Preparation method of cellulose nanocrystals

A nanocrystal and cellulose technology, applied in the field of preparation of cellulose nanocrystals, can solve the problems of low yield, high energy consumption, and long preparation cycle, and achieve the effects of less environmental pollution, uniform particle size distribution, and short preparation cycle

Active Publication Date: 2021-04-16
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Another object of the present invention is to solve the problems of high energy consumption, low yield, and long preparation cycle in the existing nanocellulose preparation process, and use a cellulose solvent system to disassemble the strong hydrogen bond network structure of lignocellulose under mild conditions The idea of ​​​​providing a mild and controllable method for the preparation of cellulose nanocrystals

Method used

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  • Preparation method of cellulose nanocrystals
  • Preparation method of cellulose nanocrystals
  • Preparation method of cellulose nanocrystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Weigh 0.05g of microcrystalline cellulose powder as cellulose raw material and slowly add it into a 10mL glass bottle, add 1g of 40% TBPH (tetrabutylphosphine hydroxide, the same below) with a mass fraction of 1g and add a magnetic rotor, put the glass bottle into 50 ℃ in a constant temperature oil bath for 1 h, and the samples were mixed evenly by magnetic stirring during the processing. After the treatment, add 10 mL of deionized water to regenerate the cellulose, pour the regenerated cellulose into a beaker, and filter and clean it with a suction filter. After repeated washing 3 times, 50 mL of deionized water was added to the washed regenerated cellulose again. The cleaned regenerated cellulose was ultrasonically dispersed with an ultrasonic cell pulverizer, the ultrasonic power was 1200W, and the ultrasonic time was 4min. A mixed solution of cellulose nanocrystals was prepared after ultrasonication. The prepared cellulose nanocrystal mixed solution was centrifuge...

Embodiment 2

[0042] Weigh 0.05g of bagasse pulp as cellulose raw material and slowly add it into a 10mL glass bottle, add 1g of TBPH with a mass fraction of 40% and add a magnetic rotor, put the glass bottle in a constant temperature oil bath at 50°C for 1 hour, and process The samples were mixed homogeneously by magnetic stirring. After the treatment, add 10 mL of deionized water to regenerate the cellulose, pour the regenerated cellulose into a beaker, and filter and clean it with a suction filter. After repeated washing 3 times, 50 mL of deionized water was added to the washed regenerated cellulose again. The cleaned regenerated cellulose was ultrasonically dispersed with an ultrasonic cell pulverizer, the ultrasonic power was 1200W, and the ultrasonic time was 4min. A mixed solution of cellulose nanocrystals was prepared after ultrasonication. The prepared cellulose nanocrystal mixed solution was centrifuged at a speed of 8000 r / min for 5 minutes in a high-speed centrifuge. Pour out...

Embodiment 3

[0044]Weigh 0.05g of the cellulose-rich material prepared at a temperature of 240°C in the oil pan in the component separation (the preparation method of the cellulose-rich material refers to Example 16) as the cellulose raw material and slowly add it to a 10mL glass bottle, adding 1g mass fraction It is 40% TBPH and a magnetic rotor is added, and the glass bottle is placed in a constant temperature oil bath at 50°C for 1 hour. During the treatment, the sample is mixed evenly by magnetic stirring. After the treatment, add 10 mL of deionized water to regenerate the cellulose, pour the regenerated cellulose into a beaker, and filter and clean it with a suction filter. After repeated washing 3 times, 50 mL of deionized water was added to the washed regenerated cellulose again. The cleaned regenerated cellulose was ultrasonically dispersed with an ultrasonic cell pulverizer, the ultrasonic power was 1200W, and the ultrasonic time was 4min. A mixed solution of cellulose nanocrysta...

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Abstract

The invention discloses a method for preparing cellulose nanocrystals, comprising: step 1, pretreated biomass raw materials are separated to obtain cellulose-rich materials; step 2, cellulose-rich materials are used as cellulose raw materials and fibers Vegetable solvent TBPH or NMMO aqueous solution is mixed to obtain mixture; The mass concentration of TBPH is 30~60%, the mass concentration of NMMO is 75~85%; The amount of cellulose raw material added is 5%~10% of cellulose solvent quality; Step 3, Keep the mixture at 40-60°C for 1 hour; step 4, add deionized water to the mixture to obtain regenerated cellulose; step 5, filter and wash the regenerated cellulose and mix it with deionized water; step 6, carry out ultrasonic dispersion; step 7. The clear liquid after centrifugation is dried to obtain cellulose nanocrystals. The method of the invention has simple technological process, less environmental pollution, short preparation period and mild reaction conditions. The particle size distribution of the cellulose nano crystal prepared by the invention is uniform, the crystal diameter is 5-15nm, the length is 30-200nm, and the yield is as high as 70-80%.

Description

technical field [0001] The invention relates to the technical field of cellulose treatment, and more specifically, the invention relates to a preparation method of cellulose nanocrystals. Background technique [0002] Nanocellulose is a linear organic polymer nanomaterial extracted from natural fiber materials such as agricultural and forestry biomass. It mainly includes two types of nanofibrillated cellulose and cellulose nanocrystals. The unique nanofibrous structure of nanocellulose makes it have physical and chemical properties such as high specific surface area, low density, high mechanical strength, low thermal expansion coefficient, and degradability. It has broad application prospects in fine chemicals, biomedicine, and advanced materials. [0003] At present, the preparation methods of nanocellulose mainly include physical methods, chemical methods and biological methods, specifically biological enzymatic hydrolysis method, high-pressure homogenization method, steam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B15/02
CPCC08B15/02
Inventor 程芳超欧阳土龙农育红柯少秋王志气
Owner GUANGXI UNIV
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