CN111440312A - Polycondensation process of chinlon 6 colored chips - Google Patents
Polycondensation process of chinlon 6 colored chips Download PDFInfo
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- CN111440312A CN111440312A CN201911345322.9A CN201911345322A CN111440312A CN 111440312 A CN111440312 A CN 111440312A CN 201911345322 A CN201911345322 A CN 201911345322A CN 111440312 A CN111440312 A CN 111440312A
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- nylon
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- caprolactam
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- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000006068 polycondensation reaction Methods 0.000 title claims abstract description 12
- 229920006052 Chinlon® Polymers 0.000 title claims abstract description 11
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 44
- 238000000605 extraction Methods 0.000 claims abstract description 39
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229920000642 polymer Polymers 0.000 claims abstract description 21
- 239000000049 pigment Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000005266 casting Methods 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- 239000003607 modifier Substances 0.000 claims abstract description 4
- 238000010008 shearing Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000012644 addition polymerization Methods 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims description 5
- 238000007142 ring opening reaction Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000009987 spinning Methods 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 6
- 239000004595 color masterbatch Substances 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/04—Pigments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Polyamides (AREA)
Abstract
The invention discloses a polycondensation process of chinlon 6 colored chips, which comprises the following steps: 1) mixing PTA modifier, water, pigment dispersant and caprolactam solution according to a certain proportion, and carrying out in-situ polymerization on the mixed solution; 2) feeding the polyamide-6 polymer melt into a double-screw extruder, adding a color paste solution, shearing and blending uniformly; 3) carrying out belt casting, underwater grain cutting and sieving on the nylon 6 polymer melt to obtain initial colored nylon 6 slices; 4) extracting the colored nylon-6 slices at the initial stage; 5) evaporating and concentrating the extraction water, recovering caprolactam monomer in the extraction water, dehydrating the colored nylon-6 slices, and circularly drying. The invention adopts a double-screw melt blending method to directly prepare the nylon-6 colored chips, has long service cycle, uniform color, no color difference, environmental protection, no pollution and no damage to the surface of the inner structure of the polymerization tube.
Description
Technical Field
The invention relates to the field of chinlon, in particular to a polycondensation process of chinlon 6 colored chips.
Background
At present, the color yarn manufactured at home and abroad is mainly obtained by blending bright chips and color master batches and then spinning. Or spinning with bright section and dyeing in the next process. The conventional manufacturing method has the following problems and disadvantages:
1. the pigment particle size in the color master batch is larger (more than micron level), so that the service cycle of a spinning assembly is shorter (generally 7-20 days) in the spinning process, and the spinning cost is increased. The particle size greatly affects the spinnability, and the yarn is easy to float and break.
2. Because the bright chips and the color master batches are blended, the mixing is uneven, and the spun silk has color difference.
3. The color silk spun by using the color master batch has insufficient vividness and brightness.
4. The dyeing process produces a large amount of waste water, and about 2 tons of waste water is produced when 1 ton of cloth is dyed.
5. The original polymerization process can mix a large amount of polymer tubes in the product switching process, the switching period is long, and a large amount of waste slices are caused.
Disclosure of Invention
In order to solve the problems, the invention provides a polycondensation process of a chinlon 6 colored slice, which has the advantages of small pigment particle size, long service cycle of a spinning assembly, good brightness, environmental protection, no pollution and no damage to the internal structure of a polymerization tube.
A polycondensation process of a chinlon 6 colored slice comprises the following steps:
s1, dissolving and mixing PTA and caprolactam according to a certain proportion; dissolving and mixing a modifier and caprolactam according to a certain proportion; dispersing, grinding and mixing water, caprolactam, pigment and a pigment dispersing agent according to a certain proportion; feeding the caprolactam raw material liquid and each solution into a double-screw extruder according to a certain proportion through a static mixer to obtain a mixed solution;
s2, 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, and conveying the generated initial polymer into a rear polymerizer for addition polymerization and chain equilibrium reaction to generate a polyamide-6 polymer melt;
s3, feeding the polyamide-6 polymer melt into a double-screw extruder, adding color paste solution in proportion, shearing and blending uniformly; carrying out belt casting, underwater grain cutting and sieving on the nylon 6 polymer melt to obtain initial colored nylon 6 slices;
s4, placing the initial colored nylon-6 chips into a pre-extraction water tank, performing pre-extraction treatment by using water, placing the treated initial colored nylon-6 chips and pre-extraction water into an extraction tower for extraction, extracting the initial colored nylon-6 chips containing monomers and oligomers in the extraction tower by using extraction water in countercurrent contact with the chips to obtain extracted colored nylon-6 chips, and discharging the extraction water containing the monomers and oligomers into the pre-extraction water tank from the top of the extraction tower;
s5, evaporating and concentrating the extraction water in the pre-extraction water tank, and recovering caprolactam monomer in the extraction water; dehydrating the extracted colored nylon-6 slices, and then circularly drying in a drying tower by using nitrogen to obtain colored dry nylon-6 slices.
Further, caprolactam: 100 parts of (A); water: 3-10 parts; PAT: 0.05-0.5 part; modifying agent: 0.1-0.2 parts; pigment: 1-30 parts; pigment dispersing agent: 0.2-6 parts.
Further, the pressure polymerizer is subjected to hydrolytic ring opening and preliminary addition polymerization at a temperature of 260-280 ℃ and a pressure of 0.1-1.2MPa, and the molecular weight of the initial polymer is 8800-10000.
Further, the polymerization reactor carries out addition polymerization and chain equilibrium reaction, the temperature at the upper section is 260-280 ℃, the temperature at the lower section is 235-250 ℃, the pressure is normal pressure or micro negative pressure, and the molecular weight of the polyamide-6 polymer melt is 9800-15100.
Further, the particle size of the pigment is 100-300 nanometers.
Further, the viscosity of the nylon-6 chip is 2.0-2.8.
Compared with the prior art, the invention has the beneficial effects that:
1. the grain diameter of the pigment is nano-grade, so that the service life of the spinning component is prolonged, and the spinning component can be used for 3-6 months generally, thereby greatly reducing the production cost of spinning.
2. Some toning additives are added in the polymerization process, and the particle size of the pigment is nano-scale, so that the pigment of the spun silk is more bright, uniform in color and free of color difference. 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.
3. The product switching process of the process is switched in the double-screw extruder, the switching period is very short, and the generated waste chips are few.
4. The dispersant used by the product is high temperature resistant, does not participate in polymerization reaction, does not influence the subsequent spinning process, and has good spinnability.
Detailed Description
The present invention will be described in detail with reference to examples.
Firstly, dissolving and mixing PTA and caprolactam in a first preparation tank according to a certain proportion; dissolving and mixing a modifier and caprolactam in a second preparation tank according to a certain proportion; dispersing, grinding and mixing water, caprolactam, pigment and a pigment dispersant in a third preparation tank according to a certain proportion; the caprolactam raw material liquid and the solution in the first preparation tank and the second preparation tank are pumped into a dynamic mixer according to a certain proportion through a static mixer to obtain a mixed solution. Caprolactam: 100 parts of (A); water: 3-10 parts; PAT: 0.05-0.5 part; modifying agent: 0.1-0.2 parts; pigment: 1-30 parts; pigment dispersing agent: 0.2-6 parts.
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 at the temperature of 260-280 ℃, the pressure of 0.1-1.2Mpa and the molecular weight of the initial polymer of 8800-10000, conveying the generated initial polymer to a rear polymerization reactor for addition polymerization and chain equilibrium reaction to generate a nylon 6 polymer melt, wherein the temperature of the upper section is 260-280 ℃, the pressure of the lower section is 235-250 ℃, the pressure is normal pressure or micro negative pressure, and the molecular weight of the nylon 6 polymer melt is 9800-15100. (ii) a Feeding the polyamide-6 polymer melt into a double-screw extruder, adding the color paste solution in the third preparation tank in proportion, shearing and blending uniformly; carrying out belt casting, underwater grain cutting and sieving on the nylon 6 polymer melt to obtain initial colored nylon 6 slices;
putting the initial colored nylon-6 chips into a pre-extraction water tank, performing pre-extraction treatment by using water, pumping the treated initial colored nylon-6 chips and water into an extraction tower together by using a slurry pump for extraction, extracting the initial colored nylon-6 chips containing monomers and oligomers in the extraction tower by using extraction water in countercurrent contact with the initial colored nylon-6 chips to obtain extracted colored nylon-6 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; evaporating and concentrating the extraction water overflowing from the pre-extraction water tank, and recovering caprolactam monomers in the extraction water; dehydrating the extracted colored nylon-6 slices, and then circularly drying in a drying tower by using nitrogen to obtain colored dry nylon-6 slices.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. A polycondensation process of a chinlon 6 colored slice comprises the following steps:
s1, dissolving and mixing PTA and caprolactam according to a certain proportion; dissolving and mixing a modifier and caprolactam according to a certain proportion; dispersing, grinding and mixing water, caprolactam, pigment and a pigment dispersing agent according to a certain proportion; feeding the caprolactam raw material liquid and each solution into a dynamic mixer according to a certain proportion through a static mixer to obtain a mixed solution;
s2, 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, and conveying the generated initial polymer into a rear polymerizer for addition polymerization and chain equilibrium reaction to generate a polyamide-6 polymer melt;
s3, feeding the polyamide-6 polymer melt into a double-screw extruder, adding color paste solution in proportion, shearing and blending uniformly; carrying out belt casting, underwater grain cutting and sieving on the nylon 6 polymer melt to obtain initial colored nylon 6 slices;
s4, placing the initial colored nylon-6 chips into a pre-extraction water tank, performing pre-extraction treatment by using water, pumping the treated initial colored nylon-6 chips and water into an extraction tower together by using a slurry pump for extraction, extracting the initial colored nylon-6 chips containing monomers and oligomers in the extraction tower by using extraction water in countercurrent contact with the chips to obtain extracted colored nylon-6 chips, and discharging the extraction water containing the monomers and oligomers into the pre-extraction water tank from the top of the extraction tower;
s5, evaporating and concentrating the extraction water overflowing from the pre-extraction water tank, and recovering caprolactam monomer in the extraction water; dehydrating the extracted colored nylon-6 slices, and then circularly drying in a drying tower by using nitrogen to obtain colored dry nylon-6 slices.
2. The polycondensation process of chinlon 6 colored chips as claimed in claim 1, wherein the ratio of caprolactam: 100 parts of (A); water: 3-10 parts; PAT: 0.05-0.5 part; modifying agent: 0.1-0.2 parts; pigment: 1-30 parts; pigment dispersing agent: 0.2-6 parts.
3. The polycondensation process for colored polyamide-6 chips as claimed in claim 1, wherein the pressure polymerizer is used for the hydrolytic ring-opening and initial polyaddition reaction at a temperature of 260-280 ℃ and a pressure of 0.1-1.2MPa, and the molecular weight of the initial polymer is 8800-10000.
4. The polycondensation process for colored nylon-6 chips as claimed in claim 1, wherein the polymerization reactor comprises polyaddition and chain equilibrium reactions at an upper temperature of 260-280 ℃, a lower temperature of 235-250 ℃, and normal or micro-negative pressure, and the molecular weight of the nylon-6 polymer melt is 9800-15100.
5. The polycondensation process for colored nylon-6 chips as claimed in claim 2, wherein the particle size of the pigment is 100-300 nm.
6. The polycondensation process of chinlon 6 colored chips, as recited in claim 1, wherein the viscosity of the chinlon 6 chips is 2.0-2.8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911345322.9A CN111440312A (en) | 2019-12-24 | 2019-12-24 | Polycondensation process of chinlon 6 colored chips |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911345322.9A CN111440312A (en) | 2019-12-24 | 2019-12-24 | Polycondensation process of chinlon 6 colored chips |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111440312A true CN111440312A (en) | 2020-07-24 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911345322.9A Pending CN111440312A (en) | 2019-12-24 | 2019-12-24 | Polycondensation process of chinlon 6 colored chips |
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| Country | Link |
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| CN (1) | CN111440312A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724398A (en) * | 2021-01-28 | 2021-04-30 | 海阳科技股份有限公司 | Production device and process for in-situ polymerization coloring graphene modified polyamide-6 slice |
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| CN102464799A (en) * | 2010-11-15 | 2012-05-23 | 中国水产科学研究院东海水产研究所 | Coloring method of nylon-6 by using liquid coloring technology |
| CN108570228A (en) * | 2018-01-16 | 2018-09-25 | 江苏海阳锦纶新材料有限公司 | A kind of 6 black of polyamide fibre slice and manufacturing method |
| CN108570147A (en) * | 2018-01-19 | 2018-09-25 | 江苏海阳锦纶新材料有限公司 | A kind of 6 coloured slice continuous production device of polyamide fibre and production method |
| CN108794739A (en) * | 2018-03-26 | 2018-11-13 | 中纺院（天津）科技发展有限公司 | A kind of continuous polymerization technique and products thereof of branched PA6 |
| CN110105563A (en) * | 2019-04-10 | 2019-08-09 | 江苏海阳锦纶新材料有限公司 | A kind of additive agent modified lab scale craft of functional nylon PA6 in-situ polymerization |
-
2019
- 2019-12-24 CN CN201911345322.9A patent/CN111440312A/en active Pending
Patent Citations (6)
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| CN101885842A (en) * | 2010-07-09 | 2010-11-17 | 北京三联虹普纺织化工技术有限公司 | Continuous Polymerization Production Process of Nylon 6 |
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| CN108570228A (en) * | 2018-01-16 | 2018-09-25 | 江苏海阳锦纶新材料有限公司 | A kind of 6 black of polyamide fibre slice and manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112724398A (en) * | 2021-01-28 | 2021-04-30 | 海阳科技股份有限公司 | Production device and process for in-situ polymerization coloring graphene modified polyamide-6 slice |
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Effective date of registration: 20201112 Address after: No.30 Haiyang Road, Hailing District, Taizhou City, Jiangsu Province 225300 Applicant after: Haiyang Technology (Jiangsu) Research Institute Co., Ltd Address before: 225300 No. 122 Haiyang West Road, Taizhou City, Jiangsu Province Applicant before: Haiyang Technology Co., Ltd Applicant before: JIANGSU HAIYANG POLYAMIDE NEW MATERIAL Co.,Ltd. |
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