Synthetic method of photoinitiator dual (2,4,6-trimethylbenzene formyl group) phenyl phosphine oxide

A technology of trimethylbenzoyl and photoinitiator, applied in the field of chemical industry, can solve problems such as unsafe yield, and achieve the effects of low comprehensive cost, high safety, and not easy to fire

Active Publication Date: 2015-05-27
SHANDONG UNIV OF SCI & TECH
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  • Description
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Problems solved by technology

[0004] In order to overcome the unsafe and low-yield technical defects existing in the existing method for synthesizing photoinitiator 819, the present invention provides a bis( The synthetic method of 2,4,6-trimethylbenzoyl)-phenylphosphine oxide (photoinitiator 819 for short)

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  • Synthetic method of photoinitiator dual (2,4,6-trimethylbenzene formyl group) phenyl phosphine oxide

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Experimental program
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Effect test

Embodiment 1

[0021] Step 1: Add 17.9 grams of phenylphosphine dichloride and 100 mL of toluene into a 250 mL reactor as a solvent, pass through nitrogen to remove oxygen, and add 4.0 grams of pure water dropwise under nitrogen protection to control the temperature within 0°C. Incubate at -10°C for 2 hours to generate phenylphosphine and by-product phenylphosphonic acid.

[0022] The second step: filter, the filter cake is washed with an appropriate amount of toluene, and the obtained solid is the by-product phenylphosphonic acid; a small amount of anhydrous calcium chloride is added to the filtrate, and the calcium chloride is removed by filtration, and the filtrate is transferred to the reactor, and the temperature is controlled at 60 Add 12.2 grams of 2,4,6-trimethylbenzoyl chloride dropwise at ℃, keep warm at 60℃ for 2 hours after the addition, adjust the reaction solution to neutral with 10% sodium hydroxide, separate the organic layer to obtain the intermediate product Bis(2,4,6-trime...

Embodiment 2

[0026] Step 1: Add 17.9 grams of phenylphosphine dichloride and 100 mL of chloroform into a 250 mL reactor as a solvent, pass through nitrogen to remove oxygen, control the temperature within 0 ° C under the protection of nitrogen, add 3.8 grams of pure water dropwise, after adding 0-10 ° C for 2 hours to generate phenylphosphine and by-product phenylphosphonic acid.

[0027] The second step: filtering, the filter cake is washed with an appropriate amount of chloroform, and the obtained solid is the by-product phenylphosphonic acid. Add a small amount of anhydrous calcium chloride to the filtrate, remove the calcium chloride by filtration, transfer the filtrate to the reactor, add 12.2 grams of 2,4,6-trimethylbenzoyl chloride dropwise at a controlled temperature of 60°C, and add it at 60 The temperature was kept at ℃ for 2 hours, and after the heat preservation, the reaction solution was adjusted to neutrality with 10% sodium hydroxide, and the organic layer was separated to o...

Embodiment 3

[0032] Step 1: Add 17.9 grams of phenylphosphine dichloride to a 250 mL reactor, then add 100 mL as a solvent, pass through nitrogen to remove oxygen, control the temperature within 0°C under the protection of nitrogen, add 3.8 grams of pure water dropwise, after adding Incubate at 80°C for 2 hours.

[0033] The second step: filtering, the filter cake is washed with an appropriate amount of chloroform, and the obtained solid is the by-product phenylphosphonic acid. Add a small amount of anhydrous calcium chloride to the filtrate, remove the calcium chloride by filtration, transfer the filtrate to the reactor, add 12.2 grams of 2,4,6-trimethylbenzoyl chloride dropwise at a controlled temperature of 60°C, and add it at 60 The temperature was kept at ℃ for 2 hours, and after the heat preservation, the reaction solution was adjusted to neutrality with 10% sodium hydroxide, and the organic layer was separated to obtain the intermediate product bis(2,4,6-trimethylbenzoyl)phenylphosp...

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Abstract

The invention discloses a synthetic method of photoinitiator dual (2, 4, 6-trimethylbenzene formyl group) phenyl phosphine oxide. The synthetic method comprises processes of using dichlorophenylphosphine and 2, 4, 6-trimethylbenzene acyl chloride to serve as raw materials, conducting a classification reaction under protection of nitrogen to generate dual(2, 4, 6-trimethylbenzene formyl group) phenyl phosphine, oxidizing hydrogen peroxide to obtain a target object-dual (2, 4, 6-trimethylbenzene formyl group) phenyl phosphine oxide. Compared with the existing industrial production, the process has the advantages of being safe in operation process, free of needs of dangerous metallic sodium or potassium, free of needs of using inflammable midbody phenyl phosphine, simple in reaction process, safe, easy to control, high in obtained product yield, good in quality and prone to achieve mass production and the like.

Description

technical field [0001] The invention relates to a synthesis method of bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide, an organophosphorus compound, and belongs to the technical field of chemical industry. Background technique [0002] Bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide (product code photoinitiator 819), is a highly efficient photoinitiator, suitable for initiating some unsaturated resins under ultraviolet light irradiation Radiation polymerization reaction, especially suitable for white formulations and glass fiber reinforced polyester / styrene systems and for outdoor varnish systems and paint systems in combination with light stabilizers, such as for wood, paper, metal, plastics, optical fibers As well as printing inks and prepreg systems, etc. [0003] At present, there are mainly two methods for industrial synthesis of photoinitiator 819. One is to react with metal sodium or potassium in a solvent by phenylphosphine dichloride, and then react with 2,4,6-t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/53
Inventor 王忠卫于青靳涛武清浴刘炳艳
Owner SHANDONG UNIV OF SCI & TECH
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