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Preparation method of cellulose acetate butyrate

A technology of acetic acid butyric acid and cellulose, which is applied in the field of preparing cellulose acetate butyrate, which can solve the problems of low substitution degree of ethyl ester, low substitution degree of butyl ester, difficult control of raw material selection and process parameters, and achieve uniform substitution degree and reproducible Good sex and full activation effect

Inactive Publication Date: 2013-01-16
WUXI KAILI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material selection and process parameters of this method are difficult to master, and it is easy to obtain products with lower degrees of ethyl ester substitution and butyl ester substitution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Butyric acid, acetic acid and 3 g of refined cotton linters were put into a blender and stirred for activation, and activated at 45° C. for 4 hours; the mass of the acetic acid was 15 g, and the mass of the butyric acid was 36 g;

[0023] (2) Add acetic anhydride to the activated refined cotton, carry out esterification with sulfuric acid as a catalyst, and stir the esterification at 45°C for 6 hours; the mass of the acetic anhydride is 26.7g, and the mass of the sulfuric acid is 0.15g;

[0024] (3) After the esterification is completed, add butyric acid aqueous solution to the esterification liquid, stir and hydrolyze at 45°C for 6 h; the mass concentration of the butyric acid aqueous solution is 20%, and the mass of the butyric acid aqueous solution is 30g;

[0025] (4) After the hydrolysis, it is not necessary to keep the temperature, keep stirring, add sodium butyrate to neutralize sulfuric acid, then add acetic acid aqueous solution to dilute, and finally pour i...

Embodiment 2

[0027] (1) Butyric acid, acetic acid and 3 g of refined cotton linters were put into a blender and stirred for activation, and activated at 50° C. for 3 hours; the mass of the acetic acid was 21 g, and the mass of the butyric acid was 45 g;

[0028] (2) Add acetic anhydride to the activated refined cotton, carry out esterification with sulfuric acid as a catalyst, and stir the esterification at 50°C for 5 hours; the mass of the acetic anhydride is 26.7g, and the mass of the sulfuric acid is 0.15g;

[0029] (3) After the esterification is completed, add butyric acid aqueous solution to the esterification liquid, stir and hydrolyze at 50°C for 5 h; the mass concentration of the butyric acid aqueous solution is 20%, and the mass of the butyric acid aqueous solution is 39g;

[0030] (4) After the hydrolysis, it is not necessary to keep the temperature, keep stirring, add sodium butyrate to neutralize sulfuric acid, then add acetic acid aqueous solution to dilute, and finally pour i...

Embodiment 3

[0032] (1) Butyric acid, acetic acid and 3g of refined cotton linters were put into a blender and stirred for activation, and activated at 60°C for 2 hours; the mass of the acetic acid was 30, and the mass of the butyric acid was 60g;

[0033] (2) Add acetic anhydride to the activated refined cotton, carry out esterification with sulfuric acid as a catalyst, and stir the esterification at 60°C for 4 hours; the mass of the acetic anhydride is 26.7g, and the mass of the sulfuric acid is 0.15g;

[0034] (3) After the esterification is completed, add butyric acid aqueous solution to the esterification liquid, stir and hydrolyze at 60°C for 4 h; the mass concentration of the butyric acid aqueous solution is 20%, and the mass of the butyric acid aqueous solution is 45g;

[0035] (4) After the hydrolysis, it is not necessary to keep the temperature, keep stirring, add sodium butyrate to neutralize sulfuric acid, then add acetic acid aqueous solution to dilute, and finally pour into wa...

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Abstract

The invention discloses a preparation method of cellulose acetate butyrate, of which the specific steps are as follows: (1) putting butyric acid, acetic acid and refined cotton linter into a blender together to stir for activation, and ensuring the activation last for 2 to 4 hours at a temperature of 45 to 60 DEG C; (2) adding acetic anhydride into the activation processed refined cotton linter, carrying out esterification by using sulfuric acid as catalyst, and stirring for esterification for 4 to 6 hours at a temperature of 45 to 60 DEG C; (3) after esterification is finished, adding butyric acid aqueous solution into esterifying liquid, and stirring for hydrolysis for 4 to 6 hours at a temperature of 45 to 60 DEG C; and (4) keeping stirring after the hydrolysis is finished, adding sodium butyrate to neutralize the sulfuric acid, then adding acetic acid aqueous solution for dilution, at last keeping stirring while pouring into the water for precipitation, and then washing and drying the obtained product. The preparation method provided by the invention has the advantages that the process is simple, materials are saved, the steps are optimized and the cost is low.

Description

technical field [0001] The invention relates to the technical field of cellulose derivatives, in particular to a method for preparing cellulose acetate butyrate. Background technique [0002] Cellulose acetate is used as an additive in many coatings to give them many good properties, but it lacks the solubility range, miscibility and moisture resistance necessary for some coatings. After cellulose acetate butyrate is introduced into butyl ester, it has a wider solubility range and miscibility than pure cellulose acetate. It is not only soluble in common solvents such as acetone, but also soluble in organic acids, methyl isobutyl ketone, butyl acetate Solvent systems such as esters and ethyl acetate, cellulose acetate butyrate with a high degree of substitution of butyl esters can even be dissolved in ethanol and other alcohol solvents, which makes it widely used in the coating industry to improve the fluidity and leveling of coatings Performance, outdoor durability, pigment...

Claims

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Application Information

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IPC IPC(8): C08B3/18
Inventor 杨毅跃康国伟姚程成蒙相锋鲁尧
Owner WUXI KAILI PHARMA
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