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Method for preparing cellulose acetate butyrate with high hydroxyl content

A technology of acetic acid butyric acid and cellulose, which is applied in the field of preparation of cellulose ester derivatives, can solve the problems of consumption of acid anhydride, waste of materials, low production efficiency, etc., reduce waste water discharge, reduce production cost, and reduce hydrogenolysis reaction time Effect

Active Publication Date: 2020-01-03
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] To sum up, the current production process of cellulose acetate butyrate uses hydrolysis to obtain cellulose acetate butyrate with a hydroxyl content of 1wt%-2wt%. The cellulose acetate butyrate has a very long hydrolysis reaction time and low production efficiency. At the same time, adding water will consume the unreacted anhydride in the system, resulting in waste of materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Use a grinder to crush 1000g of refined cotton, take the crushed 200-300 mesh sieve; weigh 100g of crushed cellulose, put it in a beaker, add 500g of acetic acid, mix well, soak for 10 hours, and then centrifuge to remove part Acetic acid to obtain 155 g of activated cellulose mixture with an acetic acid content of 35 wt%.

[0041] Weigh 20g of acetic anhydride, 700g of butyric anhydride, 750g of n-butyric acid, and 2g of concentrated sulfuric acid into a 2000ml three-neck flask, then add the above-mentioned 155g of activated cellulose, heat up to 100°C with stirring, and keep it warm for 1 hour to complete the esterification reaction.

[0042] Add 1.5g of palladium-carbon catalyst with a palladium load of 5wt%, 2g of formic acid, and 1g of ammonium formate to the above-mentioned esterification reaction solution in sequence, stir and control the temperature at 100°C, and stop the reaction after 10 minutes; filter the reaction solution after cooling to obtain 1627g of hydro...

Embodiment 2

[0045] Use a pulverizer to pulverize 1000g of refined cotton, take the crushed 200-300 mesh sieve; weigh 100g of pulverized cellulose, put it in a beaker, add 5000g of acetic acid, mix well, soak for 6 hours, and then centrifuge to remove part of the acetic acid , Obtain the 240g activated cellulose mixture of acetic acid content 58wt%.

[0046] Weigh 200g of acetic anhydride, 700g of butyric anhydride, 600g of n-butyric acid, and 15g of concentrated sulfuric acid into a 2500ml three-necked flask, then add the above-mentioned 240g of activated cellulose, heat up to 70°C with stirring, and keep it warm for 3 hours to complete the esterification reaction.

[0047] Add 5g palladium-carbon catalyst with palladium loading capacity of 2wt%, 5g formic acid, and 8g sodium formate to the above-mentioned esterification reaction solution in turn, stir and control the temperature at 70°C, and stop the reaction after 60 minutes; filter the reaction solution after cooling to obtain 1775g hyd...

Embodiment 3

[0050] Use a grinder to crush 1000g of refined cotton, take the crushed 200-300 mesh sieve; weigh 100g of crushed cellulose, put it in a beaker, add 2500g of acetic acid, mix well, soak for 2 hours, and then centrifuge to remove part Acetic acid to obtain 180 g of activated cellulose mixture with an acetic acid content of 44 wt%.

[0051] Weigh 300g of acetic anhydride, 400g of butyric anhydride, 650g of n-butyric acid, and 30g of concentrated sulfuric acid into a 2000ml three-neck flask, then add the above-mentioned 180g of activated cellulose, heat up to 50°C with stirring, and keep it warm for 5 hours to complete the esterification reaction.

[0052] Add 9g of palladium-carbon catalyst with a palladium load of 0.5wt%, 9g of formic acid, and 16g of calcium formate to the above-mentioned esterification reaction solution in sequence, and control the temperature at 50°C under stirring, and stop the reaction after 25 minutes; filter the reaction solution after cooling to obtain 1...

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PUM

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Abstract

The invention discloses a method for preparing cellulose acetate butyrate with a high hydroxyl content. The method comprises the following steps: cellulose activation, cellulose esterification and cellulose hydrogenolysis to obtain cellulose acetate butyrate with the hydroxyl content of 4-6 wt%. The method removes acyl groups of the cellulose acetate butyrate by adopting a hydrogenolysis process to obtain high-content hydroxyl groups, so a large amount of acid wastewater generated by hydrolysis through adding water is avoided, the reaction time is remarkably shortened, the production cost is greatly reduced, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of cellulose ester derivatives, in particular to a method for preparing cellulose acetate butyrate with high hydroxyl content. [0002] technical background [0003] 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. [0004] A certain amount of hydroxyl groups needs to be retained in ...

Claims

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Application Information

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IPC IPC(8): C08B3/18C08B3/22
CPCC08B3/18C08B3/22
Inventor 崔乾余炎冰王鹏何金同袁帅黎源孔令晓张明峰
Owner WANHUA CHEM GRP CO LTD
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