymerization coloring graphene modified polyamide-6 slices comprises a raw material storage tank 1, a preparation system, a reaction system and a mixing bin 14, wherein the raw material storage tank 1, the preparation system, the reaction system and the mixing bin 14 are sequentially communicated.

The preparation system comprises a purified terephthalic acid preparation tank 3, a modifier preparation tank 4, a graphene preparation tank 5 and a colorant preparation tank 6, wherein the bottoms of the purified terephthalic acid preparation tank 3, the modifier preparation tank 4, the graphene preparation tank 5 and the colorant preparation tank 6 are communicated with a static mixer 2, and the static mixer 2 is communicated with a dynamic mixer 7.

The reaction system comprises a front pressurizing polymerizer 8, a rear polymerizing reactor 9, a casting belt underwater pelletizing system 10, a pre-extraction water tank 11, an extraction tower 12, a drying tower 13 and a mixing bin 14, wherein the static mixer 2, the dynamic mixer 7, the front pressurizing polymerizer 8, the rear polymerizing reactor 9, the casting belt underwater pelletizing system 10, the pre-extraction water tank 11, the extraction tower 12, the drying tower 13 and the mixing bin 14 are sequentially communicated. Wherein the front pressure polymerizer 8 has a stirrer at the top for stirring.

A production process of in-situ polymerized colored graphene modified polyamide-6 slices comprises the following steps:

step 1: firstly, dissolving and mixing purified terephthalic acid and caprolactam in a purified terephthalic acid preparation tank 3 according to a certain proportion;

step 2: dissolving and mixing a modifier and caprolactam in a modifier preparation tank 4 according to a certain proportion;

and step 3: dispersing, grinding and mixing water, caprolactam, graphene and a graphene dispersion viscosity reducer in a graphene preparation tank 5 according to a certain proportion;

and 4, step 4: dispersing, grinding and mixing water, caprolactam, a coloring agent and a coloring agent dispersing agent in a coloring agent preparation tank 6 according to a certain proportion;

and 5: the caprolactam liquid in the raw material storage tank 1 is quantitatively pumped into the static mixer 2 through a pump, a starting regulating valve and a mass flow meter, the caprolactam raw material liquid and the solution in each preparation tank pass through the static mixer 2 according to a certain proportion, are pumped into the dynamic mixer 7, are mixed by the dynamic mixer 7 and are pumped into the front pressurizing polymerizer 8;

step 6: carrying out in-situ polymerization on the mixed solution, firstly carrying out hydrolytic ring opening and preliminary addition polymerization reaction by a front pressure polymerizer 8 at the temperature of 270-300 ℃ and the pressure of 0.1-1.2 Mpa, stirring the mixed solution by a stirrer at the top of the front pressure polymerizer 8 to prevent the colorant and the graphene from generating an agglomeration reaction, simultaneously further uniformly mixing the colorant, the graphene and caprolactam, conveying the generated initial-stage polymer into a rear polymerization reactor 9 to carry out addition polymerization and chain equilibrium reaction, and generating a polyamide-6 polymer melt by the rear polymerization reactor 9 at the temperature of 270-300 ℃ at the upper section and 245-260 ℃ at the lower section and under normal pressure or micro negative pressure;

and 7: the polyamide-6 polymer melt is processed by a casting belt underwater pelletizing system 10 to obtain initial polyamide-6 graphene colored chips;

and 8: putting the initial polyamide-6 graphene colored chips into a pre-extraction water tank 11, performing pre-extraction treatment by using water, conveying the treated initial polyamide-6 graphene chips and pre-extraction water into an extraction tower 12 through a slurry pump for extraction, extracting the initial polyamide-6 graphene colored chips containing monomers and oligomers in the extraction tower 12 by using extraction water in countercurrent contact with the initial polyamide-6 graphene colored chips, wherein the extraction water temperature is 90-120 ℃, so as to obtain the extracted polyamide-6 graphene colored chips, and discharging the extraction water containing the monomers and the oligomers from the top of the extraction tower into the pre-extraction water tank;

and step 9: dehydrating the extracted polyamide-6 graphene colored slices, and then circularly drying in a drying tower by using nitrogen to obtain polyamide-6 graphene colored dry slices; and finally conveying the mixture to a mixing bin through nitrogen.

Wherein, in the step 1 to the step 8: 100 parts of caprolactam, 2-25 parts of water, 0.05-0.5 part of purified terephthalic acid, 0.1-0.2 part of modifier, 0.8-28 parts of colorant, 0.16-5.6 parts of colorant dispersant, 0.1-2 parts of graphene and 0.0002-0.004 part of graphene dispersion viscosity reducer.

Wherein, in the step 4: the particle size of the colorant is 100-300 nanometers.

Wherein, in the step 3: the particle size of the graphene is 600-900 nanometers.

Wherein, in the step 6: the molecular weight of the initial polymer is 8800-10000, and the molecular weight of the polyamide-6 polymer melt is 9800-15100.

Wherein, in the step 8: the viscosity of the in-situ polymerized colored graphene modified polyamide-6 slice is 2.0-2.8.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.