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A kind of preparation method of 2,4,6 trimethylbenzoyl diphenyl phosphine oxide

A technology of trimethylbenzoyldiphenyl and triphenylphosphine, applied in the field of preparation of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, which can solve the difficulty of recovery and high equipment requirements , Difficult to purify and other problems, to achieve the effect of easy industrialization, solving difficult and difficult preparation

Active Publication Date: 2017-08-25
SHANDONG JIURI CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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  • A kind of preparation method of 2,4,6 trimethylbenzoyl diphenyl phosphine oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 The preparation method of 2,4,6-trimethylbenzoyldiphenylphosphine oxide

[0033] 1) Under the protection of nitrogen, suspend metal sodium block (6.9g, 0.3mol) in 80ml toluene, heat until reflux, and stir vigorously to form a suspension of powdery sodium, then add triphenylphosphine dropwise under vigorous stirring (26.2g, 0.1mol), after dropping, heat to reflux for reaction, when the reaction of triphenylphosphine is complete, cool down to room temperature, add phosphorus trichloride (6.9g, 0.05mol) dropwise, stir vigorously during the dropwise addition After dropping, heat to 100°C to keep warm for reaction, and TLC to monitor 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, and react after dropping, keep warm for the reaction, after the reaction is complete , add water to the reaction system, stir and react for 0.5h;

[0035] 3) Add 30% hydrogen perox...

Embodiment 2

[0036] Example 2 The preparation method of 2,4,6-trimethylbenzoyldiphenylphosphine oxide

[0037]1) Under the protection of nitrogen, suspend metal sodium block (6.9g, 0.3mol) in 80ml ethylbenzene, heat until reflux, stir vigorously, after forming a suspension of powdery sodium, add triphenyl triphenyl under vigorous stirring Phosphine (26.2g, 0.1mol), after dropping, heat to reflux for reaction, when the reaction of triphenylphosphine is complete, cool down to room temperature, add phosphorus trichloride (6.9g, 0.05mol) dropwise, stir vigorously during the dropwise addition Reaction, heating to 100°C for reaction after dropping, TLC monitoring reaction;

[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, and react after dropping, keep warm for the reaction, after the reaction is complete , add water to the reaction system, stir and react for 0.5h;

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

Embodiment 3

[0040] Example 3 Preparation method of 2,4,6-trimethylbenzoyldiphenylphosphine oxide

[0041] 1) Under the protection of nitrogen, suspend metal sodium block (6.9g, 0.3mol) in 80ml toluene, heat until reflux, and stir vigorously to form a suspension of powdery sodium, then add triphenylphosphine dropwise under vigorous stirring (26.2g, 0.1mol), after dropping, heat to reflux for reaction, when the reaction of triphenylphosphine is complete, cool down to room temperature, add phosphorus trichloride (6.9g, 0.05mol) dropwise, stir vigorously during the dropwise addition After dropping, heat to 100°C to keep warm for reaction, and TLC to monitor the reaction;

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

[0043] 3) Add 30% hydrogen peroxide ...

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PUM

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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 diphenylphosphine oxide, in particular to a preparation method using triphenylphosphine as raw material, which has simple process, low cost and environment-friendly. 4,6-Trimethylbenzoyldiphenylphosphine oxide method. Background technique [0002] TPO is a high-efficiency free radical (I) type photoinitiator that absorbs 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 that of conventional initiators, and it can generate two free radicals, benzoyl and phosphoryl, after being illuminated. , can initiate polymerization, so the photocuring speed is fast, and it is suitable for deep curing of thick films. It also has photobleaching effect, and the coating does not yellow. It can be completely cured on white or high-titanium dioxide pigmented surf...

Claims

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Application Information

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Patent Type & Authority Patents(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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