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A method for preparing cellulose acetate butyrate with high butyryl content

A technology of acetic acid butyric acid and high butyryl group is applied in the field of preparing cellulose acetate butyrate with high butyryl content, which can solve the problems of high production cost, serious equipment corrosion, strong corrosiveness, etc. Corrosive, source-rich effects

Active Publication Date: 2019-01-29
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent CN101668779 describes the preparation of cellulose ester with acid chloride as an acylating agent, but a large amount of hydrogen chloride is produced after esterification of acid chloride, which seriously corrodes the equipment, and a large amount of acidic wastewater is generated after hydrogen chloride post-treatment
In the patent CN105085689A, vinyl esters are used as esterification agents to prepare cellulose acetate butyrate, but the reaction is a homogeneous reaction, which requires the use of a large amount of solvent (N,N-dimethylacetamide / lithium chloride mixed solution). After analyzing the product, N,N-dimethylacetamide and lithium chloride enter the water, resulting in a large amount of waste water. It is difficult to reuse N,N-dimethylacetamide / lithium chloride, which is not suitable for industrial production
[0005] In summary, the current production process of cellulose acetate butyrate with high butyryl content uses acid anhydride or acid chloride as the esterification agent, which is highly corrosive and cannot be recycled and reused in excess, and the production cost is high; The preparation of cellulose acetate butyrate by corrosive vinyl ester esterification agents requires the use of special solvents to dissolve cellulose, which is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Grinding 100.0 g of refined cotton to 500 mesh using a heavy-pressure grinding type ultrafine pulverizer;

[0029] (2) Weigh 10.0 g of pulverized refined cotton, place it in a single-necked flask, add 30.0 g of acetic acid, mix well and soak for 30 minutes, then centrifuge to remove most of the acetic acid to obtain 13.2 g of activated refined cotton;

[0030] (3) Weigh 195.5g of n-butyl butyrate and 0.6g of concentrated sulfuric acid into a 250ml three-neck flask, then add the above-mentioned 13.2g of activated refined cotton, connect the upper end of the flask to a rectification device with 14 plates, and tap water to condense. Stir rapidly, raise the temperature to 135°C, maintain full reflux in the rectification part, adjust the reflux ratio to 10:1 after 30 minutes, start to extract light components, stop rectification after 4 hours, and the reaction is complete.

[0031] (4) After cooling, the reaction solution was added to 1000 g of water with mechanical stir...

Embodiment 2

[0034] (1) 100.0g of cotton pulp is crushed to 600 mesh with a heavy pressure grinding type ultrafine pulverizer;

[0035] (2) Weigh 14.0 g of pulverized cotton pulp, place it in a single-necked flask, add 375.0 g of acetic acid, mix well and soak for 6 hours, then centrifuge to remove most of the acetic acid to obtain 15.2 g of activated cotton pulp;

[0036] (3) Weigh 167.0g of ethyl butyrate and 1.1g of concentrated sulfuric acid into a 250ml three-necked flask, then add the above-mentioned 15.2g of activated cotton pulp, connect the upper end of the flask to a rectification device with a plate number of 20, and tap water to condense. Stir rapidly, raise the temperature to 105°C, maintain full reflux in the rectification part, adjust the reflux ratio to 15:1 after 1 hour, start to extract light components, stop rectification after 5.5 hours, and the reaction is complete.

[0037] (4) After cooling, the reaction solution was added to 1500 g of water with mechanical stirring,...

Embodiment 3

[0040] (1) 100.0g of wood pulp is crushed to 400 mesh using a heavy pressure grinding type ultrafine pulverizer;

[0041] (2) Weigh 8.0 g of pulverized wood pulp, place it in a single-necked flask, add 60.0 g of acetic acid, mix well and soak for 1 hour, then centrifuge to remove most of the acetic acid to obtain 11.4 g of activated wood pulp;

[0042] (3) Weigh 163.0g of n-hexyl butyrate and 1.6g of concentrated sulfuric acid into a 250ml three-neck flask, then add the above-mentioned 11.4g of activated wood pulp, the upper end of the flask is connected to a rectification device, the number of plates is 35, and tap water is condensed. Stir rapidly, raise the temperature to 176°C, maintain full reflux in the rectification part, adjust the reflux ratio to 15:1 after 1.5 hours, start to extract light components, stop rectification after 4 hours, and the reaction is complete.

[0043] (4) After cooling, the reaction liquid was added to 1380 g of water with mechanical stirring, and ...

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PUM

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Abstract

The invention discloses a method for preparing cellulose acetate butyrate with high butyryl group content, which comprises the following steps: After the crushed cellulose is activated with acetic acid, under the catalysis of sulfuric acid, transesterification occurs with alkyl butyrate to generate high butyrate For cellulose acetate butyrate with acyl group content, the alcohol produced by rectification during the transesterification reaction promotes the positive reaction. In the cellulose acetate butyrate prepared by the method, the acetyl group content is 1-2 wt%, and the butyryl group content is 50-53 wt%. The invention adopts a non-corrosive esterification agent, the excess esterification agent can be recycled, greatly reduces the production cost, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing cellulose acetate butyrate with high butyryl content, belonging to the field of cellulose ester derivatives. technical background [0002] Cellulose acetate butyrate (abbreviated as CAB) is a kind of cellulose mixed ester, which is mainly used to make high-transparency, good-weather-resistant plastic substrates, films and leveling agents for various coatings, film-forming substances, etc. CAB is compatible with a variety of synthetic resins, has good flexibility, cold resistance, leveling, and color retention, and is anti-aging and non-yellowing. It is ideal for contemporary automotive paints, motorcycle paints, wood paints, inks, and pens An important additive in the industry, especially used in automotive paint to control the alignment of aluminum powder and increase the metallic flash of automotive paint. [0003] Cellulose acetate butyrate with high butyryl content has excellent compatibility and low...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B3/18
CPCC08B3/18
Inventor 崔乾何光文王鹏丛鑫郑超董科黎源
Owner WANHUA CHEM GRP CO LTD
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