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Preparation method for water-redispersible nanocrystalline cellulose

A cellulose, redispersion technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of harsh reaction conditions, limited application scope, etc., achieve environmentally friendly operation, improve water availability. Redispersibility, the effect of broad industrial application prospects

Active Publication Date: 2020-02-21
克林斯曼新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above reaction conditions are relatively harsh, so the application range of the above two methods in actual production is limited to a certain extent. Therefore, it is particularly important to develop a simple and environmentally friendly preparation method for water-redispersible cellulose nanocrystals.

Method used

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  • Preparation method for water-redispersible nanocrystalline cellulose
  • Preparation method for water-redispersible nanocrystalline cellulose
  • Preparation method for water-redispersible nanocrystalline cellulose

Examples

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preparation example Construction

[0022] A method for preparing water-redispersible cellulose nanocrystals, comprising the following steps:

[0023] 1) Disperse 3-5g of fiber material in 35-40ml of acid solution (the ratio of fiber material to acid solution is 1:8-11g / ml, in this ratio, the unit of fiber material is g, and the unit of acid solution is ml) , the acid solution is hydrochloric acid or sulfuric acid with an acid concentration of less than 0.1%, and the reaction is carried out under heating, pressure and stirring conditions; the reaction temperature is 150-180°C, the reaction time is 50-80min, and the reaction pressure is 5-20MPa; filtration is not hydrolyzed Cellulose obtains filtrate for subsequent use;

[0024] 2) adding the obtained filtrate to the organic solvent under stirring, centrifuging, and collecting the centrifugal precipitate;

[0025] 3) drying the obtained precipitate until obtaining a cellulose nanocrystalline solid with an initial water content of 10%-20% by weight.

[0026] The...

Embodiment 1

[0029] 1) Take 4g of bamboo pulp fibers (1.8mm≤length≤2.5mm, 15μm≤width≤20μm), add 38ml of hydrochloric acid with a mass fraction of 0.08%; the reaction temperature is 150°C, the reaction time is 50min, and the reaction pressure is 20MPa;

[0030] 2) After the reaction is finished, the reaction mixture is filtered through a nylon filter (pore size <1 μm) to separate unhydrolyzed cellulose; the resulting filtrate (containing cellulose nanocrystals and soluble sugar) is added dropwise to tert-butyl In an alcohol solvent, perform solvent replacement to deposit soluble sugar on the surface of cellulose nanocrystals; then centrifuge to precipitate, remove the lower layer of precipitate, and dry at a constant temperature at 60°C until the water-redispersible cellulose nanocrystal solid contains 20% of the initial water content form.

Embodiment 2

[0032] 1) Take 3g of wheat straw pulp fiber (0.8mm≤length≤1.5mm, 10μm≤width≤15μm), add 38ml of hydrochloric acid with a mass fraction of 0.1% and 0.9ml of distilled water; the reaction temperature is 160°C, the reaction time is 70min, and the reaction pressure is 10Mpa ;

[0033] 2) After the reaction is finished, filter the reaction mixture through a nylon filter (pore size <1 μm) to separate unhydrolyzed cellulose; add the obtained filtrate (containing cellulose nanocrystals and soluble sugar) dropwise to ethanol under stirring , to perform solvent replacement to deposit soluble sugars on the surface of cellulose nanocrystals; then centrifuge to precipitate, remove the lower layer of precipitate, and dry at a constant temperature at 60°C to a water-redispersible cellulose nanocrystal solid form with an initial water content of 20%.

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Abstract

The invention provides a preparation method for water-redispersible nanocrystalline cellulose. The method comprises the following steps: 1) dispersing a fiber raw material into an acid solution havingan acid concentration of less than 0.1% according to the ratio of the fiber raw material to the acid solution of 1 g:(8-11) ml, wherein the acid solution is hydrochloric acid or sulfuric acid; performing a reaction under heating, pressure and stirring conditions, wherein the reaction temperature is 150-180 DEG C, the reaction time is 50-80 min, and the reaction pressure is 5-20 MPa; and performing filtration to separate unhydrolyzed cellulose to obtain a filtrate for standby application; 2) adding the obtained filtrate into an organic solvent under stirring, performing centrifugal separation,and collecting the centrifuged precipitate; and 3) drying the obtained precipitate until the nanocrystalline cellulose solid with an initial water content of 10%-20% by weight is obtained. Accordingto the preparation method provided by the invention, the water redispersibility of the nanocrystalline cellulose is improved by depositing by-product soluble sugar on the surface of the nanocrystalline cellulose in the preparation process, and the method has the advantages of environmental friendliness and simple operation.

Description

technical field [0001] The invention relates to the field of dispersing cellulose nanocrystals, in particular to a method for dispersing cellulose nanocrystals in an aqueous medium. Background technique [0002] Cellulose nanocrystal (Nanocrystalline Cellulose, referred to as NCC) is a renewable and cyclic carbon-neutral material. These factors and potential unique properties make cellulose nanocrystal-based materials have a wide range of application potential. At present, the solid content concentration of well-dispersed unmodified cellulose nanocrystal suspension is up to 1%, and the remaining 99% is all water, resulting in high storage and transportation costs of cellulose nanocrystal, and it is difficult to prevent bacteria and fungi in the suspension In addition, when cellulose nanocrystals are dispersed into solvents for modification and preparation of composite materials, a high solid content is required. Therefore, the suspension of cellulose nanocrystals must be dr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/02B82Y40/00B82Y30/00
CPCB82Y30/00B82Y40/00C08B15/02
Inventor 徐永建张永奇唐超群张兰张娅倩师云李伟刘燕
Owner 克林斯曼新材料有限公司