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Preparation method of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide

A technology of trimethylbenzoyl and phenyl phosphine oxide, which is applied in the field of preparation of high-efficiency free radical photoinitiator phenyl bis phosphine oxide, can solve the problems of excessive waste water, high cost, and difficult industrial implementation, and achieve reaction yield The effect of high efficiency, cost saving, and avoiding expensive prices

Active Publication Date: 2016-01-13
湖南久日新材料有限公司
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation process can overcome the problems of high cost, high toxicity, large amount of waste water, and difficult industrial implementation in the existing methods of starting materials or processes. It is a low-cost, environmentally friendly, high yield, easy to operate, and has industrial production value. preparation method

Method used

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  • Preparation method of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide

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Embodiment 1

[0033]Embodiment 1: Preparation of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

[0034] 1) Preparation of phenylphosphine:

[0035] Add 800ml of toluene and sodium block (10.1g, 0.88mol) into a 2000ml reaction bottle under nitrogen protection, heat until reflux, stir vigorously, and slowly drop P,P- Dichlorophenylphosphine (39.4g, 0.22mol), after 0.5h of dripping, continue to keep warm for 16h, cool down to below the boiling point, add water (10.0g, 0.55mol) dropwise within 0.5h, reflux until the sodium is completely consumed, and get Solutions containing phenylphosphine. Low-pressure distillation recovery solvent purification, collecting 40-45 ℃ / 10mHg fraction, nuclear magnetic resonance confirmation, 31 P: -123ppm. After recovering the solvent, the next reaction can be directly carried out without purification;

[0036] 2) Preparation of phenylphosphine oxide:

[0037] Under a nitrogen atmosphere, dissolve the phenylphosphine (12.1g, 0.11mol) prepared in step ...

Embodiment 2

[0042] Embodiment 2: Preparation of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

[0043] 1) Bishydroxyphosphine oxide ( A ) preparation

[0044] Under nitrogen protection, dissolve 12.6g of phenylphosphine oxide (0.10mol) in 100ml of dichloroethane, add 40.0g of 20% sodium hydroxide, cool down to -5°C, and slowly add 37.1g of 2,4,6-tri Methyl benzaldehyde (0.25mol), after 1 hour of dripping, then heat up to 60°C, keep warm for reaction, 31 P-NMR monitors the reaction. When the phenylphosphine oxide disappears, the reaction is complete and cooled to room temperature. The obtained reaction solution is directly reacted in the next step without purification;

[0045] 2) Preparation of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide

[0046] The bishydroxyphosphine oxide ( A ) The reaction solution is directly used in this step reaction, adding 2.5gV(Ⅳ)(acac) 2 , under stirring, slowly add 28.3g of 30% hydrogen peroxide dropwise, after 0.5h drop, react at room tem...

Embodiment 3

[0047] Embodiment 3: Preparation of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

[0048] 1) Bishydroxyphosphine oxide ( A ) preparation

[0049] Under nitrogen protection, dissolve 12.6g of phenylphosphine oxide (0.10mol) in 100ml of dichloroethane, add 22.5g of 40% dimethylamine aqueous solution, cool down to -5°C, and slowly add 37.1g of 2,4,6 -Trimethylbenzaldehyde (0.25mol), dripping for 1 hour, then heating up to 60°C, keeping warm for reaction, 31 P-NMR monitors the reaction. When the phenylphosphine oxide disappears, the reaction is complete and cooled to room temperature. The obtained reaction solution is directly reacted in the next step without purification;

[0050] 2) Preparation of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide

[0051] The bishydroxyphosphine oxide ( A ) The reaction solution is directly used in this step reaction, adding 2.5gV(Ⅳ)(acac) 2 , under stirring, slowly add 28.330% (mass percentage) hydrogen peroxide dropwise, 0.5h to...

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Abstract

The invention discloses a preparation method of a high-efficiency free radical photoinitiator phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide, specifically phenylbis(2,4,6-trimethylbenzoyl) The preparation method of benzoyl)phosphine oxide uses 2,4,6-trimethylbenzaldehyde as a raw material, in the presence of a catalyst, undergoes condensation reaction with phenylphosphine oxide, and then undergoes oxidation reaction. The reaction process does not need to be purified, and the solvent can be continuously reacted without changing the solvent. The preparation method of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide disclosed by the present invention is a cheap, environmentally friendly, easy-to-operate, The preparation method is suitable for industrialization.

Description

technical field [0001] The invention relates to a preparation method of a high-efficiency free radical photoinitiator phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide, in particular to phenyl bis (2,4,6-trimethylbenzoyl) Formyl)phosphine oxide uses rice aldehyde (2,4,6-trimethylbenzaldehyde) and phenylphosphine oxide as raw materials, and the reaction intermediate can be continuously reacted without purification and solvent replacement, providing a cheap and environmentally friendly , easy to operate and suitable for industrialized preparation method. Background technique [0002] Phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide is a very efficient bisacylphosphine oxide photoinitiator, suitable for the radiation polymerization of some unsaturated resins under ultraviolet light irradiation , its deep curing effect is ideal. Suitable for UV-curable varnish and paint systems, such as for wood, paper, metal, plastic, optical fiber and printing inks and prepreg systems, etc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/53
Inventor 吕振波毛桂红石智铭张磊刘川伟张建锋武瑞张齐徐新元赵国锋
Owner 湖南久日新材料有限公司