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Preparation method for high-purity ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate

A technology of ethyl trimethylbenzoyl and phenylphosphinate, which is applied in the field of preparation of high-purity ethyl phenylphosphinate, can solve the problem of low purity, and achieve the effect of ensuring product purity and stable properties

Active Publication Date: 2017-10-03
江苏富比亚化学品有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to provide a kind of preparation method of high-purity (2,4,6-trimethylbenzoyl) ethyl phenyl phosphinate, the feature of this method is that can overcome the low shortcoming of prior art product purity , Through raw material selection and process control, impurities can be effectively removed, and the target substance with a purity higher than 99% can be obtained

Method used

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  • Preparation method for high-purity ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate

Examples

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Comparison scheme
Effect test

Embodiment 1

[0020] Add 0.1mol of phenylphosphinic acid and 100mL of toluene into the reaction kettle, control the temperature at 100-120°C and add 0.11mol of 2,4,6-trimethylbenzaldehyde dropwise, after the addition is completed, at this temperature (100-120°C) The reaction was carried out under heat preservation for 2 hours to prepare the intermediate. Cool down to room temperature, add a small amount of hydrochloric acid to adjust the pH to 4-6, add 0.13 g of vanadium diacetylacetonate as a catalyst, add 0.12 mol of tert-butanol peroxide dropwise at 5-10 °C, and keep warm at 5-10 °C after the addition is completed. It was observed by TLC that all the intermediates were completely reacted, and a reaction mixture 1 was obtained. Add 100mL of water to the reaction mixture 1, adjust the pH to neutral with saturated aqueous sodium bicarbonate solution, separate the aqueous layer, wash it twice with water, reduce the excess oxidant with an appropriate amount of aqueous sodium sulfite solution,...

Embodiment 2

[0022] Add 0.1mol of phenylphosphinic acid and 100mL of chlorobenzene into the reaction kettle, control the temperature at 100-120°C, add 0.11mol of 2,4,6-trimethylbenzaldehyde dropwise, and keep the temperature at 100-120°C for reaction After 2 hours, the intermediate was prepared. Cool down to room temperature, add a small amount of hydrochloric acid to adjust the pH to 4-6, add 0.13 g of vanadium diacetylacetonate as a catalyst, add 0.15 mol of tert-butanol peroxide dropwise at 5-10 °C, and keep warm at 5-10 °C after the addition is completed. It was observed by TLC that all the intermediates were completely reacted, and a reaction mixture 1 was obtained. Add 100mL of water to the reaction mixture 1, adjust the pH to neutral with saturated aqueous sodium bicarbonate solution, separate the aqueous layer, wash it twice with water, reduce the excess oxidant with an appropriate amount of aqueous sodium sulfite solution, separate the organic layer, and wash it twice with water. ...

Embodiment 3

[0024] Add 0.1mol of phenylphosphinic acid and 100mL of chlorobenzene into the reaction kettle, control the temperature at 100-120°C, add 0.11mol of 2,4,6-trimethylbenzaldehyde dropwise, and keep the temperature at 100-120°C for reaction After 2 hours, the intermediate was prepared. Then cool down to room temperature, add a small amount of hydrochloric acid to adjust the pH to 4-6, add catalyst V 2 o 5 0.1 g, 0.15 mol of tert-butanol peroxide was added dropwise under control of 5-10°C, and kept warm at 5-10°C after the addition was completed. It was observed by TLC that all intermediates were completely reacted, and reaction mixture 1 was obtained. Add 100mL of water to the reaction mixture 1, adjust the pH to neutral with saturated aqueous sodium bicarbonate solution, separate the aqueous layer, wash it twice with water, reduce the excess oxidant with an appropriate amount of aqueous sodium sulfite solution, separate the organic layer, and wash it twice with water. Once ag...

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Abstract

The invention discloses a preparation method for high-purity ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate. The preparation method comprises the following concrete steps: reacting phenylphosphinate with aromatic aldehyde so as to prepare an intermediate, subjecting the intermediate to catalytic oxidation so as to obtain benzoylphenylphosphinic acid and subjecting benzoylphenylphosphinic acid and diethyl sulfate to an ethylation reaction so as to obtain ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate. According to the invention, raw materials have high quality and stable properties; by-produced impurities produced during synthesis of ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate can be removed through neutralization, and ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate with a purity of higher than 99.0%, which meets market demands for the high-purity photoinitiator ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate.

Description

technical field [0001] The invention relates to a preparation method of high-purity ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate, belonging to the field of fine chemicals preparation. Background technique [0002] (2,4,6-trimethylbenzoyl) ethyl phenylphosphinate (photoinitiator TPO-L) is an important photoinitiator, because it is liquid at normal temperature, it is easy to use, and Good base material compatibility and other characteristics are widely used in the paint and coating industry. At present, there are mainly two methods for the preparation of TPO-L. One is the Abuzoff reaction method through diethoxyphenylphosphine and 2,4,6-trimethylbenzoyl chloride. The main problem of this method is its second The raw material of ethoxyphenylphosphine is easy to decompose, and the impurity of diethyl phenylphosphonate in the preparation leads to poor purity of the target compound, which can only reach about 95%. The application of the synthesized product in the high-end fiel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32
CPCC07F9/3252C07F9/3264
Inventor 王忠卫吴邦元王祥李焕成侯计金
Owner 江苏富比亚化学品有限公司
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