Method for preparing photoinitiator, namely TPO and simultaneously preparing byproduct, namely benzyl chloride
A photoinitiator and by-product technology, which is applied in the field of preparing photoinitiator TPO and by-product benzyl chloride, can solve the problems of shortening the reaction time, achieve the effects of reducing production costs, avoiding environmental hazards, and reducing recycling costs and losses
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Embodiment 1
[0033] Embodiment 1: the preparation of TPO and benzyl chloride
[0034] Dissolve 109.2g of benzyl alcohol in 100ml of toluene, add 108.1g of sodium carbonate, cool to 15°C, add 221g of diphenylphosphorus chloride dropwise, and control the temperature at 15±5°C. After the dropwise addition, slowly raise the temperature to 25°C and keep it warm for 2 hours. The reaction of diphenylphosphorous chloride is complete by gas phase monitoring, and the residual benzyl alcohol is less than 0.5%. After the reaction was completed, the insoluble salt was filtered out.
[0035] The temperature of the filtrate was raised to 100°C, and 200.1 g of 2,4,6-trimethylbenzoyl chloride was slowly added dropwise, and the reaction was continued for 4 hours after the drop was completed. After the reaction was completed, the temperature was lowered to cool and crystallize, and the product TPO 300g was obtained by filtration, with a yield of 86.2%. The solvent was distilled from the crystallization mot...
Embodiment 2
[0036] Embodiment 2: the preparation of TPO and benzyl chloride
[0037] Dissolve 110.3g of benzyl alcohol in 100ml of toluene, add 115g of sodium carbonate, control the temperature at 25°C, add dropwise 221g of diphenylphosphorus chloride, and control the temperature at 25±5°C. After the dropwise addition, slowly raise the temperature to 35°C and keep it warm for 3 hours. The reaction of diphenylphosphorus chloride is complete by gas phase monitoring, and the residual benzyl alcohol is less than 0.5%. After the reaction was completed, the insoluble salt was filtered out.
[0038] The temperature of the filtrate was raised to 110°C, and 190 g of 2,4,6-trimethylbenzoyl chloride was slowly added dropwise, and the reaction was kept for 4 hours after dropping. After the reaction was completed, the temperature was lowered to cool and crystallize, and the product TPO 295g was obtained by filtration, with a yield of 84.8%. The filtrate was evaporated to remove the solvent under nor...
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