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Water-soluble cationic cellulose material and preparation method thereof

A technology of cationic cellulose and water-soluble cations, applied in the field of cellulose materials, can solve the problems of poor water solubility, low degree of cationization, uneven etherification, etc., and achieve the effect of controllable degree of substitution

Inactive Publication Date: 2013-01-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the current method used to produce cationic cellulose is mainly to etherify cellulose with a cationic etherifying agent (3-chloro-2-hydroxypropyltrimethylammonium chloride). Due to the poor solubility of cellulose, it is difficult to Uniform etherification of cellulose, most products are etherification of the surface of cellulose, resulting in uneven etherification, low degree of cationization, and poor water solubility

Method used

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  • Water-soluble cationic cellulose material and preparation method thereof
  • Water-soluble cationic cellulose material and preparation method thereof
  • Water-soluble cationic cellulose material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] Take 1g of microcrystalline cellulose in a 500mL three-neck flask, add 200mL of N,N-dimethylacetamide / lithium chloride (the mass volume ratio of DMAc / LiCl is 0.1g / ml) solution, and raise the temperature to 120°C, under electric mechanical stirring for 10 hours, dissolve; cool down to room temperature, add 0.9gNaH, after 10 minutes, heat up to 55°C, measure 8mL N,N-dimethyl-2-chloroethylamine in a constant pressure dropping funnel Add dropwise within 15 minutes and react for 5 hours; add glacial acetic acid dropwise to adjust the pH to 7, add 1mL dimethyl sulfate dropwise, and react for 5 hours; transfer the reaction solution to a 1000mL beaker, add reaction solution 3 Double the volume of absolute ethanol, let it stand for 3 hours, transfer the supernatant to the recovery bottle, filter with suction, wash the filter residue with 95% ethanol solution three times, then dissolve the obtained solid in deionized water, and transfer to the dialysis bag , dialyzed against deio...

Embodiment 2

[0050]Take 7g of absorbent cotton cellulose and 80g of 1-butyl-3-methylimidazolium chloride in a 250mL three-necked flask, and stir it electrically and mechanically at 100°C for 24 hours; cool down to room temperature, under nitrogen protection, 8gNaH, after 10 minutes, Raise the temperature to 55°C, measure 45mL of N,N-dimethyl-2-chloroethylamine in a constant pressure dropping funnel, add dropwise within 30 minutes, and react for 5 hours; add dropwise glacial acetic acid to adjust the pH value to 6 , raised the temperature to 75°C, added 15 mL of dimethyl sulfate dropwise, and reacted for 5 hours; transferred the reaction solution to a 1000 mL beaker, added 3 times the volume of acetonitrile, and allowed it to stand for 3 hours, then transferred the supernatant to a recovery bottle, and pumped Filter, wash the filter residue three times with 95% acetonitrile solution, then dissolve the obtained solid in deionized water, transfer it to a dialysis bag, and dialyze it with deion...

Embodiment 3

[0053] Take 5g of microcrystalline cellulose in a 500mL three-necked flask, add 200mL of N,N-dimethylacetamide / lithium chloride (the mass volume ratio of DMAc / LiCl is 0.1g / ml) solution, and raise the temperature to 120°C, under electric mechanical stirring for 10 hours, dissolve; cool down to room temperature, add 20mL triethylamine, add 56.72g p-toluenesulfonyl chloride (TsCl) within two hours, after 10 minutes, heat up to 55°C; measure 10mLN,N - Dimethyl-2-hydroxyethylamine in a 50mL conical flask with a stopper, weigh 3gNaH in the conical flask, shake well; quickly transfer to the constant pressure dropping funnel of the reactor, and drop it within 15 minutes , reacted for 5 hours; added dropwise glacial acetic acid to adjust the pH value to 7, added dropwise 5mL dimethyl sulfate, and reacted for 5 hours; the reaction solution was transferred to a 1000mL beaker, added 3 times the volume of methanol, and allowed to stand for 3 hours. Transfer the supernatant to a recovery bo...

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Abstract

The invention discloses a water-soluble cationic cellulose material and a preparation method of the water-soluble cationic cellulose material. The method comprises the following steps of: taking high-purity alpha-cellulose as raw material, dissolving by a certain solvent, carrying out milder quaternization or tertiary amination on hydroxyl of cellulose by proper primary alkyl halide, acid halide, anhydride or epoxy compound with tertiary amine or quaternary ammonium structure under the condition of the existence of different catalysts to obtain cellulose derivatives with even cationization; and washing, dialyzing and drying, so that the pure cationic cellulose material can be obtained, and the complete water-soluble effect can be achieved.

Description

technical field [0001] The invention relates to a cellulose material, especially a water-soluble cationic cellulose material and a preparation method thereof. Background technique [0002] Cellulose is the most abundant natural polymer material in nature. It is a natural polymer polysaccharide linked by β-D-glucopyranose through β-1-4-glycosidic bonds. Each glucose unit on the cellulose macromolecule has three hydroxyl groups, one primary hydroxyl group and two secondary hydroxyl groups. By etherification or esterification of these three hydroxyl groups, cellulose derivatives can be obtained. [0003] Cationic macromolecules are very important polyelectrolyte materials, widely used as bactericides, advanced surfactants, polymer flocculants, hygroscopic agents and humectants, among which cationic macromolecules are more important in genetic engineering research Playing an important role, cationic macromolecules can be used to coat DNA macromolecules. At present, the cation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B11/145C08B3/14
Inventor 丁恩勇熊俊军
Owner SOUTH CHINA UNIV OF TECH