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Copolymerized flame-retardant polyamide fiber and preparation method thereof

A polyamide fiber and flame retardant polyamide technology are applied in the fields of copolymerization flame retardant polyamide fiber and its preparation, the preparation of flame retardant salt, and the preparation of phosphorus-containing copolymer flame retardant polyamide functional fiber, which can solve the problem of polymer Molecular weight decrease, fiber is easy to fade and feel, low reactivity, etc.

Active Publication Date: 2020-12-29
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

[0059] A preparation method of flame-retardant polyamide 6 / 66 copolymer, the steps are as follows:

[0060] (1) prepare flame retardant salt;

[0061] (1.1) Combine DOPO derivatives and diamine NH 2 R 2 NH 2 Mix at a molar ratio of 1:2.1, then add deionized water accounting for 25wt% of the total mass of the system as a reaction solvent, heat up (starting point of temperature rise is 25°C) and stir under nitrogen protection, and the stirring speed is 100r / min, DOPO derivatives The structural formula is shown in formula (I), in the formula, R 1 for CH 2 , diamine NH 2 R 2 NH 2 is hexamethylenediamine;

[0062] The preparation process of DOPO derivatives is as follows: put DOPO-HQ and acid-binding agent (triethylamine) into a three-necked flask, add solvent (ethanol) to dissolve, add chloroacetate (methyl chloroacetate) dropwise at 100°C ), after reacting for 14 hours, the solvent and unreacted chloroacetate were removed by rotary evaporation, and an ethanol solution of...

Embodiment 2

[0093] A preparation method of flame-retardant polyamide 6 / 66 copolymer, the steps are as follows:

[0094] (1) prepare flame retardant salt;

[0095] (1.1) Combine DOPO derivatives and diamine NH 2 R 2 NH 2 Mix at a molar ratio of 1:2.02, then add deionized water accounting for 26wt% of the total mass of the system as a reaction solvent, and heat up (starting point of temperature rise is 25°C) and stir under nitrogen protection, and the stirring speed is 120r / min, DOPO derivatives The structural formula is shown in formula (I), in the formula, R 1 for (CH 2 ) 2 , diamine NH 2 R 2 NH 2 is decyl diamine;

[0096] The preparation process of DOPO derivatives is as follows: put DOPO-HQ and acid-binding agent (triethylamine) into a three-necked flask, add solvent (ethanol) to dissolve, and add chloropropionate (3-chloropropane) dropwise at 100°C After 14 hours of reaction, the solvent and unreacted chloropropionate were removed by rotary evaporation, and an ethanol soluti...

Embodiment 3

[0118] A preparation method of flame-retardant polyamide 6 / 66 copolymer, the steps are as follows:

[0119] (1) prepare flame retardant salt;

[0120] (1.1) Combine DOPO derivatives and diamine NH 2 R 2 NH 2 Mix at a molar ratio of 1:2.15, then add deionized water accounting for 28wt% of the total mass of the system as a reaction solvent, and heat up (starting point of temperature rise is 25°C) and stir under nitrogen protection. The stirring speed is 115r / min, DOPO derivatives The structural formula is shown in formula (I), in the formula, R 1 for (CH 2 ) 3 , diamine NH 2 R 2 NH 2 Propylenediamine;

[0121] The preparation process of DOPO derivatives is as follows: put DOPO-HQ and acid-binding agent (triethylamine) into a three-necked flask, add solvent (ethanol) to dissolve, and drop chlorobutyrate (4-chlorobutyl Acetate ethyl ester), after reacting for 14 hours, spin to remove the solvent and unreacted chlorobutyrate, add ethanol solution of sodium hydroxide to hy...

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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 of spinning by taking a flame-retardantpolyamide copolymer as all or parts of spinning raw materials to obtain the copolymerized flame-retardant polyamide fibers, wherein the flame-retardant polyamide copolymer is prepared by mixing a flame retardant salt with a polyamide 6 oligomer and / or a polyamide 66 oligomer and then carrying out a condensation polymerization reaction, the flame retardant salt is prepared from a DOPO derivative and diamine NH2R2NH2 through a high-temperature and high-pressure reaction, the temperature of the high temperature is 200-250 DEG C, the pressure of the high pressure is 1.2-1.8 MPa, and the main material of the finally prepared copolymerized flame-retardant polyamide fiber is the flame-retardant polyamide copolymer. The preparation method disclosed by the invention 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 andcan better meet the requirements of the fields of medical treatment and public health, professional clothing, clothing home textiles and the like in modern life of 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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IPC IPC(8): D01F6/90D01F1/10C08G69/42
CPCC08G69/42D01F1/103D01F6/90
Inventor 肖茹陈爽郑裕磊刘畅刘可杨自由顾磊王华平
Owner DONGHUA UNIV
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