Phenyl Dichlorophosphate CAS 770-12-7

Synthesis process
In a 500mL three-neck flask, add 359g (2.3mol) of phosphorus oxychloride, heat in an oil bath, and the liquid temperature rises to 80-90°C. During this process, the system emits HCl white smoke, and the temperature is maintained until no white smoke is emitted. When the equipment is dried, 7.5g (0.068mol) of quaternary ammonium salt catalyst is added, and the liquid phase temperature is kept at 80-90℃. Phenol should be heated and dissolved in advance. After adding 150g (1.56mol) of dissolved phenol into the dropping funnel, add phenol dropwise within the range of 80-90℃ in the three-necked flask. Not too high, otherwise side reactions will occur. After dropping phenol, keep the reaction at 80-92 °C until no white smoke is released from the tail gas, and then heat up to 92-120 °C. The reaction end point is when there is little white smoke in the tail gas; the tail gas should be introduced into the water pump absorption system, and the reaction time A total of about 4h.

Distillation cutting process
(1) Atmospheric pressure distillation Excess phosphorus oxychloride is heated and evaporated under normal pressure. When the temperature of the gas phase rises to 120 °C, the atmospheric distillation is stopped when no fraction is evaporated.

(2) Distillation conditions before vacuum distillation: gas phase temperature: 140°C, liquid phase temperature: 145-150°C, vacuum degree: 0-93310Pa Phase temperature: 146-150°C, vacuum degree: 9464.3Pa, the collected product is high-content phenyl dichloride phosphate, about 250g in weight, ≥96% in content, and about 73% in yield.