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A kind of method for preparing cellulose acetate butyrate

A technology of acetic acid butyric acid and cellulose, applied in the direction of sustainable manufacturing/processing, bulk chemical production, climate sustainability, etc., can solve the problems of high equipment material requirements, waste of raw materials, high production costs, etc., and achieve the goal of overcoming solvents Recycling difficulties, avoiding equipment corrosion, and saving raw material costs

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional CAB synthesis method uses acetic anhydride and butyric anhydride as the esterification agent, a large amount of organic acid as the solvent, and sulfuric acid as the catalyst. In order to complete the esterification reaction, both acetic anhydride and butyric anhydride are in excess. After the esterification reaction, a certain amount of water needs to be added to hydrolyze the unreacted anhydride into acid, and a large amount of butyric acid aqueous solution is produced after the reaction is completed. 1. The acetic acid aqueous solution needs to be recycled, the energy consumption is high, and the three wastes are discharged more; and due to the high price of acid anhydrides, especially butyric anhydride, a large amount of waste of raw materials is caused, and the production cost is high
[0005] 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
[0006] 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
[0007] In summary, acid anhydride or acid chloride is used as the esterification agent in the current production process of cellulose acetate butyrate, the reaction system is highly corrosive and the recovery of the esterification agent is difficult, the three wastes are discharged more, and the production cost is higher; the use of special Solvent dissolves cellulose and uses non-corrosive esterification agent to prepare cellulose acetate butyrate. There is a lot of waste water in the production process, and it is difficult to reuse the solvent, so it is not suitable for industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Weigh 10.0g of pulverized refined cotton, place it in a three-necked flask, add 80g of NMMO aqueous solution containing 10% water, stir at 120°C for 4h until the refined cotton is completely dissolved, and cool to room temperature;

[0031] (2) weigh 0.5g of acetonitrile, 25g of butyronitrile, and 0.5g of concentrated sulfuric acid and add it to the above-mentioned three-necked flask, the upper end of the three-necked flask is connected to a reflux device, the tap water is condensed, and reacted at 70 ° C for 6h;

[0032] (3) After cooling, the reaction solution was added to 1420 g of water with mechanical stirring, and a white solid was precipitated, which was filtered and washed until neutral, and dried at 100° C. for 3 hours to obtain the product.

[0033] (4) The filtrate obtained by suction filtration is concentrated to a water content of 11.5% by a scraper evaporator, which can be reused.

[0034] It was determined that in this example, the acetyl group conten...

Embodiment 2

[0036] (1) Weigh 10.0 g of pulverized refined cotton, place it in a three-necked flask, add 100 g of an NMMO aqueous solution containing 12% water, stir at 130° C. for 3 hours until the refined cotton is completely dissolved, and cool to room temperature;

[0037] (2) Weigh 7.5g of acetonitrile, 17.5g of butyronitrile, and 1g of concentrated sulfuric acid and add to the above-mentioned three-necked flask, the upper end of the there-necked flask is connected to a reflux device, and the tap water is condensed and reacted at 100 ° C for 3h;

[0038] (3) After cooling, the reaction solution was added to 3200 g of water with mechanical stirring, and a white solid was precipitated, which was filtered and washed until neutral, and dried at 80° C. for 5 hours to obtain the product.

[0039] (4) The filtrate obtained by suction filtration is concentrated to a water content of 12% by a scraper evaporator, which can be reused.

[0040] It was determined that in this example, the acetyl g...

Embodiment 3

[0042] (1) Weigh 10.0 g of pulverized refined cotton, place it in a three-necked flask, add 150 g of NMMO aqueous solution containing 15% of water, stir at 130 ° C for 2 h until the refined cotton is completely dissolved, and cool to room temperature;

[0043] (2) Weigh 10g of acetonitrile, 15g of butyronitrile, 2g of vitriol oil and add to the above-mentioned three-necked flask, the upper end of the three-necked flask is connected to a reflux device, the tap water is condensed, and reacted at 120 ° C for 3h;

[0044] (3) After cooling, the reaction solution was added to 21,000 g of water with mechanical stirring, and a white solid was precipitated, which was filtered and washed until neutral, and dried at 100° C. for 2 hours to obtain the product.

[0045] (4) The filtrate obtained by suction filtration is concentrated to a water content of 14% by a scraper evaporator, which can be reused.

[0046] It was determined that in this example, the acetyl group content in cellulose ...

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Abstract

The invention discloses a method for preparing cellulose acetate butyrate, which comprises the following steps: after dissolving pulverized cellulose in a solvent, alcoholysis reacts with acetonitrile and butyronitrile under the catalysis of concentrated sulfuric acid to generate cellulose acetate butyrate . In the cellulose acetate butyrate prepared by the method, the content of acetyl groups is 1-15wt%, and the content of butyryl groups is 35-53wt%. The invention adopts non-corrosive esterification agent and solvent, and the solvent NMMO aqueous solution can be recycled and reused after being concentrated, which 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, belonging to the field of cellulose ester derivatives. [0002] technical background [0003] Cellulose acetate butyrate (CAB for short) is an important ester derivative of cellulose. It is compatible with a variety of resins, has good flexibility, cold resistance, leveling, and color retention, and is anti-aging and non-yellowing. , can be used to make high-transparency, good weather resistance plastic base, film and leveling agent, film-forming material of various coatings, especially in automotive paint to control the orientation of aluminum powder, increase the performance of automotive paint Metallic sparkle. [0004] The traditional CAB synthesis method uses acetic anhydride and butyric anhydride as esterification agents, a large amount of organic acid as solvent, and sulfuric acid as catalyst. The reaction system is highly corrosive, requires higher equipment materials, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B3/18C08B1/00
CPCC08B3/18C08B1/003Y02P20/54
Inventor 何金同胡凯华余炎冰崔乾于冠群刘超牟通
Owner WANHUA CHEM GRP CO LTD
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