Preparation method of flame-retardant cellulose fiber

A technology of flame-retardant cellulose and cellulose, which is applied in the manufacture of artificial filaments in cellulose solution, fire-resistant and flame-retardant filaments, etc., and can solve the problem of long, usually 2 to 48 hours, or even up to 120 hours, limited functions The application and development of flame-retardant fibers, the impact of spinneret pressure resistance and drafting, etc., to achieve the effects of shortened dissolution time, easy industrial production, and no pollution to the environment

Active Publication Date: 2019-01-15
龙丝(上海)新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when using ionic liquids (alkyl quaternary ammonium salts, alkyl imidazolium salts, alkyl pyrrole salts, etc.) The obtained spinning dope has a high viscosity and poor spinnability, which has a great influence on the pressure resistance and draft of the spinneret in the subsequent spinning process, which is not conducive to the subsequent spinning; in addition, the ionic liquid is When dissolving cellulose, the dissolution time is longer, usually 2 to 48 hours, or even as high as 120 hours; and the dissolution temperature is relatively high, usually around 100 ° C, or even as high as 150 ° C, and the energy consumption is high; The use of ionic liquids to prepare functional fibers is still in the laboratory stage and cannot be realized on an industrial scale, which severely limits the application and development of functional fibers (including flame-retardant fibers).

Method used

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  • Preparation method of flame-retardant cellulose fiber
  • Preparation method of flame-retardant cellulose fiber
  • Preparation method of flame-retardant cellulose fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1. Preparation of 1,4-bis[1-(3-methylimidazolium)]butyl dichloride:

[0047] Under nitrogen protection at 80°C, slowly drop 1.2mol N-methylimidazole into 1mol 1,4-dichlorobutane, after the dropwise addition, reflux for 72 hours to complete the reaction, and cool the reaction solution to room temperature to obtain The product was washed with ether to remove unreacted raw materials, and a white solid was obtained, which was bis-1,4-bis[1-(3-methylimidazole)]butyl dichloride (HPLC purity was 98.8%, yield 88 %).

[0048] Two, the preparation of 1,4-bis[1-(3-methylimidazole)]butyl diperchlorate:

[0049] Dissolve 1 mol of 1,4-bis[1-(3-methylimidazolium)]butyl dichloride and 1.2 mol of lithium perchlorate in 1L of water, then stir and react at 80°C for 36 hours, then cool to room temperature, Stirring was continued at room temperature for 12 hours, the reaction solution was dispersed into an equal volume of chloroform, separated, the chloroform phase was washed with water u...

Embodiment 2

[0065] The only difference between this example and Example 1 is: 0.8 parts by mass of SFR-100 and 9.2 parts by mass of cotton pulp (the cellulose content is 99%, and the degree of polymerization is 600) are mixed uniformly, and then 100 parts by mass, 85wt % in the ionic liquid aqueous solution, all the other contents are the same as those described in Example 1.

[0066] After testing, the flame-retardant cellulose fiber prepared in this example has a breaking strength of about 3.2 cN / dtex when the monofilament fineness is 1.67 dtex; and the experiment shows that: under the same conditions, 85 wt% of 1- Butyl-3-methylimidazolium chloride, 1,4-bis[1-(3-methylimidazolium)]butyl dichloride or 1,4-bis[1-(3-methylimidazolium)] When the single ionic liquid aqueous solution of butyl diperchlorate dissolves the flame retardant and cotton pulp, it needs to be stirred at 110-130°C for 3-5 hours to obtain a stable and uniform spinning solution, and the single fiber fineness is the same...

Embodiment 3

[0068] The only difference between this example and Example 1 is that 1.2 parts by mass of SFR-100 and 8.8 parts by mass of cotton pulp (the cellulose content is 99%, and the degree of polymerization is 600) are evenly mixed, and then 100 parts by mass, 85 wt. % in the ionic liquid aqueous solution, all the other contents are the same as those described in Example 1.

[0069]After testing, the flame-retardant cellulose fiber prepared in this example has a breaking strength of about 3.4 cN / dtex when the monofilament fineness is 1.67 dtex; and the experiment shows that: under the same conditions, using 85 wt% of 1- Butyl-3-methylimidazolium chloride, 1,4-bis[1-(3-methylimidazolium)]butyl dichloride or 1,4-bis[1-(3-methylimidazolium)] When the single ionic liquid aqueous solution of butyl diperchlorate dissolves the flame retardant and cotton pulp, it needs to be stirred at 110-130°C for 3-5 hours to obtain a stable and uniform spinning solution, and the single fiber fineness is ...

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Abstract

The invention discloses a preparation method of a flame-retardant cellulosic fiber. The preparation method comprises the following steps: a) mixing a flame retardant and cellulose to obtain a mixture,and then dissolving the mixture in an aqueous solution of an ionic liquid to prepare a mixed spinning stock solution; b) filtering the stock solution of the step a), performing spinning, solidification, stretching, water washing, bleaching, oiling and drying to obtain the flame-retardant cellulose fiber; wherein the ionic liquid is prepared by mixing 1-butyl-3-methylimidazolium chloride, bi-1,4-bis [1-(3-methylimidazolyl)] butyl dichloride and bi-1,4-bis[1-(3-methylimidazolyl) butyl diperchlorate. Experiments show that the flame-retardant cellulosic fiber prepared by the method has excellentmechanical properties, flame retardancy and stability, simple preparation process and low cost, does not need any organic solvent, is environment-friendly and pollution-free, does not need special equipment and harsh conditions, is easy to realize industrial production and has extremely high practical value.

Description

technical field [0001] The invention relates to a method for preparing flame-retardant cellulose fibers, which belongs to the technical field of functional cellulose fibers. Background technique [0002] Cellulose is the most widely distributed and most abundant polysaccharide in nature, accounting for more than 50% of the carbon content in the plant kingdom, and is one of the most abundant natural organic substances in nature. Cellulose mainly comes from plants, such as cotton, wood, cotton linters, wheat straw, straw, reed, hemp, mulberry bark, etc. Among them, the cellulose content of cotton is close to 100%, which is the purest natural source of cellulose, while general wood Among them, cellulose accounts for 40-50%, and there are 10-30% hemicellulose and 20-30% lignin. As a degradable green biomaterial, natural fibers are gradually playing an increasingly important role due to their superior properties such as light weight, degradability, low cost, high modulus, and hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F2/02D01F1/07
CPCD01F1/07D01F2/02
Inventor 俞啸华郭建雄
Owner 龙丝(上海)新材料科技有限公司
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