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

A technology of trimethylbenzoyl and phenylphosphine oxide, which is applied in the field of preparation of high-efficiency free radical photoinitiator phenylphosphine oxide, can solve the problems of high cost, difficult industrial implementation, and large amount of waste water, and achieve cost saving , avoid the effect of high price and high reaction yield

Active Publication Date: 2014-08-13
湖南久日新材料有限公司
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  • Summary
  • Abstract
  • 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 phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide

Examples

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Embodiment 1

[0033] Example 1: Preparation of phenylbis(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 flask under nitrogen protection, heat it to reflux, stir vigorously until the sodium block becomes very fine, slowly add P,P- Dichlorophenylphosphine (39.4g, 0.22mol) was dripped in 0.5h, the reaction was continued for 16h, the temperature was lowered to below the boiling point, water (10.0g, 0.55mol) was added dropwise within 0.5h, and the reaction was refluxed until the sodium was completely consumed to obtain Phenylphosphine-containing solution. The solvent was recovered by low-pressure distillation, and the fractions at 40-45°C / 10 mHg were collected and confirmed by nuclear magnetic resonance. 31 P: -123ppm. After the solvent is recovered, the next step reaction can also be carried out directly without purification;

[0036] 2) Preparation of phenylphosphine o...

Embodiment 2

[0042] Example 2: Preparation of phenylbis(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 dropwise add 37.1g of 2,4,6 -Trimethylbenzaldehyde (0.25mol), dripped for 1h, then heated up for reaction, heated to 60°C, kept for reaction, 31 P-NMR monitors the reaction, when the phenylphosphine oxide disappears, the reaction is complete, and the reaction is lowered to room temperature, and the obtained reaction solution can be directly reacted in the next step without purification;

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

[0046] The bishydroxyphosphine oxide prepared in step 3) ( A ) The reaction solution was directly used in this step, and 2.5g of V(IV)(acac) was added. 2 , under stirring, slowly add 28.3g of 30% h...

Embodiment 3

[0047] Example 3: Preparation of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide

[0048] 1) Bishydroxyphosphine oxide ( A ) preparation

[0049] Under nitrogen protection, 12.6g of phenylphosphine oxide (0.10mol) was dissolved in 100ml of dichloroethane, 22.5g of 40% dimethylamine aqueous solution was added respectively, the temperature was lowered to -5°C, and 37.1g of 2,4 was slowly added dropwise. , 6-trimethylbenzaldehyde (0.25mol), dripped for 1h, then heated up for the reaction, heated to 60°C, kept for the reaction, 31 P-NMR monitors the reaction, when the phenylphosphine oxide disappears, the reaction is complete, and the reaction is lowered to room temperature, and the obtained reaction solution can be directly reacted in the next step without purification;

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

[0051] The bishydroxyphosphine oxide prepared in step 3) ( A ) The reaction solution was directly used in this step, and 2.5g ...

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Abstract

The invention discloses a preparation method of phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide as an efficient free radical photoinitiator. The preparation method of phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide comprises the concrete steps of with 2,4,6-trimethylbenzaldehyde as a raw material, enabling 2,4,6-trimethylbenzaldehyde and phenylphosphine oxide to be subjected to condensation reaction in the existence of a catalyst, and then, carrying out oxidation reaction. Extraction and solvent replacement are not needed and continuous reaction can be realized in the reaction process. The preparation method of phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide, disclosed by the invention, is low in price, environment-friendly, easy to operate and suitable for realizing 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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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
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