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

A technology of trimethylbenzoyl and phenylbis, which is applied in the field of preparation of high-efficiency free radical photoinitiator phenylbisphosphine oxide, can solve the problems of high environmental pressure, difficult industrial implementation, and high cost, and achieves no environmental pressure. , Improve the reaction rate, the effect of cleaning by-products

Active Publication Date: 2015-04-29
TIANJIN JIURI NEW MATERIALS CO LTD
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Problems solved by technology

[0007] The technical problem to be solved in the present invention is to provide a new phenyl bis(2,4,6-trimethylbenzoyl) phosphine oxide preparation process to...

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

Examples

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Embodiment 1

[0042] Embodiment 1: the preparation of phenylphosphine

[0043] Add 500ml of toluene and sodium block (10.1g, 0.88mol) into a 1000ml reaction bottle under the protection of argon, heat until reflux, stir vigorously, and slowly add dichlorobenzene dropwise when the sodium block becomes very fine Phenylphosphine (39.4g, 0.22mol), after 0.5h of dripping, continue to keep warm for 16h, cool down to below the boiling point, then slowly add water (10.0g, 0.55mol), reflux reaction until the sodium is completely consumed, and the phenylphosphine containing solution.

[0044] Low-pressure distillation recovered the solvent for purification, and collected 40-45°C / 10 mHg fractions to obtain 20.0 g of phenylphosphine, which was confirmed by nuclear magnetic resonance. 31 P: -123ppm.

[0045] Or install a water separator, reflux for dehydration, and remove 50ml of toluene-water mixture to obtain anhydrous toluene solution of phenylphosphine, which is confirmed by nuclear magnetic reson...

Embodiment 2

[0046] Embodiment 2: Preparation of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

[0047] Under the protection of argon, take 17.3g of sodium hydride (60%, 0.44mol) and evenly disperse in 50ml of toluene, slowly add dropwise 20.0g (0.18mol) of phenylphosphine (dissolved in 450ml of toluene solution) prepared in Example 1 After dropping, reflux reaction for 2-4h, the color of the reaction system changed from yellow-green to dark yellow, and finally into a reddish-brown viscous system, down to room temperature, dropwise added 73.1g (0.40mol) 2,4,6-trimethyl Benzoyl chloride, the reaction is exothermic, after dripping, the reaction system gradually turns into a red transparent solution, an orange transparent solution, the temperature is raised to about 40°C, and the reaction is kept for about 5 hours. The reaction is monitored by liquid chromatography. After the reaction is complete, add hydrochloric acid solution to wash , adjust the pH at 4-6, stir for 30min, stand and...

Embodiment 3

[0048] Embodiment 3: Preparation of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

[0049] Under the protection of argon, get 17.3g sodium hydride (60%, 0.44mol) and evenly disperse in 50ml toluene, slowly add the anhydrous toluene solution of the phenylphosphine prepared after embodiment 1 divides water (from dichlorobenzene phenylphosphine (39.4g, 0.22mol) prepared phenylphosphine solution), dropwise, reflux reaction for 2-4h, the color of the reaction system changed from yellow-green to dark yellow, and finally into a reddish-brown viscous system, down to room temperature , add 80.4g of 2,4,6-trimethylbenzoyl chloride dropwise, the reaction is exothermic, after dropping, the reaction system gradually turns into a red transparent solution, an orange transparent solution, the temperature is raised to about 40°C, and the reaction is kept for about 5 hours. Monitor the reaction by phase chromatography. After the reaction is complete, add 120ml of 5% hydrochloric acid so...

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Abstract

The invention discloses a preparation method of an efficient free radical photoinitiator phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide. Specifically, phenyl phosphine is used as a raw material and reacts with 2,4,6-trimethylbenzoyl chloride under the effect of an alkaline compound to obtain an intermediate; and through an oxidation reaction of the intermediate, the phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide is obtained. The preparation method disclosed by the invention is cheap, easy to operate, high in yield, environmentally friendly and suitable for industrialization.

Description

technical field [0001] The invention relates to a preparation method of a high-efficiency free radical photoinitiator phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide, in particular to phenylphosphine as a raw material and 2 under the action of a basic compound , 4,6-trimethylbenzoyl chloride reaction, the obtained intermediate is prepared through oxidation reaction to obtain the method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide. Background technique [0002] Phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide is a highly efficient bisacylphosphine oxide photoinitiator, suitable for initiating the radiation polymerization of some unsaturated resins under ultraviolet light irradiation, Its deep curing effect is very 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., especially suitable for white formulations and glass fiber reinforced polyester / styrene system...

Claims

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Application Information

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IPC IPC(8): C07F9/53
CPCC07F9/53
Inventor 廖文骏张磊
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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