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Method for refining acetylacetone

A technology of acetylacetone and refining method, which is applied in the separation/purification of carbonyl compounds, organic chemistry, etc., which can solve the problems of not being able to obtain high-purity products, and achieve the effects of easy control, high product purity, and stable quality content

Inactive Publication Date: 2012-07-18
SHANGHAI WUJING CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcoming that high-purity products cannot be obtained due to low boiling components such as acetone and isopropenyl acetate produced by the decomposition of acetylacetone entering the final refining tower T1 in the prior art, and to provide a stable and reliable operation The continuous refining method of high-purity acetylacetone, not only can be operated continuously, but also the final product has high purity and a mass content of 99.9%, which is suitable for large-scale industrial production

Method used

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  • Method for refining acetylacetone
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Effect test

Embodiment 1

[0024] The feed position is the 30th theoretical plate from the top of the tower, and the content of the crude acetylacetone component in the feed is the same as in Comparative Example 1.

[0025] Operating conditions of the refining tower: the pressure at the top of the tower is gauge pressure -63kPa, the reflux ratio is 5, the temperature at the top of the tower is 108°C, the temperature at the bottom of the tower is 125°C, and the temperature of the side line of acetylacetone is 110°C.

[0026] Rectification result: the extraction position of acetylacetone is the 10th theoretical plate counted from the top of the column from the side line of the refining column T1, and the product purity is 99.9%.

Embodiment 2

[0028] Due to fluctuations in the working conditions of the previous section, the isopropenyl acetate in the feed enters the refining tower T1, and the feed position is the 35th theoretical plate from the top of the tower. The composition of the crude acetylacetone of the feed is: 97.7% acetylacetone, 0.3% acetone, 1% isopropenyl acetate, 1% high boiling components.

[0029] The operating conditions of the refining tower T1 are: the pressure at the top of the tower is gauge pressure -86kPa, the reflux ratio is 5, the temperature at the top of the tower is 75°C, the temperature at the bottom of the tower is 104°C, and the temperature of the side line of acetylacetone is 86°C.

[0030] Acetylacetone is withdrawn from the side line of the refining tower T1, and its position is the 15th theoretical plate from the top of the tower. The rectification result: the product purity is 99.9%.

Embodiment 3

[0032] The feed position is the 32nd theoretical plate from the top of the tower. Since acetylacetone decomposes into acetone and other low-boiling components and enters the refining tower T1, the composition of the feed crude acetylacetone is: 97.7% acetylacetone, 1% acetone , 0.3% isopropenyl acetate, 1% high boiling components.

[0033] The operating conditions of the refining tower T1 are: the pressure at the top of the tower is -45kPa, the reflux ratio is 8, the temperature at the top of the tower is 113°C, the temperature at the bottom of the tower is 129°C, and the temperature of the side line of acetylacetone is 117°C.

[0034] Acetylacetone is withdrawn from the side line of the refining tower T1, and its position is the ninth theoretical plate from the top of the tower. The rectification result: the product has a purity of 99.9%.

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Abstract

A method for refining high-purity acetylacetone comprises procedures of devolatiligation, deacidification and deanhydride to coarse acetylacetone which later on enters a refining tower T1. The method is characterized in that the refining tower T1 is a pressure relief refining tower, the high-purity acetylacetone is extracted from the upper side line of the rectification section in liquid phase, acetone generated by the decomposition of acetylacetone and low-boiling mixed components, such as isopropenyl acetate, which are not completely removed due to instability of the initial stage of the process, are collected at the top of the tower, returned to a coarse acetylacetone groove V1, placed in the refining tower T1 after the procedures of devolatiligation, deacidification and deanhydride, and the tower kettle uses high-boiling components. The invention has the advantages that the refining tower T1 has the function of removing a small mount of low-boiling components because of liquid phase side line discharge way thereof, meanwhile, the acetone and isopropenyl acetate obtained from the top of the tower can be recycled, and the tower kettle uses high-boiling components, so that the whole rectification section is easy to control, flexible in operation, high in purity of the finished products, and stable in mass content of 99.9%.

Description

technical field [0001] The invention relates to a chemical separation process, in particular to a method for continuously refining high-purity acetylacetone in an acetylacetone refining tower using vacuum distillation and side line discharge. Background technique [0002] Acetylacetone is an important chemical and pharmaceutical intermediate, which can be used to synthesize sulfonamide drugs, feed additives and catalysts, etc. With the development of society, the purity requirements for acetylacetone are getting higher and higher, and the purity requirement of superior products reaches 99.9%. , which also puts forward higher requirements for the continuous distillation process of acetylacetone. In the current acetylacetone distillation process, the last refining tower adopts the method of extracting products from the top of the tower to obtain acetylacetone. However, in actual production, acetone is produced due to the thermal decomposition of acetylacetone, or isopropenyl ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/14C07C45/82
Inventor 叶小鹤曾义红朱家文李亭顾明兰杨志东纪利俊
Owner SHANGHAI WUJING CHEM
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