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A kind of caprolactam hydrolysis polymer fiber and spinning method thereof

A technology of caprolactam and polymer, applied in the direction of single-component copolyamide artificial filament, melt spinning method, stretch spinning method, etc., can solve the problems of inability to control oligomers, low polymer molecular weight, slow reaction speed, etc. , to achieve the effects of reducing energy consumption, reducing the probability of occlusion, and reducing the possibility

Active Publication Date: 2016-08-24
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to ensure that the polymerization process is carried out in a liquid state, the polymerization temperature must be at least 10°C higher than the melting point of polyamide 6. At this time, the polymerization temperature still cannot control the oligomer in the range of direct spinning of the melt, and there is another low-temperature polymerization. Disadvantages, that is, the reaction speed is slow, and the molecular weight of the obtained polymer is low; and the polymerization process at a lower temperature is actually divided into two parts, one is a melt polymerization process, and the other is a solid phase polymerization process. The process is to obtain a polymer with sufficient molecular weight for product development, but there is no effective way to turn the solid polymer formed at low temperature into a suitable spinning method. If fibers are spun from low-temperature polymers, they must be The polymer is melted first, however, at this time, with the balance related to time and temperature, low-molecular compounds are formed, the amount of which is adapted to the temperature of melting, and is always more than that of low-temperature polymerization. In this way, Compared with the normal aggregation method, there is no advantage

Method used

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  • A kind of caprolactam hydrolysis polymer fiber and spinning method thereof
  • A kind of caprolactam hydrolysis polymer fiber and spinning method thereof
  • A kind of caprolactam hydrolysis polymer fiber and spinning method thereof

Examples

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Effect test

Embodiment 1

[0048] A kind of FDY spinning method of caprolactam hydrolysis polymer, concrete steps comprise:

[0049] The first step: at a temperature of 80°C, caprolactam, capping agent HOOC (CH 2 ) 2 COOH, deionized water and catalyst nylon 66 salt were mixed in proportion, mechanically stirred for 10min, and the rotating speed was 60r / min; wherein relative to caprolactam, the amount of deionized water added was 2wt%, and the capping agent HOOC(CH 2 ) 2 The addition of COOH is 5%, and the addition of catalyst nylon 66 salt is 0.1wt%;

[0050] The second step: pre-polymerize the mixture obtained in the first step under nitrogen atmosphere, the polymerization temperature is controlled at 150 ° C, and the polymerization pressure is controlled at 0.1 MPa; when the following conditions are met, the reaction is terminated: the molecular weight of the obtained prepolymer is 1000 , the content of terminal amino groups is less than 1mmol / kg, the content of extractables is ≤10wt%, and the cont...

Embodiment 2

[0056] A kind of FDY spinning method of caprolactam hydrolysis polymer, concrete steps comprise:

[0057] The first step: at a temperature of 140°C, caprolactam, HOOC (CH 2 ) 10 COOH, deionized water and NH 2 (CH 2 ) 4 COOH was mixed in proportion, mechanically stirred for 60min, and the rotating speed was 240r / min; wherein relative to caprolactam, the amount of deionized water added was 5wt%, HOOC(CH 2 ) 10 The amount of COOH added is 30%, NH 2 (CH 2 ) 4 The amount of COOH added is 5wt%;

[0058] The second step: pre-polymerize the mixture obtained in the first step under a nitrogen atmosphere, the polymerization temperature is controlled at 200 ° C, and the polymerization pressure is controlled at 3 MPa; when the following conditions are met, the reaction is terminated: the molecular weight of the obtained prepolymer is 5000, The content of terminal amino group is less than 1mmol / kg, the content of extractables is ≤10wt%, and the content of cyclic dimer is ≤0.3wt%; ...

Embodiment 3

[0065] A kind of UDY spinning method of caprolactam hydrolysis polymer, concrete steps comprise:

[0066] The first step: under the condition of temperature of 100 ℃, caprolactam, capping agent HOOC (CH2 ) 5 COOH, deionized water and catalyst NH 2 (CH 2 ) 10 COOH was mixed in proportion, mechanically stirred for 30min, and the rotating speed was 100r / min; wherein relative to caprolactam, the amount of deionized water added was 3wt%, and the capping agent HOOC(CH 2 ) 5 The amount of COOH added is 10%, the catalyst NH 2 (CH 2 ) 10 The amount of COOH added is 0.1-5wt%;

[0067] The second step: pre-polymerize the mixture obtained in the first step under nitrogen atmosphere, the polymerization temperature is controlled at 180 ° C, and the polymerization pressure is controlled at 0.5 MPa; when the following conditions are met, the reaction is terminated: the molecular weight of the obtained prepolymer is 3000 , the content of terminal amino groups is less than 1mmol / kg, the...

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Abstract

The invention relates to caprolactam hydrolyzed polymer fibres and a spinning method thereof. The spinning method comprises the following steps: preparing a polyamide 6 prepolymer at low temperature, pre-controlling the content of oligomers in a melt, carrying out auxiliary end-blocking by binary acid to reduce the content of end amino groups in a system, then carrying out end-blocking by ethylene glycol, after that, carrying out chain growth by means of gylcol ester removal exchange, wherein in the obtained product, the content of extractable matters is not greater than 2wt%, and the content of cyclic dimers is not greater than 0.3wt%; then, carrying out direct melt-spinning formation after the condensation polymerization reaction is concluded. The spinning method disclosed by the invention is simple in process, and capable of reducing energy consumption while increasing the utilization rate of caprolactam; the obtained melt is capable of being used for direct melt-spinning, easy in realizing high-capacity large-scale production, and capable of being applied to the fields of garment fibres, industrial silk, engineering plastics and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer fiber preparation, and relates to a caprolactam hydrolyzed polymer fiber and a spinning method thereof. Background technique [0002] Due to its excellent physical and mechanical properties and textile processing properties, nylon fiber has ranked first in the synthetic fiber family for a long period of time since its inception. However, due to price and production cost constraints and polyester fiber The rapid development of the synthetic fiber is now the second largest output. In 2013, my country's nylon output was 2.1128 million tons, a year-on-year increase of 12.44%, accounting for about 6.3% of the total synthetic fiber output. Nylon fiber has excellent physical properties unmatched by polyester fiber. For example, nylon fiber has high breaking strength, wear resistance ranks first among general textile fibers, good hygroscopicity, excellent elastic recovery rate and fatigue resistance, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/80C08G69/44D01D5/08D01D5/088D01D5/12D01D10/02D01D7/00
Inventor 汤廉王朝生王华平江振林吉鹏赵晓敏黄庆
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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