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Preparation method for cellulose acetate-butyrate

A technology for 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 cost saving , good reproducibility

Inactive Publication Date: 2013-01-30
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

[0020] (1) Butyric acid, acetic acid and 3 g of refined cotton linters were put into a blender and stirred for activation, and activated at 80° C. for 4 hours; the mass of the acetic acid was 52 g, and the mass of the butyric acid was 24 g;

[0021] (2) Add butyric anhydride to the activated refined cotton, use sulfuric acid as a catalyst to carry out esterification, and stir the esterification at 80°C for 6 hours; the mass of the butyric anhydride is 16.2g, and the mass of the sulfuric acid is 0.15g;

[0022] (3) After the esterification is completed, add butyric acid aqueous solution to the esterification liquid, stir and hydrolyze at 80°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;

[0023] (4) After the hydrolysis is completed, it is not necessary to keep the temperature, keep stirring, add sodium butyrate to neutralize sulfuric acid, then add butyric acid aqueous solution to dilute, ...

Embodiment 2

[0025] (1) Butyric acid, acetic acid and 3 g of refined cotton linters were put into a blender and stirred for activation, and activated at 95° C. for 2 hours; the mass of the acetic acid was 41.6 g, and the mass of the butyric acid was 33.5 g;

[0026] (2) Add butyric anhydride to the activated refined cotton, carry out esterification with sulfuric acid as a catalyst, and stir the esterification at 95°C for 4 hours; the mass of the butyric anhydride is 16.2g, and the mass of the sulfuric acid is 0.15g;

[0027] (3) After the esterification is completed, add butyric acid aqueous solution to the esterification liquid, stir and hydrolyze at 95°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 36g;

[0028] (4) After the hydrolysis is completed, it is not necessary to keep the temperature, keep stirring, add sodium butyrate to neutralize sulfuric acid, then add butyric acid aqueous solution to dilute...

Embodiment 3

[0030] (1) Butyric acid, acetic acid and 3 g of refined cotton linters were put into a blender and stirred for activation, and activated at 90° C. for 3 hours; the mass of the acetic acid was 20.8 g, and the mass of the butyric acid was 57.5 g;

[0031] (2) Add butyric anhydride to the activated refined cotton, use sulfuric acid as a catalyst to carry out esterification, and stir the esterification at 90°C for 5 hours; the mass of the butyric anhydride is 16.2g, and the mass of the sulfuric acid is 0.15g;

[0032] (3) After the esterification is completed, add butyric acid aqueous solution to the esterification liquid, stir and hydrolyze at 90°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 45g;

[0033] (4) After the hydrolysis is completed, it is not necessary to keep the temperature, keep stirring, add sodium butyrate to neutralize sulfuric acid, then add butyric acid aqueous solution to dilu...

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Abstract

The invention provides a preparation method for cellulose acetate-butyrate. The preparation method comprises the following concrete steps: (1) stirring butyric acid, acetic acid and refined cotton linter in a mixer and carrying out activation at a temperature of 80 to 95 DEG C for 2 to 4 h; (2) adding butyric anhydride into the activated refined cotton linter and carrying out esterification at a temperature of 80 to 95 DEG C for 4 to 6 h under stirring, with sulfuric acid used as a catalyst; (3) after esterification, adding an aqueous solution of butyric acid into esterification liquid and carrying out hydrolysis at a temperature of 80 to 95 DEG C for 4 to 6 h under stirring; and (4) after hydrolysis, maintaining stirring, adding sodium butyrate to neutralize sulfuric acid, adding the aqueous solution of butyric acid for dilution, dumping an obtained diluted solution into water under stirring for precipitation and rinsing and drying an obtained product. The method provided by the invention has the advantages of a simple process, conservation of raw materials, optimized steps and low cost.

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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