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Method for preparing cellulose and graphene compound short fibers

A graphene composite, cellulose technology, applied in the direction of single-component cellulose rayon, fiber chemical characteristics, spinning solution preparation, etc. Application and development of functional fibers, pressure resistance of spinnerets and effects of drafting, etc., to achieve the effects of excellent antistatic properties, good bonding firmness, and excellent antibacterial properties

Active Publication Date: 2019-01-11
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 the industrial scale cannot be achieved, which severely limits the application and development of functional fibers (including cellulose-graphene composite fibers).

Method used

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  • Method for preparing cellulose and graphene compound short fibers
  • Method for preparing cellulose and graphene compound short fibers
  • Method for preparing cellulose and graphene compound short fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 1. Preparation of 1,4-bis[1-(3-methylimidazolium)]butyl dichloride:

[0052] 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 %).

[0053] Two, the preparation of 1,4-bis[1-(3-methylimidazole)]butyl diperchlorate:

[0054] 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

[0073] The difference between this embodiment and Example 1 is only: 0.5 mass parts of silicon oxide (particle diameter is about 100nm), 0.015 mass parts of graphene oxide and 9.485 mass parts of cotton pulp (cellulose content is 99%, polymerized degree is 600) after mixing evenly, add 100 parts by mass, 85wt% in the ionic liquid aqueous solution, and the remaining contents are all the same as described in Example 1.

[0074] After testing, the cellulose graphene composite short fiber prepared in this example has a breaking strength of about 3.6 cN / dtex when the single filament fineness is 1.5 dtex; 1-Butyl-3-methylimidazolium chloride, 1,4-bis[1-(3-methylimidazolium)]butyl dichloride or 1,4-bis[1-(3-methylimidazolium) )] When a single ionic liquid aqueous solution of butyl diperchlorate dissolves graphene oxide 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-filament fineness In the case of t...

Embodiment 3

[0077] The difference between this embodiment and Example 1 is only: 0.5 mass parts of silicon oxide (particle diameter is about 100nm), 0.025 mass parts of graphene and 9.475 mass parts of cotton pulp (cellulose content is 99%, polymerization degree 600) after mixing evenly, add 100 parts by mass, 85 wt% of the ionic liquid aqueous solution, and the rest of the content is the same as that described in Example 1.

[0078] After testing, the cellulose graphene composite short fiber prepared in this example has a breaking strength of about 3.8 cN / dtex when the single filament fineness is 1.5 dtex; 1-Butyl-3-methylimidazolium chloride, 1,4-bis[1-(3-methylimidazolium)]butyl dichloride or 1,4-bis[1-(3-methylimidazolium) )] When a single ionic liquid aqueous solution of butyl diperchlorate dissolves cotton pulp, graphene and cotton pulp, it needs to be stirred at 110-130°C for 3-5 hours to obtain a stable and uniform spinning stock solution, and in When the monofilament fineness is...

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Abstract

The invention discloses a method for preparing cellulose and graphene compound short fibers. The method comprises the following steps: (a) mixing a dispersant, graphene oxide and cellulose, dissolvingin an ionic liquid aqueous solution to prepare a blend spinning solution, wherein the addition amount of the graphene oxide is 0.1-0.3 percent by weight of the cellulose; and (b) filtering, spinning,solidifying, stretching, rinsing, bleaching, oiling, cutting and drying the blend spinning solution to obtain the cellulose and graphene compound short fibers, wherein the ionic liquid is prepared bymixing 1-butyl-3-methylimidazolium chloride, bi-1,4-bis[1-(3-methylimidazole)] butyldichloride and bi-1,4-bis[1-(3-methylimidazole)] butyl diperchlorate. Experiments indicate that the cellulose and graphene compound short fibers have excellent mechanical performance, anti-electrostatic performance and stable performance, and are simple in preparation process, low in cost, environment-friendly andpollution-free.

Description

technical field [0001] The invention relates to a preparation method of cellulose graphene composite short fibers, belonging 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, ...

Claims

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Application Information

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IPC IPC(8): D01F2/00D01F1/10D01F1/09D01D1/02
CPCD01D1/02D01F1/09D01F1/103D01F2/00
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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