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Copolymerized flame-retardant polyamide fiber and preparation method thereof

A technology of polyamide fiber and flame-retardant polyamide, which is applied in the field of copolymerized flame-retardant polyamide fiber and its preparation, preparation of flame-retardant salt, and preparation of phosphorus-containing copolymerized flame-retardant polyamide functional fiber, which can solve air permeability Problems such as deterioration, decrease in polymer molecular weight, and influence on the polymerization process

Active Publication Date: 2020-12-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patents (publication numbers CN106633043A, CN106675007A, etc.) all prepare flame-retardant polyamides by copolymerization. When preparing flame-retardant salts, they are all carried out at low temperature (60-90°C) under normal pressure, and their reactivity is low. When the amount is large, the molecular weight of the polymer is severely reduced, and under this condition, the flame retardant monomer and the diamine are not connected by covalent bonds, so the flame retardant salt is easily destroyed during the later polymerization process, thereby affecting the polymerization. process
Microorganisms generally exist in fiber fabrics, which can reproduce rapidly in wet conditions and easily cause skin infections after contact with the skin; static electricity is common in the production, processing and use of polyamide fibers, and static electricity may cause serious safety problems; traditional fiber dyeing methods The fiber is put into the dyeing bath for dip-dyeing. Due to the stable chemical properties of polyamide, the dye only covers the surface of the fiber, and the fiber is easy to fade and the feel and air permeability are poor. Traditional synthetic fibers are mostly circular cross-section fibers, and the fabric made of them has moisture absorption and air permeability bad

Method used

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  • Copolymerized flame-retardant polyamide fiber and preparation method thereof
  • Copolymerized flame-retardant polyamide fiber and preparation method thereof
  • Copolymerized flame-retardant polyamide fiber and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0060] A preparation method of flame-retardant polyamide 66 / 6 copolymer, the steps are as follows:

[0061] (1) prepare flame retardant salt;

[0062] (1.1) Mix N,N-bis(6-aminohexyl)phenyl phosphoric acid diamide and adipic acid in an equimolar ratio, then add deionized water accounting for 55wt% of the total mass of the system as a reaction solvent, and heat up under nitrogen protection (The starting point of heating is 25°C) and stirring, the stirring speed is 50r / min, N,N-bis(6-aminohexyl)phenyl phosphoric acid diamide is a mixture of the compound of formula (I) and the compound of formula (II) ;

[0063] The preparation process of N,N-bis(6-aminohexyl)phenylphosphoryl diamine is as follows: under the condition of 25°C, dissolve hexamethylenediamine and phenylphosphoryl dichloride in an organic solvent (chloroform), and stir Add the organic solution of hexamethylenediamine dropwise to the organic solution of phenylphosphoryl dichloride, the mol ratio of phenylphosphoryl d...

Embodiment 2

[0094] A preparation method of flame-retardant polyamide 66 / 6 copolymer, the steps are as follows:

[0095] (1) prepare flame retardant salt;

[0096] (1.1) Mix N,N-bis(6-aminohexyl)phenyl phosphoric acid diamide and malonic acid in an equimolar ratio, then add deionized water accounting for 56wt% of the total mass of the system as a reaction solvent, and carry out under nitrogen protection Heating (starting point of heating is 25°C) and stirring, the stirring speed is 70r / min, N,N-bis(6-aminohexyl)phenyl phosphoric acid diamide is the compound of formula (I) structure and formula (II) structure compound mixture;

[0097] The preparation process of N,N-bis(6-aminohexyl)phenylphosphoryl diamine is as follows: under the condition of 25°C, dissolve hexamethylenediamine and phenylphosphoryl dichloride in an organic solvent (acetonitrile), and stir The organic solution of hexamethylenediamine is added dropwise in the organic solution of phenylphosphoryl dichloride, the mol ratio ...

Embodiment 3

[0119] A preparation method of flame-retardant polyamide 66 / 6 copolymer, the steps are as follows:

[0120] (1) prepare flame retardant salt;

[0121] (1.1) Mix N,N-di(6-aminohexyl)phenylphosphoric acid diamide and succinic acid in an equimolar ratio, then add deionized water accounting for 58wt% of the total mass of the system as a reaction solvent, and carry out under nitrogen protection Heating (starting point of heating is 25°C) and stirring, the stirring speed is 65r / min, N,N-bis(6-aminohexyl)phenyl phosphoric acid diamide is the compound of formula (I) structure and formula (II) structure compound mixture;

[0122] N, the preparation process of N-bis (6-aminohexyl) phenyl phosphoric acid diamide is with embodiment 1;

[0123] (1.2) After the temperature rises to 213°C, keep the pressure at 1.75MPa, and keep the pressure for 2 hours;

[0124] (1.3) Reduce the pressure to normal pressure within 0.8h, reduce the stirring speed to 50r / min, and vacuumize to -0.07MPa for 0....

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Abstract

The invention relates to a copolymerized flame-retardant polyamide fiber and a preparation method thereof. The preparation method comprises the following steps that a flame-retardant polyamide copolymer serves as all or part of spinning raw materials for spinning to obtain the copolymerized flame-retardant polyamide fiber, wherein the flame-retardant polyamide copolymer is prepared by mixing a flame retardant salt with a polyamide 66 oligomer and / or a polyamide 6 oligomer and then carrying out condensation polymerization, the flame retardant salt is prepared from N,Ndi (6aminohexyl) phenyl phosphoramide and binary acid HOOCR1COOH through a high-temperature and high-pressure reaction, the temperature of the high temperature is 210-220 DEG C, and the pressure of the high pressure is 1.7-1.9MPa, and the main material of the finally prepared copolymerized flame-retardant polyamide fiber is the flame-retardant polyamide copolymer. The preparation method is simple to operate, the flame-retardant polyamide copolymer is excellent in flame retardance and good in spinnability, and the prepared copolymerized flame-retardant polyamide fiber is a functional fiber with flame retardance and canbetter meet the requirements of the fields of medical treatment and public health, professional clothing, clothing home textiles and the like in modern life on the flame-retardant polyamide fiber.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant polyamide fiber synthesis, and relates to a flame-retardant copolymerized polyamide fiber and a preparation method thereof, in particular to a new preparation method of a flame-retardant salt, and a preparation of a phosphorus-containing copolymerized flame-retardant polyamide functional fiber Preparation. Background technique [0002] Polyamide (PA) is the earliest synthetic fiber developed, and the fabric prepared by it has excellent chemical corrosion resistance, abrasion resistance, flexibility and dyeability. However, polyamide 6 has low impact resistance, while polyamide 66 has a high melting point and a narrow processing temperature range, which limits the application of both in certain fields. Therefore, polyamide 66 and polyamide 6 are copolymerized and modified by melt copolymerization to prepare polyamide 66 / 6 composite materials, which can complement the advantages and disadva...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/80D01F1/10D01F1/09D01F8/12D01F8/14D01F8/06C08G69/42
CPCC08G69/42D01F1/09D01F1/103D01F6/80D01F8/06D01F8/12D01F8/14
Inventor 陈爽肖茹郑裕磊宋炜刘畅李圆圆谢瑾瑜王华平
Owner DONGHUA UNIV
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