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Carboxylation-modified nanocellulose crystal and preparation method thereof

A technology of nanocellulose and carboxylation, which is applied in the field of carboxylated modified nanocellulose crystals and its preparation, can solve the problems of lack of charge repulsion on the surface of nanocellulose, troublesome product purification and complicated product purification process, etc. Achieve the effects of improving interfacial compatibility, increasing oxidation efficiency, and enhancing mechanical properties

Inactive Publication Date: 2018-09-04
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional method of preparing nanocellulose crystals is acid hydrolysis, which requires the use of concentrated acid, and the purification of the product is cumbersome, which limits its industrial production
At present, relevant domestic researches include: Chinese patent CN102675475B discloses a preparation method of hemp fiber carboxylated cellulose nanocrystals, which uses TEMPO oxidation system for oxidation pretreatment, and then prepares cellulose nanocrystals through multi-step mechanical treatment. Complicated; Chinese patent CN105603020A discloses a method for preparing nanocellulose crystals. The method is to prepare nanocellulose crystals through multi-step mechanical treatment in the process of enzyme treatment. The operation is complicated, and nanocellulose lacks charge repulsion on the surface. , the dispersion is not stable enough; Chinese patent CN104448007A discloses a method for preparing nanocellulose, which uses formic acid to hydrolyze cellulose to prepare nanocellulose crystals, and the product purification process is relatively complicated
[0005] The mechanical treatment of nanocellulose fibers includes high-pressure homogenization, grinding, ultrasonic cell crushing, etc., but the high-pressure homogenizer is expensive and easy to block

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 70ml of acetic acid buffer solution with a pH value of 6.0 to 10g of microcrystalline cellulose, add purified water after mixing evenly to form a microcrystalline cellulose dispersion with a mass fraction of 1% of microcrystalline cellulose, and then add 11.5g of multiple oxidants , the reaction system was stirred and reacted for 5 hours at 25°C under dark conditions, and 20ml of ethanol solution with a volume fraction of 90% was added to terminate the reaction, and the reaction product was obtained by suction filtration under a pressure of 0.3psi, and washed with purified water at 75°C The reaction product is neutralized until the washing solution is neutral, and then the reaction product is washed 3 times with an ethanol solution with a volume fraction of 50% to obtain carboxylated modified microcrystalline cellulose; Water is made into a dispersion liquid with a mass fraction of 0.1%, and it is processed 10 times under a pressure of 10,000 psi using a micro-jet hi...

Embodiment 2

[0033] In 20g microcrystalline cellulose, add 160ml pH value to be 5.7 acetate buffers, add purified water after mixing evenly and be made into the microcrystalline cellulose dispersion liquid that microcrystalline cellulose mass fraction is 1.5%, then add 30g multi-component oxidizing agent, The reaction system was stirred and reacted for 9 hours at 26°C under dark conditions, and 40ml of ethanol solution with a volume fraction of 91% was added to terminate the reaction, and the reaction product was obtained by suction filtration under a pressure of 0.35psi, and the reaction was washed with purified water at 76°C Product until the washing solution is neutral, then wash the reaction product twice with a 52% ethanol solution to obtain carboxylated modified microcrystalline cellulose; then add purified water to the carboxylated modified microcrystalline cellulose Prepare a dispersion liquid with a mass fraction of 0.5%, and use a micro-jet high-pressure homogenizer to process it ...

Embodiment 3

[0037] In 30g microcrystalline cellulose, add the acetic acid buffer solution that 270mlpH value is 5.5, add purified water after mixing again and be made into the microcrystalline cellulose dispersion liquid that microcrystalline cellulose mass fraction is 2%, add the multiple oxidant of 60g again, The reaction system was stirred and reacted for 14 hours at 27°C under dark conditions, and 60ml of ethanol solution with a volume fraction of 92% was added to terminate the reaction, and the reaction product was obtained by suction filtration under a pressure of 0.4psi, and the reaction was washed with purified water at 77°C Product until the washing solution is neutral, then wash the reaction product once with a 55% ethanol solution by volume fraction to obtain carboxylated modified microcrystalline cellulose; then add purified water to the carboxylated modified microcrystalline cellulose Prepare a dispersion liquid with a mass fraction of 1.2%, and use a micro-jet high-pressure h...

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Abstract

The invention discloses a carboxylation-modified nanocellulose crystal and a preparation method thereof. The preparation method comprises the following steps: adding acetic acid buffer solution to microcrystalline cellulose, preparing microcrystalline cellulose dispersion liquid after uniformly mixing, and adding TEMPO-sodium periodate-sodium hypochlorite-sodium chlorite polybasic oxidizing agent, stirring and reacting for 5-48 h in 25-35 DEG C under a dark condition, performing suction filtration, washing, enabling a product to be prepared as dispersion liquid of which a mass fraction is 0.1-4%, and processing for 1-10 times by using a micro-jet high-pressure homogenizer, obtaining the carboxylation-modified nanocellulose crystal. An oxidation system of the preparation method is capableof selectively oxidizing in allusion to different sites of the cellulose, and improving the oxidation efficiency of the natural cellulose with a high crystallinity degree. Surface carboxyl group content, a water retention value, a carboxyl substitution degree, and the crystallinity degree of the nanocellulose crystal are remarkably improved, and the process is stable, the operation is simple and convenient. A raw material is cheap in price and abundant, and pollution-free. The carboxylation-modified nanocellulose crystal can be popularized and produced in large scale, and has the good application prospect in the fields of papermaking, foods, cosmetics, electronic products, medicine and the like.

Description

technical field [0001] The invention relates to the field of biopolymer materials, in particular to a carboxylated modified nano-cellulose crystal and a preparation method thereof. Background technique [0002] With the severe shortage of resources and people's increasing emphasis on environmental protection, it is of great significance to effectively utilize cheap and abundant green renewable resources, and cellulose, as the most abundant biodegradable polymer material in nature, can be used to Spinning, film making, production of non-woven fabrics and various cellulose derivatives. By manipulating cellulose molecules in the nanoscale range, nanocellulose can be separated by physical, chemical or biological methods. Compared with natural cellulose and microcrystalline cellulose, nanocellulose crystals have many excellent properties, such as larger Specific surface area, high crystallinity, high hydrophilicity, high modulus, high strength, ultra-fine structure and high tran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/04
CPCC08B15/04
Inventor 刘新亮孔松林嘉渭童张法宋雪萍聂双喜姚双全白云霞
Owner GUANGXI UNIV
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