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Method for preparing cellulose acetate butyrate

A technology of acetate butyrate and cellulose, applied in the field of preparation of cellulose esters, can solve the problems of great damage, complicated product separation process, etc., and achieves reduction of damage, simple post-processing and product separation, and improved leveling. Effect

Inactive Publication Date: 2008-08-13
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the industrial production of cellulose acetate butyrate (CAB) is generally carried out in a heterogeneous system. There are not many domestic manufacturers that can produce CAB and there is still a certain gap in the quality of CAB compared with foreign companies. The esterification reaction method uses toxic solvents such as DMF (N, N-dimethylformamide), DMAC (N, N-dimethylacetamide) as the activation solvent, and its production process is very harmful to the environment and the human body. , post-treatment and product separation process is cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 3 g of pulp paper with a moisture content of 1% (the content of α-cellulose is above 90%) and add 72.8 g of acetic acid to a 250 ml three-necked bottle equipped with mechanical stirring, activate at 95 ° C for 3 hours, and then add 14.5g of butyric anhydride and 0.15g of sulfuric acid were esterified at 95°C for 5 hours, magnesium acetate was added to neutralize the concentrated sulfuric acid left by the esterification reaction, and then precipitated in a 25% ethanol aqueous solution, filtered, washed with water, and placed in The cellulose acetate butyrate can be obtained by vacuum drying at 60°C.

[0019] Using the DRX-400 superconducting nuclear magnetic resonance spectrometer of the German BRUKER company, CDCl 3 as solvent, measured at room temperature 1 H NMR is used to quantitatively measure the degree of substitution of ethyl and butyl in cellulose acetate butyrate. The degree of substitution of ethyl and butyl of the cellulose acetate butyrate prepared in t...

Embodiment 2

[0021] Add the mixture of 3g pulp paper with a moisture content of 3% (the content of α-cellulose is above 90%) and 52g acetic acid + 24g butyric acid into a 250ml three-necked bottle equipped with mechanical stirring, and activate it at 95°C 2h, then add 16.2g butyric anhydride and 0.15g sulfuric acid, carry out esterification reaction at 95°C for 5h, add magnesium acetate to neutralize the concentrated sulfuric acid left by the esterification reaction, then precipitate in 25% ethanol aqueous solution, filter, and The precipitate was washed with water and dried in vacuum at 60° C. to obtain the cellulose acetate butyrate, the degree of substitution of ethyl ester was 2.78, and the degree of substitution of butyl ester was 0.79.

Embodiment 3

[0023] Add the mixture of 3g of pulp paper with a moisture content of 5% (the content of α-cellulose is more than 90%) and 41.6g of acetic acid+33.5g of butyric acid in a 250ml there-necked bottle equipped with mechanical stirring, at 95 Activate at ℃ for 2 hours, then add 16.2g of butyric anhydride and 0.15g of sulfuric acid, perform esterification reaction at 95℃ for 5 hours, add magnesium acetate to neutralize the concentrated sulfuric acid left by the esterification reaction, then precipitate in 25% ethanol aqueous solution, filter , wash the precipitate with water and then vacuum-dry it at 60° C. to obtain the cellulose acetate butyrate with a degree of substitution of ethyl ester of 2.39 and a degree of substitution of butyl ester of 1.02.

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Abstract

The invention discloses a preparation of cellulose acetate-butyrate, including steps of: crushing cotton pulp paper, activating it with organic acid for 2-24 hours at the temperature of 40-110 DEG C., charging acid anhydride and concentrated sulfuric acid, esterifying them at the temperature of 25-110 DEG C. for 3-24 hours; charging adequate magnesium acetate to neutralize residual concentrated sulfuric acid after esterification, then prcipitate and filter it in ethanol-water solution, and obtaining the cellulose acetate-butyrate after scrubbing and drying. The invention avoids using toxic solutions such as DMF, DMAC as activation solution, and uses organic acid both as solution and reaction reagent, so that damage to environment and human body in production process is reduced tremendously, and processes of production, after-treatment and product separation is simple. The prepared cellulose acetate-butyrate can be used as adjuvant of multiple paint, has properties of improving leveling, outdoor durability and toughness of paint, can be applied in biodegradable plastics and films.

Description

technical field [0001] The invention belongs to the field of preparation of cellulose esters, in particular to a preparation method of cellulose acetate butyrate. Background technique [0002] Cellulose esters have low processing temperature, high impact strength, excellent solubility in non-polar solvents, great compatibility with hydrophobic polymers, and can be molded without plasticizers, etc. The advantages make it widely used in biodegradable plastics, coating industry, film and other fields. [0003] 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. The development of cellulose acetate butyrate is precisely to pursue these properties. After the introduction of 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 ...

Claims

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Application Information

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IPC IPC(8): C08B3/16
Inventor 庞浩黄彩结廖兵
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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