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Preparation method for photoinitiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide

A technology of trimethylbenzoyl and phenylphosphine oxide, applied in the chemical industry, can solve problems such as unsafe yield, and achieve the effects of reducing production cost, mild conditions, and avoiding pollutant discharge

Inactive Publication Date: 2014-11-19
ZHANGJIAGANG JIMUTE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to overcome the unsafe and low-yield technical defects in the existing method for synthesizing photoinitiator 819, the present invention provides a method with low preparation cost, simple and safe operation process, easy control of the reaction process, high product yield and good purity , the preparation method of bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide (photoinitiator 819 for short) that is easy to realize large-scale production

Method used

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  • Preparation method for photoinitiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of preparation method of two (2,4,6-trimethylbenzoyl) phenyl phosphine oxides of photoinitiator, the steps are as follows:

[0029] (1) Under nitrogen protection, add 100ml of toluene as solvent and aluminum trichloride (0.28mol, 37.2g) to the 250ml reaction bottle, at room temperature, stir and add trimethylsilane (0.25mol, 0.25mol, 18.5g), and continued to stir for 0.5 hours; then slowly add phenylphosphine dichloride (0.1mol, 19.4g) dropwise to the reaction flask after heating up to 80°C, and control the rate of addition to keep the reaction temperature constant. After the phosphine was added dropwise, continue to stir for 3 hours to obtain two (aluminum dichloride) phosphine salt intermediates;

[0030] (2) When the temperature of the reaction flask drops to 50°C, slowly add 2,4,6-trimethylbenzoyl chloride (0.22mol, 40g) dropwise into the reaction flask. After the addition is complete, continue heating to control the reaction temperature In the range of 70-8...

Embodiment 2

[0035] (1) Add 200ml toluene as solvent and aluminum trichloride (0.56mol, 74.4g) to the 500ml reaction flask under nitrogen protection, at room temperature, stir and add trimethylsilane (0.5mol, 37.0g), and keep stirring for 45 Minutes; then heat up to 70-80°C, slowly add phenylphosphine dichloride (0.2mol, 38.8g) dropwise to the reaction flask, keep the reaction temperature constant, and continue stirring after the addition of phenylphosphine dichloride is completed In 3 hours, two (aluminum dichloride) phosphonium salt intermediates were obtained;

[0036] (2) Lower the temperature of the reaction flask to 50°C, add 2,4,6-trimethylbenzoyl chloride (0.44mol, 80.0g) dropwise to the reaction flask, and continue heating after the addition is completed, at 100°C Under the conditions of reaction for 4.5 hours, the intermediate product bis(2,4,6-trimethylbenzoyl)phenylphosphine was obtained;

[0037] (3) Cool the reaction flask to 50°C, feed excess nitrogen dioxide gas into the r...

Embodiment 3

[0041] (1) Add 200ml of toluene as solvent and aluminum trichloride (0.56mol, 74.4g) to a 500ml reaction flask under nitrogen protection, at room temperature, stir and add trimethylsilane (0.5mol, 37.0g), and continue stirring for 30min Then be warming up to 100 ℃, slowly dropwise add phenylphosphine dichloride (0.2mol, 38.8g) in reaction flask, keep reaction temperature constant, after treating that phenylphosphine dichloride is added dropwise, continue to stir for 3 hours, Obtain bis (aluminum dichloride) phosphonium salt intermediate;

[0042] (2) Lower the temperature of the reaction flask to 50°C, add 2,4,6-trimethylbenzoyl chloride (0.44mol, 80.0g) dropwise to the reaction flask, and continue heating after the addition is completed, at 100°C Under the conditions of reaction for 4 hours, the intermediate product bis(2,4,6-trimethylbenzoyl)phenylphosphine was obtained;

[0043] (3) The reaction flask is cooled to room temperature, and excessive nitrogen dioxide gas is pas...

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Abstract

The invention discloses a preparation method for a photoinitiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide. The preparation method comprises the synthesis steps: under the protection of inert gas, carrying out a reaction of aluminium trichloride or tin tetrachloride and trimethylsilane in the temperature range of 0-100 DEG C to obtain aluminium dichloride ions, and rapidly acting with dichlorophenyl phosphine in the reaction system, to obtain a bis(aluminium trichloride or tin tetrachloride)phosphine salt intermediate; then carrying out a reaction of the intermediate and 2,4,6-trimethyl benzoyl chloride, to obtain bis(2,4,6-trimethylbenzoyl)phenyl phosphine; and under the condition of the temperature of 20-50 DEG C, oxidizing by nitrogen dioxide, to obtain the target product. The method avoids use of a dangerous active metal potassium or sodium, and adopts aluminium trichloride or tin tetrachloride with relatively low price and trimethylsilane for on-site generation of the active intermediate to achieve the reaction. The method has the characteristics of low preparation cost, simple and safe operation process, easy control of the reaction process, high product yield, good purity, easy realization of mass production and the like.

Description

technical field [0001] The invention relates to a preparation method of a photoinitiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide, which belongs to the technical field of chemical industry. Background technique [0002] Bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide (product code photoinitiator 819) is a new type of photoinitiator with good photochemical reactivity. It can efficiently generate aroyl-phosphinyl radicals, has fast photodecomposition speed, fast photocuring speed, and has a bleaching effect, which is conducive to the curing of thick coatings. Bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide has excellent properties and is often used in combination with secondary and tertiary amines in many fields such as coatings, inks, adhesives, resists, soldering agents, etc. be widely used. In recent years, with the development of UV curing technology, photoinitiator 819 has also been widely used and developed in this field. It can be used to initiate polymeriza...

Claims

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Application Information

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IPC IPC(8): C07F9/53C07F7/12
Inventor 赵经伟沈清胡王漪
Owner ZHANGJIAGANG JIMUTE CHEM TECH
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