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A method for preparing nanocellulose by catalyzed hydrolysis using ionic liquid

A technology of nanocellulose and ionic liquids, which is applied in fiber raw material processing, textiles and papermaking, etc., can solve the problems of severe equipment corrosion and large environmental pollution, achieve low equipment corrosion, small environmental pollution, and overcome equipment corrosion Effect

Inactive Publication Date: 2015-08-12
FUJIAN AGRI & FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the conventional technology for preparing NCC generally involves an acid treatment process or an alkali treatment process, which seriously corrodes equipment and pollutes the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Weigh 2g of pulp and add it to 50ml of ionic liquid 1-allyl-3-methylimidazolium chloride [Amim]Cl, raise the temperature to 70°C under the action of ultrasonic waves with a power of 300W, and react for 1h. Quickly freeze with liquid nitrogen for 20 minutes; then slowly thaw, and raise the temperature to 70°C. After repeating the liquid nitrogen quick freezing-slow melting-heating operation twice, the ionic liquid will be extracted from the suspension, and the remaining liquid will be further purified by high-speed centrifugation to obtain a milky white cellulose colloid. After vacuum freeze-drying for 24 hours, the nano Cellulose powder.

[0014] The Morfi Compact fiber morphology analyzer produced by Techpap Company in France was used to analyze the morphology of cellulose. The measured average length of the nanocellulose is 589 nm; the average width is 46 nm; the length is mainly distributed in the range of 450-750 nm, and the length of 550-650 nm accounts for 93.2%....

Embodiment 2

[0016] Weigh 5g of pulp and add it to 100ml of ionic liquid 1-octyl-3-methylimidazolium bromide [Omim]Br, raise the temperature to 50°C under the action of ultrasonic waves with a power of 500W, and react for 3 hours, then use Quickly freeze in liquid nitrogen for 20 minutes; then slowly thaw, and raise the temperature to 50°C. After repeating the liquid nitrogen quick freezing-slow melting-heating operation 5 times, the ionic liquid will be extracted from the suspension, and the remaining liquid will be further purified by high-speed centrifugation to obtain milky white cellulose colloid. After vacuum freeze-drying for 24 hours, the nano Cellulose powder.

[0017] The Morfi Compact fiber morphology analyzer produced by Techpap Company in France was used to analyze the morphology of cellulose. The average length of the nanocellulose was measured to be 381 nm; the average width was 32 nm; the length was mainly distributed in the range of 300-450 nm, and the length of 350-400 n...

Embodiment 3

[0019] Weigh 3g of pulp and add it to 80ml of 1-butyl-3-methylimidazolium chloride [Bmim]Cl, raise the temperature to 60°C under the action of ultrasonic waves with a power of 400W, and react for 2 hours. Nitrogen rapid freezing treatment for 20min; then slowly thawed, and the temperature was raised to 60°C. After repeating the liquid nitrogen quick freezing-slow melting-heating operation 4 times, the ionic liquid will be extracted from the suspension, and the remaining liquid will be further purified by high-speed centrifugation to obtain a milky white cellulose colloid. After vacuum freeze-drying for 24 hours, the nano Cellulose powder.

[0020] The Morfi Compact fiber morphology analyzer produced by Techpap Company in France was used to analyze the morphology of cellulose. The measured average length of the nanocellulose is 508 nm; the average width is 39 nm; the length is mainly distributed in the range of 400-650 nm, and the length of 450-550 nm accounts for 94.3%.

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PUM

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Abstract

The invention discloses a method for preparing nano-cellulose by catalytic hydrolysis of ionic liquid. Pulp is added to ionic liquid, and the temperature is raised to 50-70°C under the action of ultrasonic waves. After reacting for 1-3 hours, it is quickly frozen with liquid nitrogen. Treat for 20 minutes; then melt slowly, and raise the temperature to 50~70°C; repeat the liquid nitrogen quick freezing-slow melting-heating operation several times, extract the ionic liquid from the suspension, and purify the remaining liquid by high-speed centrifugation to obtain milky white The cellulose colloid was subjected to vacuum freeze-drying for 24 hours to obtain nanocellulose powder. The invention has the advantages of less corrosion to equipment, less environmental pollution, less damage to cellulose degradation, high yield of nano cellulose, reusable ionic liquid, etc., and overcomes the disadvantages of preparing nano cellulose with traditional liquid acid.

Description

technical field [0001] The invention belongs to the field of biomass cellulose, and in particular relates to a method for preparing nanometer cellulose by catalytic hydrolysis of ionic liquid. Background technique [0002] Cellulose is a linear polymer composed of D-glucopyranose rings linked by β-1,4-glycosidic bonds, and it is a rich renewable resource in nature. Under appropriate environmental conditions, it can break glycosides, reduce the degree of polymerization, and finally form nanocrystalline fibers (nanocrystalline cellulose, NCC for short). NCC has a huge specific surface area, the number of surface atoms and special surface effects, and still has the crystal form and properties of cellulose. At present, NCC has been used as a drug carrier, nano-enhancer, paint thickener, dispersant, pharmaceutical excipient, food additive, cosmetic matrix, membrane filter, etc. [0003] At present, the conventional technology for preparing NCC generally involves acid treatment ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D21C5/00
Inventor 陈孝云陆东芳陈星常鼎伟高骁敏
Owner FUJIAN AGRI & FORESTRY UNIV
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