Method for preparing acetate by using clay-based solid acid

An acetate and clay-based technology, applied in the field of clay-based solid acid to prepare acetate, achieves high catalytic efficiency, simple preparation and operation, and reduces equipment costs

Inactive Publication Date: 2020-02-18
JINJIANG TAIXING CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problems described in the technical background, the method for preparing acetate from clay-based solid acid provided by the invention, the clay-based solid acid catalyst of its nanostructure has a high specific surface area, and is

Method used

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  • Method for preparing acetate by using clay-based solid acid

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Effect test

Embodiment 1

[0011] Preparation of clay-based solid acid catalyst: Stir and disperse 1kg halloysite and 20kg absolute ethanol in ultrasonic for 1min, then add 20g of tin tetrachloride, continue to disperse under ultrasonic stirring for 5min, drop ammonia water, adjust the pH of the system to 6, Then aged at 70°C for 8h. After drying the aged colloid at 80°C, it was acidified and impregnated with 2M sulfuric acid for 1 hour, and finally the obtained catalyst was calcined in a muffle furnace at 500°C for 3 hours.

[0012] Clay-based solid acid catalyst catalyzed synthesis of propyl acetate: 1 kg of clay-based solid acid catalyst was added to a heated and stirred reactor, and acetic acid and propanol were continuously added to the reactor at a molar ratio of 1:1 to make the reactor, the catalyst Maintain at about 8wt%, heat to 115°C for continuous reaction, the reaction product is separated and removed after azeotropic distillation in the esterification tower, and the crude product of propyl ...

Embodiment 2

[0015] Preparation of clay-based solid acid catalyst: Stir and disperse 1kg of halloysite and 35kg of absolute ethanol in ultrasonic for 5 minutes, then add 24g of tin tetrachloride, continue to disperse with ultrasonic stirring for 10min, add ammonia water dropwise, adjust the pH of the system to 6, Then aged at 70°C for 24h. After drying the aged colloid at 80°C, it was acidified and impregnated with 2M sulfuric acid for 2h, and finally the obtained catalyst was calcined in a muffle furnace at 600°C for 2h.

[0016] Clay-based solid acid catalyst catalyzed synthesis of butyl acetate: 1kg of catalyst was added to a heated and stirred reactor, and acetic acid and butanol were continuously added to the reactor at a molar ratio of 1:1 to keep the catalyst at 5wt% Heating to 120°C for continuous reaction, the reaction product is separated and removed from water after azeotropic distillation in the esterification tower, and the crude product of butyl acetate with a content of 95% ...

Embodiment 3

[0019] Preparation of clay-based solid acid catalyst: Stir and disperse 1kg of halloysite and 20kg of absolute ethanol in ultrasonic for 3 minutes, then add 24g of tin tetrachloride, continue to disperse with ultrasonic stirring for 10min, add ammonia water dropwise, adjust the pH of the system to 6, Then aged at 70°C for 24h. After drying the aged colloid at 80°C, it was acidified and impregnated with 2M sulfuric acid for 2h, and finally the obtained catalyst was calcined in a muffle furnace at 500°C for 2h.

[0020] Clay-based solid acid catalyst catalyzed synthesis of ethyl acetate: 1 kg of clay-based solid acid catalyst was added to a reactor with heating and stirring, and acetic acid and ethanol were continuously added to the reactor at a molar ratio of 1:1 to maintain the catalyst in the reactor at About 10wt%, heating to 110°C for continuous reaction, the reaction product is separated and removed after azeotropic distillation in the esterification tower, and the crude p...

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Abstract

The invention relates to a method for preparing an acetate by using a clay-based solid acid. The solid acid is prepared by using natural clay halloysite as a base material. Halloysite and tin tetrachloride are used to form a colloid, the colloid is subjected to aging and then acidification with sulfuric acid, an acetate solid catalyst with a large specific surface area is obtained, the prepared catalyst is added into a reactor, then acetic acid and an alcohol are continuously added, and a reaction is continuously carried out at 90-120 DEG C to obtain the acetate. The solid acid catalyst has excellent esterification reaction catalytic activity, higher efficiency, low preparation and use cost, low corrosion to equipment, and easy recovery and utilization, and the environmental protection andcost problems of industrial production of acetate products can be greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, in particular to a method for preparing acetate from clay-based solid acid. Background technique [0002] The current global production capacity of acetate products exceeds 5 million tons. As a commonly used chemical basic product, concentrated sulfuric acid is still used as a catalyst in the production of most enterprises. In the state of bubbling, dripping, and leaking, it is easy to cause complaints or stop production risks due to environmental protection issues. For corrosion, special metals can be used to prepare equipment, but this will greatly increase capital investment and double the risk of corporate actions. A small number of enterprises use mixed acid catalysts such as p-toluenesulfonic acid and methanesulfonic acid, which can reduce the corrosion problem to a certain extent. However, on the other hand, the cost of p-toluenesulfonic acid and methanesulfonic acid is relatively h...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J37/34B01J37/02B01J37/08C07C67/08C07C69/14
CPCB01J27/053B01J37/0201B01J37/08B01J37/343C07C67/08C07C69/14B01J37/02B01J37/34Y02P20/584
Inventor 李庭忠张明康马文优
Owner JINJIANG TAIXING CHEM IND CO LTD
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