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Purification method of 1-hydroxycyclohexyl phenyl ketone

A technology of hydroxycyclohexyl phenyl ketone and purification method is applied in the separation/purification of carbonyl compounds, organic chemistry methods, organic chemistry and other directions, and can solve the problems of low production efficiency, blockage, and decreased thermal conductivity of reaction kettles, etc. To achieve the effect of uniform crystallization and high production efficiency

Inactive Publication Date: 2019-04-26
安达市多森新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the large amount of heat generated during crystallization, there is a large temperature difference with the wall of the kettle, which leads to a large amount of crystals on the wall of the kettle, and it is easy to form a crystalline layer with a thickness of 2-8 cm on the crystallization kettle, resulting in the reaction kettle. The thermal conductivity decreases, which delays the crystallization time; and during the centrifugal discharge process, the agglomerated 1-hydroxycyclohexyl phenyl ketone that is easy to fall from the kettle wall blocks the bottom valve, making it difficult to discharge the material and making the production efficiency lower. Low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] First complete the rectification and water washing operation of the crude product of 1-hydroxycyclohexyl phenyl ketone, then add the 1-hydroxy cyclohexyl phenyl ketone that has been rectified and washed into the crystallization kettle, and then add 1-hydroxy cyclohexyl phenyl ketone Petroleum ether with 6 times the weight of the crude phenyl ketone, then turn on the vacuum and begin to precipitate petroleum ether. When the temperature drops to 10°C, stop the vacuum precipitation, keep stirring for 0.5 hours, and finally centrifuge and dry to obtain 1-hydroxycyclohexyl Phenyl ketone, centrifugal speed 800r / min is 85% crystallization yield.

Embodiment 2

[0015] First complete the rectification and water washing operation of the crude product of 1-hydroxycyclohexyl phenyl ketone, then add the 1-hydroxy cyclohexyl phenyl ketone that has been rectified and washed into the crystallization kettle, and then add 1-hydroxy cyclohexyl phenyl ketone Petroleum ether with 4 times the weight of the crude phenyl ketone, then turn on the vacuum and begin to precipitate petroleum ether. When the temperature drops to 5°C, stop the vacuum precipitation, keep stirring for 1 hour, and finally centrifuge and dry to obtain 1-hydroxycyclohexyl For phenyl ketone, the crystallization yield was 80% at a centrifugal speed of 1200r / min.

Embodiment 3

[0017] First complete the rectification and water washing operation of the crude product of 1-hydroxycyclohexyl phenyl ketone, then add the 1-hydroxy cyclohexyl phenyl ketone that has been rectified and washed into the crystallization kettle, and then add 1-hydroxy cyclohexyl phenyl ketone Petroleum ether with 3 times the weight of the crude phenyl ketone, then turn on the vacuum and begin to precipitate petroleum ether. When the temperature drops to 8°C, stop the vacuum precipitation, keep stirring for 0.5 hours, and finally centrifuge and dry to obtain 1-hydroxycyclohexyl For phenyl ketone, the crystallization yield was 88% at a centrifugal speed of 1000r / min.

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Abstract

The invention relates to a purification method of 1-hydroxycyclohexyl phenyl ketone. The method comprises the following steps: adding excess petroleum ether in 1-hydroxycyclohexyl phenyl ketone crudeproduct after performing rectification and washing operation, and desolventizing and cooling in vacuum to obtain 1-hydrocyclohexyl phenyl ketone. The condition that a large amount of crystalline is formed on a kettle wall under this process condition is avoided, and the production efficiency is high; the condition that the caked 1-hydroxycyclohexyl phenyl ketone falls off from the kettle wall to block a bottom valve is avoided, and the obtained 1-hydroxycyclohexyl phenyl ketone is uniform in crystallization, and the crystallization yield is 80% and more.

Description

technical field [0001] The invention belongs to the field of chemical substance purification, in particular to a method for purifying 1-hydroxycyclohexyl phenyl ketone. Background technique [0002] In the field of initiators, 1-hydroxycyclohexyl phenyl ketone is a powder solid, and the traditional crystallization method of 1-hydroxy cyclohexyl phenyl ketone is to distill and wash the 1-hydroxy cyclohexyl phenyl ketone solution Transfer to a crystallization kettle with stirring, and cool the crystallization by passing cooling water through the jacket. When the temperature in the enamel crystallization kettle is lower than 30 degrees, crystals are precipitated. Due to the large amount of heat generated during crystallization, there is a large temperature difference with the wall of the kettle, resulting in a large amount of crystals adhering on the wall of the kettle, and it is easy to form a crystalline layer with a thickness of 2-8 cm on the crystallization kettle, resulti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/83C07C45/78
CPCC07B2200/13C07C45/78C07C49/83
Inventor 林大勇何连成杨宇澄付景明祝晶晶
Owner 安达市多森新材料科技有限公司