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Preparation method of photoinitiator 1-hydroxycyclohexyl benzophenone

The technology of hydroxycyclohexyl phenyl ketone and photoinitiator is applied in the field of preparation of photoinitiator 1-hydroxycyclohexyl phenyl ketone, and can solve the problems of large environmental pollution, high cost, low production efficiency and the like, Achieving the effect of avoiding environmental pollution, high yield and purity, and increasing production income

Inactive Publication Date: 2018-11-30
宁夏沃凯珑新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the synthetic process method of 1-hydroxycyclohexyl phenyl ketone at present, the purity of the finished product of 1-hydroxy cyclohexyl phenyl ketone generated is low, and the reaction residue cannot be recycled, the production efficiency is low, and the cost is high. It is suitable for large-scale production, and harmful gases such as chlorine gas will be produced during the production process, which will cause great environmental pollution. For this reason, we have designed a preparation method of a photoinitiator 1-hydroxycyclohexyl phenyl ketone to solve the above problems

Method used

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  • Preparation method of photoinitiator 1-hydroxycyclohexyl benzophenone

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Embodiment 1

[0019] A preparation method of photoinitiator 1-hydroxycyclohexyl phenyl ketone, comprising the following steps,

[0020] S1, Reduction: pump a proportioned amount of liquid cyclohexanecarboxylic acid into the high-level metering tank, turn on the vacuum pump of the dissolution kettle to maintain a slight negative pressure state, put in benzoic acid, seal, stop the vacuum pump, and put cyclohexanecarboxylic acid in the metering tank In the kettle, heat up to dissolve, add catalyst to the dissolved solution, then replace the air in the hydrogenation kettle with nitrogen, and introduce hydrogen into the kettle when the temperature rises to 78°C until no hydrogen is absorbed, and the sampling is qualified Finally, lower the temperature to 35°C, pass the residual hydrogen in the kettle through the pressure relief buffer tank and the lye washing tank, and control the flow to empty it. After the hydrogen is exhausted to a slight positive pressure, it is completely replaced by nitroge...

Embodiment 2

[0027] A preparation method of photoinitiator 1-hydroxycyclohexyl phenyl ketone, comprising the following steps,

[0028] S1, Reduction: pump a proportioned amount of liquid cyclohexanecarboxylic acid into the high-level metering tank, turn on the vacuum pump of the dissolution kettle to maintain a slight negative pressure state, put in benzoic acid, seal, stop the vacuum pump, and put cyclohexanecarboxylic acid in the metering tank In the kettle, heat up to dissolve, add catalyst to the dissolved solution, then replace the air in the hydrogenation kettle with nitrogen, and introduce hydrogen into the kettle when the temperature rises to 80°C until no hydrogen is absorbed, and the sampling is qualified Finally, lower the temperature to 38°C, pass the residual hydrogen in the kettle through the pressure relief buffer tank and the lye washing tank, and control the flow to empty it. After the hydrogen is discharged to a slight positive pressure, it is completely replaced by nitrog...

Embodiment 3

[0035] A preparation method of photoinitiator 1-hydroxycyclohexyl phenyl ketone, comprising the following steps,

[0036]S1, Reduction: pump a proportioned amount of liquid cyclohexanecarboxylic acid into the high-level metering tank, turn on the vacuum pump of the dissolution kettle to maintain a slight negative pressure state, put in benzoic acid, seal, stop the vacuum pump, and put cyclohexanecarboxylic acid in the metering tank In the still, heat up to dissolve, add catalyst to the dissolved solution, then replace the air in the hydrogenation kettle with nitrogen, and introduce hydrogen into the kettle when the temperature rises to 82°C until no hydrogen is absorbed, and the sampling is qualified Finally, the temperature is lowered to 40°C, and the residual hydrogen in the kettle is emptied through the pressure relief buffer tank and the lye washing tank, and the flow is controlled. After the hydrogen is exhausted to a slight positive pressure, it is completely replaced by ...

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Abstract

The invention discloses a preparation method of a photoinitiator 1-hydroxycyclohexyl benzophenone. The preparation method comprises the following steps: S1, reduction; S2, acylation; S3, a Friedel-crafts reaction; S4, a chlorination reaction; S5, an alkali hydrolysis reaction; and S6, refining. After the chlorination reaction is completed, chlorine gas in exhaust gas can be completely eliminated through absorption of a first-stage reaction kettle and trapping absorption of a liquid in a second-stage reaction kettle, so that pollution to the environment is avoided; the yield and purity of the product 1-hydroxycyclohexyl benzophenone are high, the HCl gas generated during the reaction can be absorbed by second-stage water and first-stage alkaline so as to obtain hydrochloric acid of 30%, andmeanwhile, by-products phosphorous acid and aluminum trichloride can be obtained in the preparation process, so that the production yield is increased; in the processes of acylation and refining, excessive phosphorus trichloride and petroleum ether are separately recovered through distillation, so that recycling use and cost saving are achieved.

Description

technical field [0001] The invention relates to the technical field of photoinitiators, in particular to a preparation method of photoinitiator 1-hydroxycyclohexyl phenyl ketone. Background technique [0002] Photocuring technology is an efficient, environmentally friendly, energy-saving and excellent material surface treatment technology and processing technology. It is known as a new technology of green industry in the 21st century. The photoinitiator industry, one of the raw materials, has begun to improve its concentration, and the market demand is growing rapidly. The photoinitiator 1-hydroxycyclohexyl phenyl ketone is suitable for light-curing varnish systems such as plastic and metal varnishes, white wood varnishes and paper varnishes, and is also used as a co-initiator for UV-printing inks, generally with other initiators It can be added together with the UV absorber and can be used together with the UV absorber if necessary. [0003] The synthesis process of 1-hyd...

Claims

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Application Information

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IPC IPC(8): C07C49/83C07C45/64C07C45/82C07C51/36C07C51/60C07C61/08C07C45/46C07C49/792C07C45/63C07C49/813C08F2/48
CPCC07C45/46C07C45/63C07C45/64C07C45/82C07C51/36C07C51/60C08F2/48C07C2601/14C07C61/08C07C49/792C07C49/813C07C49/83
Inventor 郭徐良万学明张涛
Owner 宁夏沃凯珑新材料有限公司
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