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Method for preparing cellulose nano microcrystal through solvothermal hydrolysis assisted mechanical grinding peeling

A technology of nano-microcrystals and auxiliary machinery, which is applied in the field of preparation of cellulose nano-crystals, can solve problems such as shortening the process flow, achieve the effects of shortening the process flow, reducing the amount of acid, and saving the dialysis link

Inactive Publication Date: 2018-12-14
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for preparing cellulose nanocrystals by solvent thermal hydrolysis assisted by mechanical sand milling, which overcomes the need to use a large amount of acid solution in the existing acid hydrolysis method, and the time-consuming dialysis and waste acid treatment in the later stage This method greatly reduces the amount of acid used and solves the big problem of waste acid treatment. At the same time, it saves the dialysis link, saves time, shortens the process flow, responds to the new concept of green environmental protection, and greatly expands Expand the range of application of cellulose microcrystals, so that it has a better application prospect

Method used

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  • Method for preparing cellulose nano microcrystal through solvothermal hydrolysis assisted mechanical grinding peeling
  • Method for preparing cellulose nano microcrystal through solvothermal hydrolysis assisted mechanical grinding peeling
  • Method for preparing cellulose nano microcrystal through solvothermal hydrolysis assisted mechanical grinding peeling

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Take microcrystalline cellulose 5g, add microcrystalline cellulose in the mixed solvent (v / v=65 / 35) of 15mL ethanol and water and add the sulfuric acid of 100mM as catalyst, in polytetrafluoroethylene high-temperature high-pressure reaction kettle 200 Under the condition of ℃, react for 60min. Then add all the reacted solid-liquid mixture into a sand mill, then add 200g of zirconium beads and grind for 10 hours at 20°C to obtain a white jelly, add the white jelly to 100mL distilled water and stir evenly, and use deionized The water was centrifuged at 9000r / min for 5min and washed repeatedly by centrifugation for 5 times, the ethanol was removed, and the white precipitate was collected. After the white precipitate was shaken with water, the cellulose nanocrystal suspension obtained was ultrasonicated for 40min at a power of 100W. A cellulose nanocrystal suspension with uniform size is obtained. The yield is 75.6%, the diameter is 8-12 nanometers, and the length is about...

Embodiment 2

[0033] Take microcrystalline cellulose 5g, add microcrystalline cellulose in the mixed solvent (v / v=65 / 35) of 25mL ethanol and water and add the sulfuric acid of 80mM as catalyst, in polytetrafluoroethylene high-temperature high-pressure reactor 190 Under the condition of ℃, react for 80min. Then put all the reacted solid-liquid mixture into a sand mill, then add 150g of zirconium beads, and grind for 8 hours at 40°C to obtain a white jelly, add the white jelly to 100mL distilled water and stir evenly, use Ionized water was centrifuged at 9000r / min for 5min and washed with water for 4 times, ethanol was removed, and the white precipitate was collected. After the white precipitate was shaken with water, the cellulose nanocrystal suspension obtained was ultrasonicated for 30min at a power of 200W, that is, A suspension of cellulose nanocrystals with uniform size can be obtained. Yield 74.9%. The diameter is 9-15 nanometers, and the length is about 200-310 nanometers.

[0034]...

Embodiment 3

[0036] Take microcrystalline cellulose 5g, add microcrystalline cellulose in the mixed solvent (v / v=65 / 35) of 50mL ethanol and water and add the sulfuric acid of 60mM as catalyst, in polytetrafluoroethylene high-temperature high-pressure reactor 170 Under the condition of ℃, react for 120min. Then put all the reacted solid-liquid mixture into a sand mill, then add 150g of zirconium beads, and grind for 6 hours at 60°C to obtain a white jelly, add the white jelly to 100mL distilled water and stir evenly, use Ionized water was centrifuged at 9000r / min for 5min and washed 4-5 times by centrifugation repeatedly, the ethanol was removed, and the white precipitate was collected. After the white precipitate was shaken with water, the cellulose nanocrystal suspension obtained was ultrasonicated for 20min at a power of 300W. , the cellulose nanocrystal suspension with uniform size can be obtained. Yield 78.5%. The diameter is 9-13 nanometers, and the length is about 220-280 nanometer...

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Abstract

The invention relates to a method for preparing a cellulose nano microcrystal through solvothermal hydrolysis assisted mechanical grinding peeling. The method comprises the following steps: by takingmicrocrystal cellulose as a raw material, putting the microcrystal cellulose into a mixed solvent, carrying out a solvothermal reaction; by taking an acid as a catalyst, further putting zirconium beads into substances after the reaction to implement grinding so as to obtain a colloid substance, uniformly stirring the colloid substance in distilled water, carrying out centrifugal washing, collecting precipitate, and carrying out dispersion, thereby obtaining the cellulose nano microcrystal. Compared with a conventional acid hydrolysis method, the method has the advantages that the amount of theacid is greatly reduced, the difficulty of acid treatment is solved, a dialysis procedure is avoided, the time is shortened, the process course is shortened, and the method meets the new idea of green and environment protection. The prepared cellulose nano microcrystal has good thermal stability, the decomposition temperature of the cellulose nano microcrystal is higher than a conventional acid hydrolysis decomposition temperature (257 DEG C), and can be up to 288 DEG C. The application range of the cellulose nano microcrystal can be greatly widened, and the cellulose nano microcrystal has good application prospects.

Description

technical field [0001] The invention belongs to the field of preparation of cellulose nano crystals, in particular to a method for preparing cellulose nano crystals by solvent thermal hydrolysis assisted by mechanical sand milling. Background technique [0002] Cellulose is a natural organic polymer widely present in nature, which accounts for more than 50% of the carbon content in the plant kingdom. The cellulose content of cotton is the purest natural source of cellulose. In general wood, cellulose accounts for 40-50%, and there are 10-30% hemicellulose and 20-30% lignin. Microcrystalline cellulose (cellulosemicrociystalline), the main component is β-1,4-glucosidic bonded linear polysaccharides. The degree of polymerization is about 3000-10000 glucose molecules. In general plant fibers, microcrystalline cellulose accounts for about 73% of the cellulose content, and the other 30% is amorphous cellulose. The following formula is the molecular structure of microcrystallin...

Claims

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Application Information

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IPC IPC(8): C08B15/02
CPCC08B15/02
Inventor 侯爱芹高爱芹谢孔良唐靖陈煌煌王菊
Owner DONGHUA UNIV
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