Method for preparing nanometer microcrystalline cellulose by combining acid hydrolysis and ultrasonic treatment

A nano-crystal, ultrasonic treatment technology, applied in fiber raw material processing, textiles and papermaking, etc., to achieve the effects of easy operation and control, simple preparation process, and improved yield

Active Publication Date: 2013-06-26
SHANGHAI TONNOR MATERIAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the environmental pollution caused by acid hydrolysis has become a bottleneck restricting the development of nanocrystalline cellulose

Method used

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  • Method for preparing nanometer microcrystalline cellulose by combining acid hydrolysis and ultrasonic treatment

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 1. Sulfuric acid hydrolysis of cellulose: First, add concentrated sulfuric acid into distilled water to prepare a sulfuric acid solution with a mass concentration of 65%. The sulfuric acid solution to be diluted is cooled to room temperature. Slowly add TONNOR EM100 powder provided by Shanghai Tonghua New Material Technology Co., Ltd., and start timing after mixing evenly. After reacting for 120 minutes, add water to terminate the reaction, and obtain a mixed solution of nano-microcrystalline cellulose prepared by acid hydrolysis. 2. Preparation of nano-microcrystalline cellulose colloid: first, the nano-microcrystalline cellulose mixture prepared by acid hydrolysis obtained in step 1 was centrifuged in a centrifuge whose rotational speed was set to 11000 r / min and time was set to 10 min, and centrifuged for 3 The nano-microcrystalline cellulose colloid can be collected in ~6 times, and the collected nano-microcrystalline cellulose colloid is placed in a dialysis bag wit...

Embodiment 2

[0015] 1. Sulfuric acid hydrolysis and ultrasonic treatment of cellulose: First, add concentrated sulfuric acid into distilled water to prepare a sulfuric acid solution with a mass concentration of 65%. The sulfuric acid solution to be diluted is cooled to room temperature. At the same time, slowly add TONNOR EM100 powder provided by Shanghai Tonghua New Material Technology Co., Ltd., and start timing after mixing evenly. After 110 minutes of reaction, 10 minutes of ultrasonic cleaning in an ultrasonic cleaner with a power of 100W, water is added to terminate the reaction, and acid hydrolysis and Ultrasonic treatment of co-prepared nano-microcrystalline cellulose mixture. 2. Preparation of nano-microcrystalline cellulose colloid: first, the nano-microcrystalline cellulose mixture prepared in step 1 by acid hydrolysis and ultrasonic treatment was centrifuged in a centrifuge with a speed of 11,000 r / min and a time of 10 min. After separation and centrifugation for 3 to 6 times, ...

Embodiment 3

[0017] 1. Sulfuric acid hydrolysis and ultrasonic treatment of cellulose: First, add concentrated sulfuric acid into distilled water to prepare a sulfuric acid solution with a mass concentration of 65%. The sulfuric acid solution to be diluted is cooled to room temperature. At the same time, slowly add TONNOR EM100 powder provided by Shanghai Tonghua New Material Technology Co., Ltd., and start timing after mixing evenly. After 100 minutes of reaction, 20 minutes of ultrasonic cleaning in an ultrasonic cleaner with a power of 100W, water is added to terminate the reaction, and acid hydrolysis and Ultrasonic treatment of co-prepared nano-microcrystalline cellulose mixture. The reaction was terminated by adding water, and the nano-microcrystalline cellulose mixed solution prepared by acid hydrolysis and ultrasonic treatment was obtained. 2. Preparation of nano-microcrystalline cellulose colloid: first, the nano-microcrystalline cellulose mixture prepared in step 1 by acid hydrol...

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Abstract

The invention discloses a method for preparing nanometer microcrystalline cellulose by combining acid hydrolysis and ultrasonic treatment. The method comprises the following steps of: preparing a sulfuric acid solution with certain concentration; slowly adding tonnor EM100 powder, which is provided by Shanghai Tonnor Material Science Co., Ltd, to the sulfuric acid solution while stirring; ultrasonically treating for certain time after the tonnor EM 100 powder is completely dissolved; adding a certain amount of distilled water to stop the reaction after the ultrasonic treatment; carrying out centrifugal separation onto the obtained mixed solution; dialyzing the collected nanometer microcrystalline cellulose colloid until the collected nanometer microcrystalline cellulose colloid is neutral; and finally refrigerating and freeze-drying the dialyzed nanometer microcrystalline cellulose colloid to obtain the nanometer microcrystalline cellulose powder. The method for preparing nanometer microcrystalline cellulose by combining acid hydrolysis and ultrasonic treatment is simple to operate, free of damages to the cellulose degradation and easy to control; and more importantly, the environment pollution can be reduced in comparison with the pure acid hydrolysis.

Description

technical field [0001] The invention relates to a preparation method of nano microcrystalline cellulose. This invention uses TONNOR EM100 powder provided by Shanghai Tonghua New Material Technology Co., Ltd. as the raw material, sulfuric acid as the reaction acid, and adopts the synergistic method of acid hydrolysis and ultrasonic to prepare nanocrystalline cellulose. Background technique [0002] In today's severe situation of rapid energy consumption and environmental degradation in the world, the development of renewable energy is of great strategic significance. As an extremely abundant renewable green polymer material in nature, cellulose has become one of the targets of human research. However, it has some disadvantages in performance, such as chemical corrosion resistance, low strength, etc., and its physical form also limits its application range. However, if it is prepared into nano-microcrystalline cellulose, its performance can be optimized to a large extent, so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21C5/00
Inventor 唐艳军杨淑杰张楠
Owner SHANGHAI TONNOR MATERIAL SCI
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