A kind of acyl phosphine efficient photoinitiator and preparation method thereof
A technology of photoinitiator and acylphosphine, which is applied in the field of photoinitiator preparation, can solve problems such as the difficulty of synthesis technology, and achieve the effect of improving yield and production efficiency
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Embodiment 1
[0038] Synthesis of bisacylphosphine compounds: Add 650ml of toluene and 124g of sodium amalgam (1:1) to a four-neck flask (1000ml) equipped with a dropping funnel, a stirrer, and a thermometer in an inert atmosphere; the temperature rises to 40°C Start stirring, continue to heat up to reflux, and dropwise add 44 g of phenylphosphorous dichloride. Heat to reflux for 1h. Add 42 g of tert-butanol dropwise to the reaction flask, and heat to reflux for 1 h. After the reaction was completed, under nitrogen protection, the temperature was lowered to below 30°C, and 93g of 2,4,6-trimethylbenzoyl chloride was added dropwise. After the drop, the temperature was controlled at 40±5°C, and the reaction was carried out for 1h. Then add 5% sodium carbonate dropwise, adjust the pH to 7, separate the water layer, wash with water, concentrate, crystallize, filter, and dry to obtain 114g of the target product, with a yield of 91%, a content of ≥99%, and a melting point of 127-131°C.
Embodiment 2
[0040] The synthesis of bisacylphosphine compound: under inert atmosphere, drop into the four-necked flask (1000ml) that is equipped with dropping funnel, stirrer, thermometer successively into toluene 650ml, metal magnesium sodium alloy (1:1) 24g; Temperature rises to 90 Start stirring at ℃, continue to heat up to reflux, and add 44 g of phenylphosphorous dichloride dropwise. Heat to reflux for 1h. Add 42 g of tert-butanol dropwise to the reaction flask, and heat to reflux for 1 h. After the reaction was completed, under nitrogen protection, the temperature was lowered to below 30°C, and 93g of 2,4,6-trimethylbenzoyl chloride was added dropwise. After the drop, the temperature was controlled at 40±5°C, and the reaction was carried out for 1h. Then add 5% sodium carbonate dropwise, adjust the pH to 7, separate the water layer, wash with water, concentrate, crystallize, filter, and dry to obtain 112g of the target product, with a yield of 90%, a content of ≥99%, and a melting ...
Embodiment 3
[0042] Synthesis of bisacylphosphine compounds: Add 650ml of toluene and 30g of metal potassium and magnesium (1:1) into a four-necked flask (1000ml) equipped with a dropping funnel, a stirrer and a thermometer in an inert atmosphere, and the temperature rises to 50°C , start stirring, continue to heat up to reflux, dropwise add 44g of phenyl phosphorus dichloride, and heat to reflux for 1h. Add 42 g of tert-butanol dropwise into the reaction flask, and heat to reflux for 1 h. After the reaction was completed, under nitrogen protection, the temperature was lowered to below 30°C, and 93g of 2,4,6-trimethylbenzoyl chloride was added dropwise, and the temperature was controlled at 40±5°C after the dropping, and reacted for 1h. Then add 5% sodium carbonate dropwise, adjust the pH to 7, separate the water layer, wash with water, concentrate, crystallize, filter, and dry to obtain 114g of the target product, with a yield of 91%, a content of ≥99%, and a melting point of 127-131°C.
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