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Synthetic method of photoinitiator 1-hydroxycyclohexyl phenyl ketone

A technology of hydroxycyclohexyl phenyl ketone and cyclohexyl phenyl ketone, which is applied in the field of preparation of chlorinated hydrolysis, can solve the problems of acid waste water and achieve the effects of reduced discharge, less loss and high yield

Inactive Publication Date: 2018-07-20
江苏优普生物化学科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention provides a method for synthesizing photoinitiator 184, which solves the problem of producing acidic wastewater in the current production process

Method used

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  • Synthetic method of photoinitiator 1-hydroxycyclohexyl phenyl ketone

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Experimental program
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Effect test

Embodiment 1

[0016] Add anhydrous AlCl to a 500ml four-neck flask equipped with stirring 3 80.0g (0.6mol), add 235g (3mol) of benzene in an ice-water bath, drop it below 0°C, add 73.3g (0.5mol) of cyclohexanoyl chloride (constant pressure funnel) to the bottle dropwise, drop Keep the temperature at 0-5°C during the addition, and the dropwise addition time is about 30 minutes. After the dropwise addition, slowly raise the temperature to 78°C, and react under reflux for 6 hours. After the reaction, pour the reactant into 360g of 20% diluted In hydrochloric acid (1.97mol), stir well and then separate the phases, take the upper organic phase and carry out vacuum distillation to recover benzene, after benzene is distilled off, 85.8g (A) of light yellow solid (content 92%, 0.42mol) is obtained, and the molar yield is 84 %. The acid water in the lower layer was distilled under reduced pressure, and 300 g (content 23%) of hydrochloric acid aqueous solution (B) was distilled off.

[0017] Add (A...

Embodiment 2

[0019] Add anhydrous AlCl to a 500ml four-neck flask equipped with stirring 3 80.0g (0.6mol), add 235g (3mol) of benzene in an ice-water bath, drop it below 0°C, add 73.3g (0.5mol) of cyclohexanoyl chloride (constant pressure funnel) to the bottle dropwise, drop Keep at 0-5°C while adding, add about 30 minutes, slowly heat up to 78°C after dropwise addition, react under reflux for 6 hours, after the reaction, cool down to about 0°C, add 360g of 20% dilute hydrochloric acid (1.97mol) Drop into the reactant, stir well and then separate the phases. Take the upper organic phase and carry out vacuum distillation to recover benzene. After benzene is distilled off, 83.2 g of light yellow solid (A) (content 91.5%, 0.4 mol) is obtained, and the molar yield is 80%. . The acid water in the lower layer was distilled under reduced pressure, and 313 g (content 22%) of hydrochloric acid aqueous solution (B) was distilled off.

[0020] Add (A) 83.2g (content 91.5%, 0.4mol), 1,1-dichloroeth...

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Abstract

The invention discloses a synthetic method of a photoinitiator 1-hydroxycyclohexyl phenyl ketone. The synthetic method comprises the following steps: enabling cyclohexanecarboxylic acid chloride and benzene to be subjected to electrophilic substitution reaction under the catalysis of Lewis acid to obtain cyclohexyl phenyl ketone; enabling the cyclohexyl phenyl ketone to react with hydrogen peroxide and a hydrochloric acid solution under the action of a molecular sieve catalyst to obtain 1-chlorocyclohexyl phenyl ketone; and enabling the 1-chlorocyclohexyl phenyl ketone and a sodium hydroxide aqueous solution to be subjected to hydrolysis reaction under the action of the catalyst to obtain the 1-hydroxycyclohexyl phenyl ketone. The synthetic method disclosed by the invention has the advantages that the raw materials are cheap, easily-available, safe and environmentally friendly; hydrogen chloride produced by electrophilic substitution reaction of acyl chloride under the catalysis of Lewis acid is fully utilized and recycled, thereby reducing the discharge of waste acid water and being friendly to the environment; and selective chlorination and hydrolysis are completed in the same reactor, the operation is simple, the loss is less, and the yield is high.

Description

technical field [0001] The invention relates to the field of photoinitiators, and relates to a method for preparing photoinitiator 184 (1-hydroxycyclohexyl phenyl ketone) by chlorination and hydrolysis during the preparation process. Background technique [0002] Photoinitiator 184 is a kind of α-hydroxyketone photoinitiator, and α-hydroxyketone photoinitiator is a new type of high-efficiency photoinitiator. Since there is no α-hydrogen atom, this type of photoinitiator system has high stability and is easy to store. Long life, wide UV absorption range, fast polymerization speed, good solubility, low odor, low pollution, the prepared photosensitive composition has excellent stability, and is widely used in coatings, inks, electronics, optical fibers, adhesives, printing and other fields , and showed strong vitality. [0003] According to previous literature reports, photoinitiator 184 is catalyzed by benzene and cyclohexyl chloride to generate cyclohexyl phenyl ketone, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/46C07C49/784C07C45/63C07C45/64C07C49/813C07C49/83
CPCC07C45/46C07C45/63C07C45/64C07C49/784C07C49/813C07C49/83
Inventor 杨建明曲红梅邱历王任伟
Owner 江苏优普生物化学科技股份有限公司
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