Method for preparing composite fibers in ionic liquid medium

An ionic liquid and composite fiber technology, which is applied in fiber treatment, plant fibers, animal fibers, etc., can solve the problems of low grafting rate and low degradability of composite fibers, and achieve the effects of improving grafting rate and simple preparation process.

Active Publication Date: 2016-05-04
JIANGSU UNIV OF SCI & TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] Purpose of the invention: In view of the shortcomings in the prior art that the current composite fiber materials are reproducible, low in degradability, and the grafting rate of composite fibers prepared from cellulose materials and silk fibroin in the prior art is low, the present invention provides an ion Preparation method of composite fiber in liquid medium

Method used

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  • Method for preparing composite fibers in ionic liquid medium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Take an appropriate amount of microcrystalline cellulose in a beaker and dry at 80°C for 4-6 hours.

[0024] (2) Take 5ml of ionic liquid ([EMIM][DEP]) and 5ml of nitric acid solution with a mass percentage concentration of 65wt%-68wt%, add them to a 30ml glass bottle successively, and then add 0.15g of dried micro Crystalline cellulose and 0.15g NaNO 2 For powder, heat in an oil bath in a collector-type constant temperature heating magnetic stirrer and assisted by magnetic stirring, and react at a constant temperature of 70°C for 1-2h; after the reaction is completed, use deionized water three times the volume of the mixed solution of nitric acid and ionic liquid to slowly add And carry out suction filtration and washing 5-7 times until the pH value of the filtrate is 6-7, and dry at 80° C. for 24 hours to obtain carboxycellulose.

[0025] (3) Take 3.75g of ionic liquid ([EMIM][DEP]) and 0.15g of carboxy cellulose and add it to a 20ml iodine measuring bottle a, an...

Embodiment 2

[0033] (1) Take an appropriate amount of microcrystalline cellulose in a beaker and dry at 80°C for 4-6 hours.

[0034] (2) Take 5ml of ionic liquid ([EMIM][DEP]) and 5ml of nitric acid solution with a mass percentage concentration of 65wt%-68wt%, add them to a 30ml glass bottle successively, and then add 0.15g of dried micro Crystalline cellulose and 0.15g NaNO 2 For powder, heat in an oil bath in a collector-type constant temperature heating magnetic stirrer and assisted by magnetic stirring, and react at a constant temperature of 70°C for 1-2h; after the reaction is completed, use deionized water three times the volume of the mixed solution of nitric acid and ionic liquid to slowly add And carry out suction filtration and washing 5-7 times until the pH value of the filtrate is 6-7, and dry at 80° C. for 24 hours to obtain carboxycellulose.

[0035] (3) Take 3.75g of ionic liquid ([EMIM][DEP]) and 0.15g of carboxy cellulose and add it to a 20ml iodine measuring bottle a, an...

Embodiment 3

[0043] (1) Take an appropriate amount of microcrystalline cellulose in a beaker and dry at 80°C for 4-6 hours.

[0044] (2) Take 5ml of ionic liquid ([BMIM][Cl]) and 5ml of nitric acid solution with a mass percentage concentration of 65wt%-68wt%, and add them to a 30ml glass bottle successively, and then add 0.15g of dried microbes to the bottle successively. Crystalline cellulose and 0.15g NaNO 2 Powder, heated in an oil bath and magnetically stirred in a collector-type constant temperature heating magnetic stirrer, and reacted at a constant temperature of 90°C for 1-2h; after the reaction was completed, slowly added deionized water three times the volume of the mixed solution of nitric acid and ionic liquid and Suction filtration and washing for 5-7 times until the pH value of the filtrate is 6-7, and drying at 60°C for 24 hours to obtain carboxycellulose.

[0045] (3) Get 3.75g ionic liquid ([BMIM][Cl]) and 0.15g carboxycellulose and add successively in the 20ml iodine mea...

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Abstract

The invention discloses a method for preparing composite fibers in an ionic liquid medium. The method comprises the following steps: (1) oxidating cellulose into carboxyl cellulose in an oxidation system prepared from ionic liquid, nitric acid and NaNO2, and preparing a carboxyl cellulose solution; (2) subjecting silkworm cocoons to soda boiling, degumming, LiBr dissolving, dialysis and vacuum freeze drying so as to obtain silk fibroin, and then, preparing a silk fibroin solution in ionic liquid; (3) grafting the carboxyl cellulose to the silk fibroin in ionic liquid, thereby obtaining the composite fibers. According to the method, the ionic liquid serves as a solvent, cellulosic materials and the silkworm cocoons serve as raw materials, the chemical principle of amidation reaction is adopted, the preparation process is simple, the reaction is green, environment-friendly and pollution-free, the ionic liquid solvent can be recovered and reused through rotary-evaporation drying, and the recovery rate reaches 98%. The reaction system only needs an isothermal reaction of 1 to 2 hours, the percentage of grafting of the cellulosic materials reaches 21% to the maximum, and the composite fibers are excellent in mechanical properties, crinkle resistance, wear resistance and hygroscopic property and are degradable and reproducible.

Description

technical field [0001] The invention belongs to the technical field of biochemical industry, and in particular relates to a preparation method of a composite fiber in an ionic liquid medium. Background technique [0002] In recent years, the preparation of cellulose composite fiber materials has become a research hotspot at home and abroad. Most of the cellulose composite fiber materials are composite fibers synthesized with chemical reagents as reinforcing materials and cellulose materials as the matrix. Traditional fiber composite fiber materials are composed of chemical fibers such as polypropylene fiber, glass fiber, aramid fiber or carbon fiber. They generally have problems such as large energy consumption, high cost, and easy pollution of the environment. Compared with chemical fibers, renewable composite fibers have the advantages of being cheap, recyclable, and degradable, and have the strength and stiffness of ordinary fibers, and have a smaller specific gravity, hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F8/02D06M13/352D06M101/06D06M101/12
CPCD01F8/02D06M13/352D06M2101/06D06M2101/12
Inventor 张大钊李强季更生毛杨杨屠洁颜辉
Owner JIANGSU UNIV OF SCI & TECH
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