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Flame-retardant cellulosic fiber and preparation method

A flame-retardant cellulose and cellulose technology, applied in the field of flame-retardant fibers, can solve the problems of low degree of substitution of flame-retardant cellulose esters, easy production of gaseous by-products, and easy fall-off of flame retardants, and achieve obvious flame-retardant effects , less reaction steps, permanent flame retardant effect

Active Publication Date: 2014-08-13
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, the degree of substitution of flame retardant cellulose ester is low, and the flame retardant effect mainly comes from unreacted flame retardant, and gaseous by-products are easily produced during the reaction process, and the residual flame retardant is easy to fall off during product application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0018] 1. Preparation of flame retardant fiber ester: dissolve cellulose in N,N-dimethylacetamide / lithium chloride or ionic liquid, add phosphorus flame retardant containing carboxylic acid functional groups, stir mechanically, and then add The sulfonyl chloride compound, the reaction temperature is 30-80°C, and the reaction time is 12-48 hours, and the flame-retardant cellulose ester is prepared. The mass ratio of cellulose to solvent is 1:99 to 25:75; the molar ratio of cellulose to flame retardant is 1:1 to 1:6; the molar ratio of flame retardant to carboxylic acid activator is 1:1.

[0019] The cellulose is one of wood pulp, cotton pulp and hemicellulose, and its degree of polymerization is 400-1000.

[0020] The ionic liquid is 1-allyl-3-methylimidazole chloride (AminCl), 1-butyl-3-methylimidazole chloride (BminCl) and 1-ethyl-3-methylimidazole chloride One of (EminCl).

[0021] The novel green phosphorus-based flame retardant containing a functional carboxyl group (-CO...

Embodiment 1

[0027] Add 6 g of pulverized cellulose wood pulp (polymerization degree DP=400) into 594 g of AminCl ionic liquid, the dissolution temperature is 70° C., and mechanically stir until completely dissolved. Then add 7.92g of flame retardant 2-carboxyethylphenyl hypophosphorous acid, stir mechanically, then add 7.06g of sulfonyl chloride compound p-toluenesulfonyl chloride, the reaction temperature is 30°C, stir for 12h, pour into 1000ml of distilled water to precipitate the product, Wash several times with distilled water and dry. Finally, the pure product flame-retardant cellulose ester 2-carboxyethylphenylphosphinate cellulose ester was obtained.

[0028] The resulting product 2-carboxyethylphenylphosphinate cellulose 5g is blended with 1g of cellulose (polymerization degree DP=400) and added to 44g of AminCl ionic liquid, at a dissolution temperature of 60°C, mechanically stirred until completely dissolved, and obtained spinning silk liquid. Then, the spinning solution is su...

Embodiment 2

[0031] Add 6 g of pulverized cellulose wood pulp (polymerization degree DP=500) into 114 g of AminCl ionic liquid, the dissolution temperature is 80° C., and mechanically stir until completely dissolved. Then add 15.84g of flame retardant 2-carboxyethylphenyl hypophosphorous acid, stir mechanically, then add 14.12g of sulfonyl chloride compound p-toluenesulfonyl chloride, the reaction temperature is 40°C, stir for 24h, pour into 1000ml of distilled water to precipitate the product, Wash several times with distilled water and dry. Finally, the pure product flame-retardant cellulose ester 2-carboxyethylphenylphosphinate cellulose ester was obtained.

[0032] The obtained product 2-carboxyethylphenylphosphinate cellulose 5g was blended with 0.5g cellulose (polymerization degree DP=500) and added to 26.85g AminCl ionic liquid, the dissolution temperature was 60°C, and mechanically stirred until completely dissolved. to obtain a spinning solution. After the spinning solution is d...

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Abstract

The invention discloses a flame-retardant cellulosic fiber and a preparation method. The preparation method comprises the steps of preparation of flame-retardant cellulose ester and preparation of the flame-retardant cellulosic fiber, wherein in the step of preparing flame-retardant cellulose ester, cellulose with a certain degree of polymerization is dissolved into a N,N-dimethylacetamide / lithium chloride or ionic liquid solvent, a flame retardant containing carboxyl is added, the components are stirred, a sulfonyl chloride compound serving as an activating agent is added, and the reaction is carried out at 30-80 DEG C for 12-48 hours to prepare the flame-retardant cellulose ester, wherein the mass ratio of the cellulose to the solvent is 1:99 to 25:75, the molar ratio of the cellulose to the flame retardant is 1:1 to 1:6, and the molar ratio of the flame retardant to the activating agent is 1:1; in the step of preparing the flame-retardant cellulosic fiber, the product is blended with cellulose acetate or cellulose, and then the flame-retardant cellulosic fiber is prepared by a dry-wet spinning process, wherein the concentration of spinning liquid is 12-30 percent, and the mass ratio of the flame-retardant cellulose ester to cellulose acetate or cellulose is 5:1 to 29:1. The flame-retardant cellulosic fiber is high in thermal stability and has a flame-retardant effect permanently; during flame retardance, toxic gas is not generated, and an environment protection requirement is met.

Description

technical field [0001] The invention relates to flame-retardant fiber technology, in particular to a method for preparing a flame-retardant cellulose fiber that first synthesizes a flame-retardant cellulose ester. Background technique [0002] Cellulose is the most abundant natural polymer substance bestowed by nature to human beings. It is a precious gift from nature to human beings. It is not only rich in sources, but also a renewable resource. Today, when petroleum resources are increasingly depleted, cellulose is more and more popular. people's attention. The cellulose fiber made of cellulose has the characteristics of good moisture absorption, strong air permeability, good dyeability, comfortable wearing, easy textile processing and biodegradability, which is unmatched by other synthetic fibers. However, the limiting oxygen index (LOI) value of cellulose fiber is about 19, and it is extremely flammable in case of fire, which seriously limits its use in the fields of li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F8/02D01F8/18C08H8/00C08B15/05C08B37/14
CPCY02P20/54
Inventor 宋俊程博闻郑云波纪秀杰袁娅
Owner TIANJIN POLYTECHNIC UNIV
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