Preparation method of cellulose acetate butyrate

A technology of acetate butyric acid and cellulose, which is applied in the field of cellulose derivatives, can solve the problems of severe cellulose degradation, uneven heating, long hydrolysis time, etc., and achieve the effects of improved reaction efficiency, stable performance, and avoiding serious degradation

Pending Publication Date: 2021-11-05
WEIFANG ENG VOCATIONAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this patent, the method of directly spraying acetic acid on the wood pulp is used for activation, and the activation effect is poor; the traditional heating method is still used in the esterification reaction, and the heating is uneven. At the same time, the hydrolysis time is long and the cellulose degradation is serious.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] (1) join coconut shell gac to soak 3h in glacial acetic acid, obtain the gac of adsorbing glacial acetic acid;

[0054] (2) Add 10 g of refined cotton linters and 80 g of activated carbon for absorbing glacial acetic acid into 200 g of 95% butyric acid aqueous solution, stir and activate for 1.2 h at 25° C., filter to obtain a mixture of activated refined cotton linters and activated carbon;

[0055] (3) Add the mixture of the activated refined cotton linters and activated carbon into DMSO / TBAF 180g and stir for 15min, filter to obtain a solution containing activated cellulose;

[0056] (4) Add 98% concentrated sulfuric acid 0.8g, acetic anhydride 15g and butyric anhydride 35g in the solution containing the activated cellulose, stir while microwave heating carries out esterification reaction, the esterification reaction temperature is 45 ℃, the esterification reaction time For 1h, the esterification feed liquid was obtained;

[0057] (5) Add 50 g of water to the esteri...

Embodiment 2

[0063] (1) Join coconut shell activated carbon and soak 2h in glacial acetic acid, obtain the activated carbon of adsorption glacial acetic acid;

[0064] (2) Add 10 g of refined cotton linters and 50 g of activated carbon for absorbing glacial acetic acid into 130 g of 93% butyric acid aqueous solution, stir and activate for 1.5 h at 20° C., filter to obtain a mixture of activated refined cotton linters and activated carbon;

[0065] (3) Add the mixture of the activated refined cotton linters and activated carbon into DMSO / TBAF 120g and stir for 30min, filter to obtain a solution containing activated cellulose;

[0066] (4) Add 0.5g of 98% concentrated sulfuric acid, 10g of acetic anhydride and 30g of butyric anhydride to the solution containing activated cellulose, stir while heating with microwave to carry out esterification reaction, the esterification reaction temperature is 40 ℃, the esterification reaction time For 2h, obtain the esterification feed liquid;

[0067] (5...

Embodiment 3

[0073] (1) join coconut shell gac to soak 6h in glacial acetic acid, obtain the gac of adsorbing glacial acetic acid;

[0074] (2) Add 10 g of refined cotton linters and 90 g of activated carbon for absorbing glacial acetic acid into 220 g of 94% butyric acid aqueous solution at 30° C. for stirring and activation for 1 h, filter to obtain a mixture of activated refined cotton linters and activated carbon;

[0075] (3) Add the mixture of activated refined cotton linters and activated carbon into DMSO / TBAF 200g and stir for 20min, filter to obtain a solution containing activated cellulose;

[0076] (4) Add 98% concentrated sulfuric acid 1g, acetic anhydride 20g and butyric anhydride 50g in the solution containing the cellulose after activation, stir while microwave heating carries out esterification reaction, and the esterification reaction temperature is 60 ℃, and the esterification reaction time is 0.5h, obtain esterification feed liquid;

[0077] (5) Add 60 g of water to the...

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Abstract

The invention belongs to the technical field of cellulose derivatives, and particularly relates to a preparation method of cellulose acetate butyrate. The method comprises the steps: adding the refined cotton linters and the activated carbon adsorbing the glacial acetic acid into a butyric acid aqueous solution, stirring, activating, and filtering to obtain an activated mixture of the refined cotton linters and the activated carbon; adding the mixture of the activated refined cotton linters and the activated carbon into a solvent, stirring, and filtering to obtain a solution containing activated cellulose; adding concentrated sulfuric acid, acetic anhydride and butyric anhydride into the solution containing the activated cellulose for esterification reaction to obtain esterified feed liquid; adding water into the esterified feed liquid for stirring, pressurizing and hydrolyzing to obtain hydrolysate; and neutralizing, filtering and precipitating the hydrolysate to obtain a precipitate, and washing, cooking and drying the precipitate to obtain the cellulose acetate butyrate. The method has the characteristics of good activation effect, high reaction efficiency, high yield and short hydrolysis time.

Description

technical field [0001] The invention belongs to the technical field of cellulose derivatives, in particular to a preparation method of cellulose acetate butyrate. Background technique [0002] The development of cellulose derivatives has a long history, especially since the 1970s, with the understanding of the limited energy and petroleum resources, and the cellulose material products themselves have the characteristics that other synthetic polymer materials do not have, in the high More and more attention has been paid to cellulose derivatives in the research and utilization of molecular materials. Cellulose ester is one of the important cellulose derivatives. [0003] Cellulose acetate butyrate (CAB) is a cellulose mixed ester obtained by introducing acetyl and butyryl groups into the macromolecular composition of cellulose. Cellulose acetate butyrate has good solubility, flexibility, weather resistance, moldability, etc., and has good compatibility with resins and high-...

Claims

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Application Information

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IPC IPC(8): C08B3/18C08B1/02
CPCC08B3/18C08B1/02
Inventor 卢金帅由文颖郝鑫王春利张兆贵
Owner WEIFANG ENG VOCATIONAL COLLEGE
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