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Method for synthesizing water-soluble cellulose acetate by one step

A cellulose acetate and water-soluble technology, which is applied in the field of one-step synthesis of water-soluble cellulose acetate, can solve the problems of uneven distribution of acetic acid substituents, high viscosity and high degree of substitution, and achieves improved solubility, low viscosity, and guaranteed cellulose. The effect of degree of aggregation

Active Publication Date: 2019-05-10
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems of uneven distribution of acetic acid substituents, high degree of substitution and high viscosity of the finished product obtained in the preparation method of water-soluble cellulose acetate in the prior art, the invention provides a method for synthesizing water-soluble cellulose acetate in one step

Method used

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  • Method for synthesizing water-soluble cellulose acetate by one step
  • Method for synthesizing water-soluble cellulose acetate by one step
  • Method for synthesizing water-soluble cellulose acetate by one step

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Take 1.8 mL of valeryl chloride and slowly add it dropwise to 30 g of ionic liquid 1-ethyl-3-methylimidazole acetate, and take 1.00 g of cotton linters to invade the above solvent system. Under 70℃ oil bath conditions Magnetic stirring is used to obtain a transparent, viscous and completely dissolved cellulose solution. Under the condition of continuous magnetic stirring, the reaction is kept at 70°C for 12 hours. After the reaction, the system was poured into 200 ml of ethanol to terminate the reaction, followed by repeated washing and filtering with a large amount of ethanol until the ionic liquid and unreacted reagents were cleaned, and a pure cellulose product was obtained. The product was verified to be soluble in water.

[0024] figure 1 It is shown that the absorption peak at 20.3 ppm indicates the presence of ethyl groups on the cellulose, and the absorption peak at 173.9 ppm indicates the presence of carbonyl groups. Combining the two absorption peaks, the cellulos...

Embodiment 2

[0029] Take 1.5 mL of valeryl chloride and slowly add dropwise to 30 g of ionic liquid 1-ethyl-3-methylimidazole acetate, and take 0.6 g of woody cellulose to invade the above solvent system, magnetically under the condition of 63℃ oil bath Stir to obtain a transparent, viscous, and completely dissolved cellulose solution. Under the condition of continuous magnetic stirring, keep the temperature for 9 hours. After the reaction, the system was poured into 200 ml of ethanol to terminate the reaction, followed by repeated washing and filtering with a large amount of ethanol until the ionic liquid and unreacted reagents were cleaned, and a pure cellulose acetate product was obtained. The product was verified to be soluble in water.

Embodiment 3

[0031] Take 3 mL of valeryl chloride and slowly add dropwise to 30 g of ionic liquid 1-ethyl-3-methylimidazole acetate, take 1.5 g of herbal cellulose into the above solvent system, and magnetically stir at 55°C in an oil bath. A transparent, viscous, and completely dissolved cellulose solution was obtained, and the reaction was maintained at 55°C for 6 hours under the condition of continuous magnetic stirring. After the reaction, the system was slowly poured into 200ml of ethanol to terminate the reaction, followed by repeated washing and filtration with a large amount of ethanol until the ionic liquid and unreacted reagents were cleaned, and a pure cellulose acetate product was obtained. water.

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Abstract

The invention relates to water-soluble cellulose acetate, in particular to a method for synthesizing water-soluble cellulose acetate by one step. The method comprises the following steps: adding valeroyl chloride as a modifier into ionic liquid 1-ethyl-3-methylimidazolium acetate to form a modifier solvent system, and adding celluloses into the modifier solvent system for reaction to obtain the water-soluble cellulose acetate. The acetic acid substituents of the finished water-soluble cellulose acetate obtained by the synthesis method are uniformly distributed, and the substitution degree andthe viscosity are both low.

Description

Technical field [0001] The invention relates to water-soluble cellulose acetate, in particular to a method for synthesizing water-soluble cellulose acetate in one step. Background technique [0002] Cellulose is considered to be the most abundant renewable resource on earth, but cellulose is insoluble in most solvents due to its unique crystalline structure and abundant intra- and intermolecular hydrogen bonds. This is serious This limits the high-value utilization of cellulose (Nishiyama et al., 2005). In order to make better use of cellulose, researchers hope to modify cellulose to obtain cellulose derivatives, which will give cellulose new characteristics while increasing the solubility of cellulose, which is more conducive to the further improvement of cellulose. Value-based utilization. Among these cellulose derivatives, cellulose acetate has been widely used in various fields of industry and is a very important cellulose derivative (Gomez-Bujedo et al., 2004; Cao et al., ...

Claims

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Application Information

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IPC IPC(8): C08B3/06
Inventor 逄锦慧李露于世涛刘毓祥
Owner QINGDAO UNIV OF SCI & TECH
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