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Flame-retardant polyamide 6 fiber and preparation method thereof

A technology of flame retardant polyamide and polyamide, which is applied in the direction of single-component copolyamide rayon, chemical characteristics of fibers, melt spinning, etc. Good effect, little effect on mechanical properties

Inactive Publication Date: 2015-12-16
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are also shortcomings in the flame retardant modification of copolymerization. Usually, the flame retardant modification of copolymerization is to directly polymerize the monomers of the flame retardant and the polyamide to obtain a random copolymer of the polyamide and the flame retardant. The flame retardant is an important component in the polyamide. Randomly distributed, for random copolymers, as the content of non-crystalline comonomer (flame retardant) increases, the melting point decreases monotonically. 6 fiber, but also need to maintain the high temperature performance of polyamide 6 fiber, which limits the use of polyamide 6 fiber

Method used

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  • Flame-retardant polyamide 6 fiber and preparation method thereof
  • Flame-retardant polyamide 6 fiber and preparation method thereof
  • Flame-retardant polyamide 6 fiber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A preparation method for flame-retardant polyamide 6 fibers, specifically comprising the following steps:

[0044] (1) Mix the flame retardant DDP, hexamethylenediamine and water, mix evenly at 50°C for 2 hours under the protection of nitrogen, then stir and react at 90°C for 2 hours, then raise the temperature to 150°C for further polymerization, and finally decompress and vacuumize, and react Finish generating flame retardant prepolymer, it is viscous liquid, number average molecular weight Mn is 1.8×10 3 , the molar ratio of flame retardant DDP, hexamethylenediamine and water is 1:1.1:2, and the two ends of the obtained flame retardant prepolymer are active end groups of carboxyl and amine groups respectively;

[0045] The structure of the flame retardant is:

[0046]

[0047] (2) 90.7 parts by mass of caprolactam, 4.0 parts by mass of water and 0.3 parts by mass of adipic acid are added to the reactor, and N 2 Exhaust the air in the kettle, stir at a speed of 2...

Embodiment 2

[0057] A preparation method for flame-retardant polyamide 6 fibers, specifically comprising the following steps:

[0058] (1) Mix the flame retardant CEPPA, hexamethylenediamine and water, mix evenly at 80°C for 3 hours under the protection of nitrogen, then stir and react at 130°C for 3 hours, then raise the temperature to 180°C for further polymerization, and finally decompress and vacuumize, react Finish generating flame retardant prepolymer, it is semi-solid, number average molecular weight Mn is 2.5 * 10 3 , the molar ratio of flame retardant CEPPA, hexamethylenediamine and water is 1:1.2:2.5, and the two ends of the obtained flame retardant prepolymer are active end groups of carboxyl and amine groups respectively;

[0059] The structure of the flame retardant is:

[0060]

[0061] (2) 88.0 parts by mass of caprolactam, 1.5 parts by mass of water and 0.5 parts by mass of adipic acid are added to the reactor, and N 2 Exhaust the air in the kettle, stir at a speed of ...

Embodiment 3

[0071] A preparation method for flame-retardant polyamide 6 fibers, specifically comprising the following steps:

[0072] (1) Mix the flame retardant BCPPO, hexamethylenediamine and water, mix evenly at 60°C for 2.5 hours under the protection of nitrogen, then stir and react at 95°C for 2 hours, then raise the temperature to 160°C for further polymerization, and finally vacuumize under reduced pressure, At the end of the reaction, a flame retardant prepolymer is generated, which is a viscous liquid with a number average molecular weight Mn of 2.8×10 3 , the molar ratio of flame retardant BCPPO, hexamethylenediamine and water is 1:1.2:2.1, and the two ends of the obtained flame retardant prepolymer are active end groups of carboxyl and amine groups respectively;

[0073] The structure of the flame retardant is:

[0074]

[0075] (2) 92.9 parts by mass of caprolactam, 0.8 parts by mass of water and 0.8 parts by mass of adipic acid are added to the reactor, and N 2 Exhaust t...

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Abstract

The invention relates to a flame-retardant polyamide 6 fiber and a preparation method thereof, especially to a method for preparing the block copolymerized flame-retardant polyamide 6 fiber by continuously and separately carrying out two-step polymerization on a phosphorus-containing reactive flame retardant. The method is characterized in that the flame retardant reacts with diamine or dihydric alcohol to produce a flame-retardant prepolymer, then the flame-retardant prepolymer and polyamide 6 prepolymer undergo copolymerization so as to obtain a flame-retardant polyamide 6 material, and then pelletizing of a cast strip, extraction and drying, melt spinning and drawing are carried out so as to obtain the flame-retardant polyamide 6 fiber. The flame-retardant polyamide 6 fiber prepared by using the method has the characteristics of a small addition amount of the flame retardant, long-lasting flame retardation effect and a limit oxygen index of more than 30%, can be used for preparation of fabric products and is widely applicable to the fields of civil filaments and industrial filaments.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant polyamide fiber synthesis, and relates to a flame-retardant polyamide 6 fiber and a preparation method thereof, in particular to a block-copolymerized fiber containing flame retardant obtained through continuous and separately carried out two-step polymerization reactions. Prepolymer flame-retardant polyamide 6 fiber and its preparation method. Background technique [0002] Polyamide fiber is called nylon in our country, and it is also called nylon, nylon, capron and so on abroad. As the earliest industrialized variety of synthetic fiber, polyamide 6 fiber has played a pivotal role in civil and industrial fields due to its excellent strength, wear resistance, hygroscopicity, and resilience. However, the limiting oxygen index of polyamide 6 fiber is only about 21%, which is a combustible fiber. The research on flame-retardant polyamide 6 fiber has become an urgent problem to be solved. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/80D01F6/82D01D5/08
Inventor 刘可肖茹李圆圆储贻健王朝生王华平
Owner DONGHUA UNIV
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