Preparation method of antibacterial cellulose fibers

A cellulose fiber and cellulose technology, applied in the direction of single-component cellulose rayon, fiber chemical characteristics, spinning solution preparation, etc., can solve the long-term, usually 2 to 48 hours, even up to 120 hours, the limit The application and development of functional fiber antibacterial fiber, the influence of spinneret pressure resistance and drafting, etc., to achieve the effects of shortened dissolution time, excellent antibacterial function, and reduced dissolution temperature

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 antibacterial fibers).

Method used

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  • Preparation method of antibacterial cellulose fibers
  • Preparation method of antibacterial cellulose fibers
  • Preparation method of antibacterial cellulose fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. Preparation of 1,4-bis[1-(3-methylimidazolium)]butyl dichloride:

[0046] 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 %).

[0047] Two, the preparation of 1,4-bis[1-(3-methylimidazole)]butyl diperchlorate:

[0048] 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

[0066] The only difference between this example and Example 1 is: 0.5 mass parts of silicon oxide (particle diameter is about 100nm), 0.09 mass parts of medical zinc oxide and 9.41 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.

[0067] After testing, the antibacterial cellulose fiber prepared in this example has a breaking strength of about 3.4 cN / dtex when the monofilament fineness is 2.5 dtex; and the experiment shows that: under the same conditions, using 85 wt% of 1-butylene Base-3-methylimidazolium chloride, 1,4-bis[1-(3-methylimidazolium)]butyl dichloride or 1,4-bis[1-(3-methylimidazolium)]butyl When a single ionic liquid aqueous solution based on diperchlorate dissolves zinc oxide and cotton pulp, it needs to be stirred at 110-130°C for 3-5 hours to obtain a stable and uniform spi...

Embodiment 3

[0070] 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 nano silver (particle diameter is about 100nm) and 9.485 mass parts of cotton pulp (cellulose The content is 99%, the degree of polymerization is 600), and after mixing evenly, add 100 parts by mass and 85 wt% of the ionic liquid aqueous solution, and the rest of the content is the same as that described in Example 1.

[0071] After testing, the antibacterial cellulose fiber prepared in this example has a breaking strength of about 3.0 cN / dtex when the monofilament fineness is 2.5 dtex; and the experiment shows that under the same conditions, using 85 wt% of 1-butyl Base-3-methylimidazolium chloride, 1,4-bis[1-(3-methylimidazolium)]butyl dichloride or 1,4-bis[1-(3-methylimidazolium)]butyl When a single ionic liquid aqueous solution based on diperchlorate dissolves nano-silver and cotton pulp, it needs to be stirred at 110-...

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Abstract

The invention discloses a preparation method of antibacterial cellulose fibers. The preparation method comprises the following steps: a) after mixing a dispersant, an antibacterial agent and cellulose, dissolving a mixture in an ionic liquid water solution to prepare a mixed spinning raw solution, wherein the adding amount of the antibacterial agent is 0.1 to 1 weight percent of the cellulose; andb) filtering the mixed spinning raw solution, spinning, condensing, stretching, washing with water, bleaching, applying oil and drying to obtain the antibacterial cellulose fibers. The ionic liquid is obtained by mixing 1-butyl-3-methylimidazolium chloride, bi1,4-di[1-(3-methylimidazolium)]butyl dichloride and bi1,4-di[1-(3-methylimidazolium)]butyl diperchlorate. An experiment shows that the antibacterial cellulose fibers prepared by the invention have excellent mechanical property, antibacterial property and stability property; and a preparation process is simple, is low in cost, is environmentally friendly and has no pollution.

Description

technical field [0001] The invention relates to a preparation method of antibacterial cellulose 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, and high st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F2/00D01F1/10D01D1/02
CPCD01D1/02D01F1/103D01F2/00
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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