CN111441097A - Fine-denier high-strength chinlon 66 fiber and preparation method thereof - Google Patents

Fine-denier high-strength chinlon 66 fiber and preparation method thereof Download PDF

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Publication number
CN111441097A
CN111441097A CN202010146804.8A CN202010146804A CN111441097A CN 111441097 A CN111441097 A CN 111441097A CN 202010146804 A CN202010146804 A CN 202010146804A CN 111441097 A CN111441097 A CN 111441097A
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China
Prior art keywords
stretching
group
hot rollers
tows
fiber
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CN202010146804.8A
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Chinese (zh)
Inventor
杜选
肖文华
杨贺
葛爱雄
宫殿敏
史晓军
刘成家
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Jihua Group Corp ltd
LIAONING YINZHU CHEMTEX GROUP Co Ltd
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Jihua Group Corp ltd
LIAONING YINZHU CHEMTEX GROUP Co Ltd
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Priority to CN202010146804.8A priority Critical patent/CN111441097A/en
Publication of CN111441097A publication Critical patent/CN111441097A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02Heat treatment
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/12Stretch-spinning methods
    • D01D5/16Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D7/00Collecting the newly-spun products

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Artificial Filaments (AREA)

Abstract

A fine denier high strength chinlon 66 fiber and a preparation method thereof belong to the field of fiber production. Firstly drying and tackifying nylon 66 slices to obtain high-viscosity slices, then melting and extruding the high-viscosity slices, adopting a one-step process route of spinning, stretching and shaping, and producing the fine denier high-strength nylon 66 fiber on a spinning and drawing integrated machine by reducing the ejection speed and improving the natural stretching ratio. The denier of the nylon 66 fiber prepared by the method is 10-40D, the number of holes is 5-34 f, and the breaking strength can reach more than 8.5 g/D.

Description

Fine-denier high-strength chinlon 66 fiber and preparation method thereof
Technical Field
The invention relates to the technical field of fiber production, in particular to fine denier high-strength chinlon 66 fiber and a preparation method thereof.
Background
The market demand for fine denier fibers is increasing as a representative variety of differential fibers. Research shows that when the fiber is thin to a certain degree, a plurality of excellent performances which cannot be compared with the traditional fiber can be exerted, and the additional value of the chinlon 66 fiber can be effectively improved, such as: soft hand feeling, large specific surface area, high heat preservation, high self-cleaning capability, high flexibility and the like.
The nylon 66 fiber as the first artificial synthetic fiber has the advantages of excellent flexibility, rebound resilience, small density, high strength, excellent wear resistance and the like, so that the nylon 66 fiber can be widely applied to clothing, industry, military and special industries. Along with the urgent need of people for high-grade and thin garment materials, the nylon 66 fiber is more and more favored by the market. The fine denier nylon 66 is used as a differentiated variety in nylon fibers, has good sweat conduction and air permeability and softer hand feeling, and is very suitable for making garments in mountaineering, traveling and special industries due to the good wear resistance, light weight and high strength of the nylon 66.
The one-step process spinning fine denier nylon 66 fiber needs to require high orientation degree of filament bundles in order to achieve high strength, the high orientation degree is usually realized by a mode of improving subsequent drawing ratio at present, the method is adopted to realize the high orientation degree, and the drawing stress is improved mainly at the later stage to force macromolecules to be regularly arranged and oriented along the direction of a macromolecular chain, so that the problems of more broken filaments (single fiber breakage), high end breakage rate and low production rate in the whole production process are easily caused by the generation of broken filaments and ends in the subsequent drawing process. The technology for avoiding broken ends of broken filaments by improving the natural draw ratio and reducing the subsequent draw ratio is rarely reported at home and abroad.
Disclosure of Invention
The invention aims to provide fine denier high-strength nylon 66 fiber and a preparation method thereof, the method adopts a one-step process route, the low denier high-strength nylon 66 fiber is produced by reducing the ejection speed of a spinneret plate and improving the natural draw ratio, the production efficiency of the method is high, and the production requirements of protofilaments with different extinction degrees can be met.
The technical scheme of the invention is as follows:
a preparation method of industrial functional chinlon 66 fibers comprises the following steps:
1) drying and tackifying: conveying the chinlon 66 slices with initial relative viscosity of 2.5-3.0 into a drying tower, and performing countercurrent circulating drying by adopting nitrogen to obtain the chinlon 66 ultrahigh-viscosity slices with water content of less than or equal to 200ppm and relative viscosity of 3.5-3.8;
2) melt extrusion: conveying the high-viscosity chinlon 66 slices into a screw extruder, wherein the temperature of each area of the screw is 285-310 ℃, and melting and extruding the high-viscosity slices;
3) high-pressure spinning: enabling the melt extruded in the step 2) to enter a spinning box through a melt pipeline with the temperature of 280-295 ℃, quantitatively pressing the melt into a spinning assembly through a metering pump, and spraying the melt from a spinneret plate to form tows; the speed of the filament bundle is 5-10 m/min;
4) and (3) cooling and forming: the melt trickle sprayed after spinning is slowly cooled and then is cooled by side blowing to form a nascent fiber tow;
5) oiling and bundling: oiling the cooled filament bundles by using an oil tanker, wherein the oiling mode is emulsion oiling, and the oiling rate is controlled to be 1.0-1.3%;
6) stretching and shaping: carrying out stretching and shaping treatment on the bunched and oiled tows; the method comprises the following steps of stretching, wherein a group of feeding rollers is adopted for natural stretching, four pairs of hot rollers are adopted for two-stage hot stretching and one-stage relaxation heat setting, the total stretching multiple is 2.5-3.5, the orientation degree of the tows in the early stage is improved by improving the natural stretching ratio, and then two-stage hot stretching is adopted for continuously orienting the macromolecules of the tows, so that higher strength is obtained;
further preferably: the feeding roller is not heated, the natural draw ratio is more than or equal to 200, and the feeding roller is mainly used for pre-orienting the tows sprayed by the spinneret plate in a viscous state, so that the subsequent draw ratio is reduced, and the generation of subsequent drawn broken filaments is reduced; the speed difference between the feeding roller and the first group of hot rollers plays a role in tensioning the slivers, and the speed ratio is 1.02-1.06; the first group of hot rollers are 40-70 ℃, the second group of hot rollers are 150-190 ℃, the first-step stretching is carried out between the second group of hot rollers and the first group of hot rollers, the speed ratio is 1.6-2.5, the first group of hot rollers and the second group of hot rollers mainly function in heating the tows to the vitrification temperature, so that macromolecules have motion conditions, and molecular chains are arranged along the stretching direction; the third group of hot rollers is 200-250 ℃, the second-step stretching is carried out between the third group of hot rollers and the second group of hot rollers, the speed ratio is 1.2-1.8 times, the second-step stretching mainly has the effect of making up the deficiency of the first-step stretching, so that hydrogen bonds among macromolecules are weakened or disappear, the macromolecules are further oriented, and the strand silk reaches the highest strength; the temperature of the fourth group of hot rollers is 170-200 ℃, the tows are subjected to relaxation heat setting between the fourth group of hot rollers and the third group of hot rollers, the speed ratio is 0.95-0.98, and the fourth group of hot rollers are used for performing relaxation setting on the tows, so that the crystallinity of the tows is improved, and the precursor with a more stable molecular structure is obtained.
7) Winding: and (3) fully automatically winding the tows subjected to the stretching and setting treatment, setting the winding speed to 5200-5800 m/min, and winding to obtain the fine denier high-strength nylon 66 fiber.
Preferably, the spinning melt ejecting speed in the step 3) is 6-8 m/min.
Preferably, the total stretching multiple in the step 6) is preferably 2.8-3.0.
Preferably, the winding speed in the step 7) is 5500-5800 m/min.
The design idea of the invention is as follows:
in order to achieve high strength and require high orientation degree of filament bundles, the conventional process for achieving the high orientation degree is usually realized by improving a subsequent drawing ratio, and the method for achieving the high orientation degree mainly depends on improving the drawing stress at the later stage to force macromolecules to be regularly arranged and oriented along a macromolecular chain direction, so that the problems of more filaments (single fiber breakage), high breakage rate and low production rate in the whole production process due to the generation of filaments and broken ends in the subsequent drawing process are easily caused.
In the invention, in order to enable the fiber macromolecules to achieve the same orientation effect and reduce the subsequent drawing ratio and reduce the generation of broken filaments and broken ends, the aim is to enable the molecular motion of molecules to generate partial orientation in a viscous state by improving the natural drawing ratio (drawing in a macromolecule cold drawing stage) to obtain low-orientation fibers, and then perform supplementary drawing on the fibers to further orient the fibers, thereby achieving the effects of reducing the subsequent drawing ratio and reducing the generation of broken ends of the filaments and obtaining the fine denier high-strength nylon 66 fibers.
The high degree of orientation is achieved in the present invention mainly by high stretching in the natural stretching stage. In the natural stretching stage, the stretching stress is unchanged, and the orientation degree is increased, so that the method not only can greatly reduce the difficulty of subsequent stretching, but also can ensure that the molecular orientation degree reaches the required value.
The invention has the following advantages:
1. the technology provided by the invention is suitable for ultrahigh-viscosity slices with different extinction degrees, and the broken rate of the broken filaments in the production process is low.
2. The spinning speed can be effectively improved by applying the process technology and the device disclosed by the invention, the higher production efficiency is achieved, and the nylon 66 fiber with fine denier (the total denier of the filament bundle is 10-40D, and the number of holes is 5-34 f) and high strength (more than or equal to 8.5g/D) is produced.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
A preparation method of industrial functional chinlon 66 fibers comprises the following steps:
1) drying and tackifying: the nylon 66 slices with the initial relative viscosity of 2.5-3.0 (sulfuric acid process) are conveyed into a drying tower, the temperature of the lower part of the drying tower is 120-155 ℃, and the flow rate is 450-700 Nm3Performing countercurrent circulation drying on the nitrogen per hour, wherein the system pressure is 8-12 Kpa, the oxygen content is less than or equal to 5ppm, and the reaction time is 30-40H, so as to obtain a nylon 66 ultrahigh-viscosity slice with the water content of less than or equal to 200ppm and the relative viscosity of 3.5-3.8 (by a sulfuric acid method);
2) melt extrusion: conveying the high-viscosity chinlon 66 slices in the step 1) into a screw extruder for melt extrusion, wherein the length-diameter ratio of the screw extruder is 30:1, the temperature of each zone of the screw is 285-310 ℃, the heating is divided into six heating zones, the temperature of the first zone is 300-310 ℃, the temperature of the second zone is 300-310 ℃, the temperature of the third zone is 295-305 ℃, the temperature of the fourth zone is 295-305 ℃, the temperature of the fifth zone is 285-295 ℃, the temperature of the sixth zone is 285-295 ℃, and the fourth zone and the fifth zone are provided with air cooling devices, namely air cooling blowing, so that the uniformity and the flowability of a melt are ensured, and the shear heat generated by pressurization and backflow is reduced;
3) high-pressure spinning: enabling the melt extruded in the step 2) to enter a spinning box through a melt pipeline with the temperature of 285-295 ℃, quantitatively pressing the melt into a spinning assembly through a metering pump, and spraying the melt from a spinneret plate to form tows; the spinning box is 2 bits/box and 10 heads/bit; the preheating temperature of the assembly is 305-320 ℃; the speed of the filament bundle is 5-10 m/min;
4) and (3) cooling and forming: the melt trickle sprayed after spinning is slowly cooled and then is cooled by side blowing to form a nascent fiber tow; the temperature of the slow cooler is 260-280 ℃; the temperature of the cross air is 18-22 ℃, and the humidity is 85-93%;
5) oiling and bundling: oiling the cooled filament bundles by using an oil tanker, wherein the oiling mode is emulsion oiling, and the oiling rate is controlled to be 1.0-1.3%;
6) stretching and shaping: carrying out stretching and shaping treatment on the bunched and oiled tows; the method comprises the following steps of stretching, wherein a group of feeding rollers is adopted for natural stretching, four pairs of hot rollers are adopted for two-stage hot stretching and one-stage relaxation heat setting, the total stretching multiple is 2.8-3.0, the orientation degree of the tows in the early stage is improved by improving the natural stretching ratio, and then two-stage hot stretching is adopted for continuously orienting the macromolecules of the tows, so that higher strength is obtained; the feeding roller is not heated, the natural draw ratio is more than or equal to 200, and the feeding roller is mainly used for pre-orienting the tows sprayed by the spinneret plate in a viscous state, so that the subsequent draw ratio is reduced, and the generation of subsequent drawn broken filaments is reduced; the speed difference between the feeding roller and the first group of hot rollers plays a role in tensioning the slivers, and the speed ratio is 1.02-1.06; the first group of hot rollers are 40-70 ℃, the second group of hot rollers are 150-190 ℃, the first-step stretching is carried out between the second group of hot rollers and the first group of hot rollers, the speed ratio is 1.6-2.5, the first group of hot rollers and the second group of hot rollers mainly function in heating the tows to the vitrification temperature, so that macromolecules have motion conditions, and molecular chains are arranged along the stretching direction; the third group of hot rollers is 200-250 ℃, the second-step stretching is carried out between the third group of hot rollers and the second group of hot rollers, the speed ratio is 1.2-1.8 times, the second-step stretching mainly has the effect of making up the deficiency of the first-step stretching, so that hydrogen bonds among macromolecules are weakened or disappear, the macromolecules are further oriented, and the strand silk reaches the highest strength; the temperature of the fourth group of hot rollers is 170-200 ℃, the tows are subjected to relaxation heat setting between the fourth group of hot rollers and the third group of hot rollers, the speed ratio is 0.95-0.98, and the fourth group of hot rollers are used for performing relaxation setting on the tows, so that the crystallinity of the tows is improved, and the precursor with a more stable molecular structure is obtained.
7) Winding: and (3) fully automatically winding the tows subjected to the stretching and setting treatment on 10-head winding equipment, setting the winding speed to 5500-5800 m/min, and winding to obtain the fine denier high-strength nylon 66 fiber.
The invention has the advantages of small broken end rate of the broken filaments in the industrialized production process, production of nylon 66 fibers with fine denier (the total denier of the filament bundles is 10-40D, the number of holes is 5-34 f) and high strength of more than or equal to 8.5g/D, and stable performance.

Claims (6)

1. A preparation method of industrial functional chinlon 66 fibers is characterized by comprising the following steps:
1) drying and tackifying: conveying the chinlon 66 slices with initial relative viscosity of 2.5-3.0 into a drying tower, and performing countercurrent circulating drying by adopting nitrogen to obtain the chinlon 66 ultrahigh-viscosity slices with water content of less than or equal to 200ppm and relative viscosity of 3.5-3.8;
2) melt extrusion: conveying the high-viscosity chinlon 66 slices into a screw extruder, wherein the temperature of each area of the screw is 285-310 ℃, and melting and extruding the high-viscosity slices;
3) high-pressure spinning: enabling the melt extruded in the step 2) to enter a spinning box through a melt pipeline with the temperature of 280-295 ℃, quantitatively pressing the melt into a spinning assembly through a metering pump, and spraying the melt from a spinneret plate to form tows; the speed of the filament bundle is 5-10 m/min;
4) and (3) cooling and forming: the melt trickle sprayed after spinning is slowly cooled and then is cooled by side blowing to form a nascent fiber tow;
5) oiling and bundling: oiling the cooled filament bundles by using an oil tanker, wherein the oiling mode is emulsion oiling, and the oiling rate is controlled to be 1.0-1.3%;
6) stretching and shaping: carrying out stretching and shaping treatment on the bunched and oiled tows; the method comprises the following steps of stretching, wherein a group of feeding rollers is adopted for natural stretching, four pairs of hot rollers are adopted for two-stage hot stretching and one-stage relaxation heat setting, the total stretching multiple is 2.5-3.5, the orientation degree of the tows in the early stage is improved by improving the natural stretching ratio, and then two-stage hot stretching is adopted for continuously orienting the macromolecules of the tows, so that higher strength is obtained;
7) winding: and (3) fully automatically winding the tows subjected to the stretching and setting treatment, setting the winding speed to 5200-5800 m/min, and winding to obtain the fine denier high-strength nylon 66 fiber.
2. The preparation method of the industrial functional polyamide 66 fiber according to claim 1,
step 6), stretching and shaping: the feeding roller is not heated, the natural draw ratio is more than or equal to 200, and the feeding roller is mainly used for pre-orienting the tows sprayed by the spinneret plate in a viscous state, so that the subsequent draw ratio is reduced, and the generation of subsequent drawn broken filaments is reduced; the speed difference between the feeding roller and the first group of hot rollers plays a role in tensioning the slivers, and the speed ratio is 1.02-1.06; the first group of hot rollers are 40-70 ℃, the second group of hot rollers are 150-190 ℃, the first-step stretching is carried out between the second group of hot rollers and the first group of hot rollers, the speed ratio is 1.6-2.5, the first group of hot rollers and the second group of hot rollers mainly function in heating the tows to the vitrification temperature, so that macromolecules have motion conditions, and molecular chains are arranged along the stretching direction; the third group of hot rollers is 200-250 ℃, the second-step stretching is carried out between the third group of hot rollers and the second group of hot rollers, the speed ratio is 1.2-1.8 times, the second-step stretching mainly has the effect of making up the deficiency of the first-step stretching, so that hydrogen bonds among macromolecules are weakened or disappear, the macromolecules are further oriented, and the strand silk reaches the highest strength; the temperature of the fourth group of hot rollers is 170-200 ℃, the tows are subjected to relaxation heat setting between the fourth group of hot rollers and the third group of hot rollers, the speed ratio is 0.95-0.98, and the fourth group of hot rollers are used for performing relaxation setting on the tows, so that the crystallinity of the tows is improved, and the precursor with a more stable molecular structure is obtained.
3. The preparation method of the industrial functional chinlon 66 fiber according to claim 2, wherein the total stretching multiple in the step 6) is preferably 2.8-3.0.
4. The preparation method of the industrial functional chinlon 66 fiber according to claim 1, wherein the spinning melt ejection speed in the step 3) is preferably 6-8 m/min.
5. The preparation method of the industrial functional chinlon 66 fiber is characterized in that the winding speed in the step 7) is preferably 5500-5800 m/min.
6. The functional nylon 66 fiber prepared by the method of any one of claims 1-5.
CN202010146804.8A 2020-03-05 2020-03-05 Fine-denier high-strength chinlon 66 fiber and preparation method thereof Pending CN111441097A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114622293A (en) * 2021-12-07 2022-06-14 嘉兴逸鹏化纤有限公司 Production process for spinning fine denier yarn on iBox 32-head equipment
CN115896961A (en) * 2022-12-27 2023-04-04 广东坚达聚纤科技实业有限公司 Melt spinning optimization process
CN116024677A (en) * 2022-12-06 2023-04-28 江苏诚业化纤科技有限公司 Preparation method of high-strength low-elongation nylon 6 fiber

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114622293A (en) * 2021-12-07 2022-06-14 嘉兴逸鹏化纤有限公司 Production process for spinning fine denier yarn on iBox 32-head equipment
CN116024677A (en) * 2022-12-06 2023-04-28 江苏诚业化纤科技有限公司 Preparation method of high-strength low-elongation nylon 6 fiber
CN116024677B (en) * 2022-12-06 2024-03-08 江苏诚业化纤科技有限公司 Preparation method of high-strength low-elongation nylon 6 fiber
CN115896961A (en) * 2022-12-27 2023-04-04 广东坚达聚纤科技实业有限公司 Melt spinning optimization process

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