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Preparation method of 2,4,6-trimethylbenzoyldiphenyl phosphine oxide

A technology of trimethylbenzoyldiphenyl and triphenylphosphine, which is applied in the field of preparation of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, can solve the problem of large-scale production difficulty, High equipment requirements, difficult recycling and other issues, to achieve the effect of easy industrialization, simple operation and environmental friendliness

Active Publication Date: 2016-05-04
SHANDONG JIURI CHEM TECH CO LTD
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

It is difficult to recover a large amount of acid-binding agents after use, which makes the preparation cost of the final product high
Simultaneously this step condensation reaction obtained intermediate Ph 2 P(OR) needs to be obtained by distillation under high vacuum conditions, so the requirements for equipment are high, and the yield is often low. The Arbusov-Michelies reaction often has a long reaction cycle and difficult post-processing, mainly due to the raw material Ph 2 PCl contains PhPCl 2 , leading to the formation of liquid by-products, which are wrapped with the product and difficult to purify, so large-scale production is difficult
[0008] In addition, this type of preparation method is prepared with diphenylphosphine chloride as the starting material, Ph 2 PCl is generally prepared from phenylphosphine dichloride, the conversion rate is generally less than 40%, the product purification is difficult, the cost is very high, and the environmental pressure is high

Method used

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  • Preparation method of 2,4,6-trimethylbenzoyldiphenyl phosphine oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 12

[0032] Example 12 Preparation method of 4,6-trimethylbenzoyl diphenyl phosphine oxide

[0033] 1) Under the protection of nitrogen, suspend the metallic sodium block (6.9g, 0.3mol) in 80ml of toluene, heat until refluxing, stir vigorously to form a powdered sodium suspension, add triphenylphosphine dropwise under vigorous stirring (26.2g, 0.1mol), after dripping, heat and reflux to react. When the triphenylphosphine reaction is complete, cool to room temperature, add phosphorus trichloride (6.9g, 0.05mol) dropwise, stir vigorously during the dripping process. , After dripping, heat to 100℃ to keep the reaction, TLC monitors the reaction;

[0034] 2) Cool the mixture obtained in step 1) to 80°C, add 2,4,6-trimethylbenzoyl chloride (27.4g, 0.15mol) dropwise at this temperature, drop the reaction, keep the reaction warm, and after the reaction is complete , Add water to the reaction system, stir and react for 0.5h;

[0035] 3) Add 30% hydrogen peroxide (51.0g, 0.45mol) to the reaction...

Embodiment 22

[0036] Example 22 Preparation method of 4,6-trimethylbenzoyl diphenyl phosphine oxide

[0037] 1) Under the protection of nitrogen, suspend the metal sodium block (6.9g, 0.3mol) in 80ml ethylbenzene, heat it until reflux, and stir vigorously to form a powdered sodium suspension, then add triphenylbenzene dropwise under vigorous stirring Phosphine (26.2g, 0.1mol), after dripping, heat to reflux for reaction, when the triphenylphosphine reaction is complete, cool to room temperature, add phosphorus trichloride (6.9g, 0.05mol) dropwise, stir vigorously during the dropping After the reaction, heat the reaction to 100°C after dropping, and monitor the reaction by TLC;

[0038] 2) Cool the mixture obtained in step 1) to 80°C, add 2,4,6-trimethylbenzoyl chloride (27.4g, 0.15mol) dropwise at this temperature, drop the reaction, keep the reaction warm, and after the reaction is complete , Add water to the reaction system, stir and react for 0.5h;

[0039] 3) Add 30% hydrogen peroxide (51.0g...

Embodiment 32

[0040] Example 32 Preparation method of 4,6-trimethylbenzoyl diphenyl phosphine oxide

[0041] 1) Under the protection of nitrogen, suspend the metallic sodium block (6.9g, 0.3mol) in 80ml of toluene, heat until refluxing, stir vigorously to form a powdered sodium suspension, add triphenylphosphine dropwise under vigorous stirring (26.2g, 0.1mol), after dripping, heat and reflux to react. When the triphenylphosphine reaction is complete, cool to room temperature, add phosphorus trichloride (6.9g, 0.05mol) dropwise, stir vigorously during the dripping process. , After dripping, heat to 100℃ to keep the reaction, TLC monitors the reaction;

[0042] 2) Cool the mixture obtained in step 1) to 80°C, add dropwise 2,4,6-trimethylbenzoyl chloride (31.1g, 0.17mol) at this temperature, drop the reaction, keep the reaction warm, and after the reaction is complete , Add water to the reaction system, stir and react for 0.5h;

[0043] 3) Add 30% hydrogen peroxide (51.0g, 0.45mol) to the reaction...

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Abstract

The invention discloses a preparation method of 2,4,6-trimethylbenzoyldiphenyl phosphine oxide. According to the preparation method, triphenyl phosphine is taken as the raw material, triphenyl phosphine reacts with metal sodium and phosphorus halide to generate reaction product (I), the reaction product (I) reacts with acyl chloride to generate reaction product (II), and the reaction product (II) is oxidized to produce 2,4,6-trimethylbenzoyldiphenyl phosphine oxide. The preparation method has the advantages of easily-available raw materials, low cost, easy operation, environment-friendliness, and easiness for industrialization.

Description

Technical field [0001] The present invention relates to a preparation process of 2,4,6-trimethylbenzoyl diphenyl phosphine oxide, in particular to a preparation process using triphenyl phosphine as a raw material, simple process, low cost, and environmentally friendly 2. 4,6-Trimethylbenzoyl diphenyl phosphine oxide method. Background technique [0002] TPO is a highly efficient free radical (I) type photoinitiator, which can absorb in the long wavelength range. Because it has a wide absorption range, its effective absorption peak is 350-400nm, and it absorbs to about 420nm. Its absorption peak is longer than conventional initiators, and it can generate benzoyl and phosphoryl radicals after exposure to light. , Can initiate polymerization, so the light curing speed is fast, and it is suitable for deep curing of thick film. It also has photobleaching effect and the coating does not turn yellow. It can be completely cured on white or high-titanium dioxide pigmented surfaces, with...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
CPCC07F9/5337
Inventor 张齐武瑞毛桂红吴吉蒋雷李扣喜敖文亮
Owner SHANDONG JIURI CHEM TECH CO LTD
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