Method used for preparing nano-microcrystalline cellulose via graphite oxide assistant-catalysis acid-hydrolysis

A technology of alkene-promoting acid and microcrystalline cellulose is applied in the field of preparation of nano-microcrystalline cellulose, which can solve the problem that the yield of nano-microcrystalline cellulose is not very high, achieve easy operation and control, and simple preparation process. Effect

Active Publication Date: 2015-09-16
SHANGHAI TONNOR MATERIAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the yield of nanocrystalline cellulose p

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) First, take 0.1 g of graphite oxide and place it in a beaker, add a certain amount of distilled water, and ultrasonically peel it in an ultrasonic cleaner with an ultrasonic power of 100W for 2 hours before taking it out. Add a certain amount of concentrated sulfuric acid with a mass fraction of 98% to prepare a mixed solution of sulfuric acid graphene oxide with a mass fraction of 65%. After the diluted sulfuric acid solution is cooled to room temperature, it is transferred to a three-necked flask and stirred at 400r / min. Slowly add 5g of microcrystalline cellulose powder under low temperature, start timing after mixing evenly, continue to react at 50°C water bath temperature for 1.5h, then add 400mL of distilled water to terminate the reaction.

[0016] (2) Next, centrifuge the nano-microcrystalline cellulose mixture obtained by graphene oxide-assisted catalytic sulfuric acid hydrolysis in step (1) at a speed of 11,000r / min for 10min, pour off the supernatant, and ...

Embodiment 2

[0020] (1) First, take 0.2 g of graphite oxide and place it in a beaker, add a certain amount of distilled water, and ultrasonically peel it in an ultrasonic cleaner with an ultrasonic power of 100W for 2 hours, then take it out. Add a certain amount of concentrated sulfuric acid with a mass fraction of 98% to prepare a mixed solution of sulfuric acid graphene oxide with a mass fraction of 65%. After the diluted sulfuric acid solution is cooled to room temperature, it is transferred to a three-necked flask and stirred at 400r / min. Slowly add 5g of microcrystalline cellulose powder under low temperature, start timing after mixing evenly, continue to react at 50°C water bath temperature for 1.5h, then add 400mL of distilled water to terminate the reaction.

[0021] (2) Next, centrifuge the nano-microcrystalline cellulose mixture obtained by graphene oxide-assisted catalytic sulfuric acid hydrolysis in step (1) at a speed of 11,000r / min for 10min, pour off the supernatant, and rep...

Embodiment 3

[0025] (1) First, take 0.3 g of graphite oxide and place it in a beaker, add a certain amount of distilled water, and ultrasonically peel it in an ultrasonic cleaner with an ultrasonic power of 100W for 2 hours, then take it out. Add a certain amount of concentrated sulfuric acid with a mass fraction of 98% to prepare a mixed solution of sulfuric acid graphene oxide with a mass fraction of 65%. After the diluted sulfuric acid solution is cooled to room temperature, it is transferred to a three-necked flask and stirred at 400r / min. Slowly add 5g of microcrystalline cellulose powder under low temperature, start timing after mixing evenly, continue to react at 50°C water bath temperature for 1.5h, then add 400mL of distilled water to terminate the reaction.

[0026] (2) Next, centrifuge the nano-microcrystalline cellulose mixture obtained by graphene oxide-assisted catalytic sulfuric acid hydrolysis in step (1) at a speed of 11,000r / min for 10min, pour off the supernatant, and rep...

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Abstract

The invention discloses a method used for preparing nano-microcrystalline cellulose via graphite oxide assistant-catalysis acid-hydrolysis. The method comprises following steps: a sulfuric acid graphite oxide mixed solution with a certain concentration is prepared; microcrystalline cellulose powder is added slowly with stirring; after reaction, distilled water is added to stop reaction; centrifugation extraction is carried out; collected nano-microcrystalline cellulose colloid is subjected to dialysis until pH value is changed to be 7; and at last nano-microcrystalline cellulose powder is obtained via freeze drying. The main innovative points are that: nano-microcrystalline cellulose is obtained via graphite oxide assistant-catalysis acid-hydrolysis of microcrystalline cellulose; hydrolysis of neighboring carboxy groups with phenolic hydroxyl groups is promoted by the flexible and soft layered structures of graphite oxide and abundant carbonyl groups; yield of nano-microcrystalline cellulose is increased; and the method possesses important theoretical significance and is high in practical value.

Description

technical field [0001] The invention relates to a preparation method of nano microcrystalline cellulose. This invention uses microcrystalline cellulose as a raw material, sulfuric acid as a reaction acid, and graphene oxide as a catalyst to assist in catalyzing acid hydrolysis to increase the yield of nano-microcrystalline cellulose. Background technique [0002] Cellulose is a ubiquitous and renewable resource on earth. Nano-microcrystalline cellulose is a kind of cellulose crystal obtained after the natural cellulose is treated (such as acid hydrolysis, biological enzyme hydrolysis, etc.), the amorphous region and the low-crystallinity crystalline region in the cellulose are broken. Nanocrystalline cellulose prepared from natural cellulose not only has the basic structure and properties of cellulose, but also has a huge specific surface area (~70), high crystallinity (>70%), high hydrophilicity, high Young's modulus Weight, high strength (7500MPa), ultra-fine structur...

Claims

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Application Information

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IPC IPC(8): C08J3/12C08B15/02
Inventor 唐艳军张婉清沈小创
Owner SHANGHAI TONNOR MATERIAL SCI
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