Method for continuously preparing pentafluorophenol by micro-reactor
A microreactor and pentafluorophenol technology are applied in the field of continuous preparation of pentafluorophenol in microreactors, which can solve the problems of inability to meet purity requirements, decrease in yield, increase in by-products of polysubstituted phenols, etc., and achieve convenient product purification and production. The effect of low cost and high reaction yield
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Embodiment 1
[0028] Add potassium hydroxide 52.5g (0.94mol) and water 78.0g to the microreactor lye kettle to form a solution, and add hexafluorobenzene 75.0g (0.40mol) to the microreactor raw material kettle. The working temperature of the microreactor is set at 160°C, the outlet of the microreactor pipeline is controlled by a quantitative pressure control valve, and the working pressure of the microreactor pipeline is set at 0.6Mpa. Potassium hydroxide aqueous solution and hexafluorobenzene are all pumped in by the metering pump according to the volume flow ratio of 2:1, and it takes 5 hours to pump them all in, and the residence time in the microreactor is 3 minutes. Collect the system liquid at the outlet of the heat exchanger of the microreactor, add 146g of 30% hydrochloric acid, and steam distill to obtain 103g of oil layer. The oil layer detection system consists of: water 30%, pentafluorophenol 70%, rectification and dehydration to obtain 72.0g of pentafluorophenol. The yield was ...
Embodiment 2
[0030] Add potassium hydroxide 271g (4.83mol) and water 321g in the microreactor lye kettle to form a solution, and add hexafluorobenzene 300g (1.61mol) in the microreactor raw material kettle. The working temperature of the microreactor is set at 140°C, the outlet of the microreactor pipeline is controlled by a quantitative pressure control valve, and the working pressure of the microreactor pipeline is set at 0.8Mpa. Potassium hydroxide aqueous solution and hexafluorobenzene are all pumped in by the metering pump according to the volume flow ratio of 2.2:1, and it takes 4 hours to pump them all in, and the residence time in the microreactor is 5 minutes. Collect the system liquid at the outlet of the microreactor heat exchanger, add 516g of 30% hydrochloric acid, and steam distill to obtain 405g of oil layer. The oil layer detection system consists of: water 30%, pentafluorophenol 70%. Rectification and dehydration gave 284g of pentafluorophenol. The yield was 95.7%, and th...
Embodiment 3
[0032] Add potassium hydroxide 95g (1.69mol), sodium hydroxide 68g (1.70mol) and water 320g to the microreactor lye still to form a solution, and add hexafluorobenzene 300g (1.61mol) to the microreactor raw material still. The working temperature of the microreactor is set at 150°C, the outlet of the microreactor pipeline is controlled by a quantitative pressure control valve, and the working pressure of the microreactor pipeline is set at 0.8Mpa. Potassium hydroxide aqueous solution and hexafluorobenzene are all pumped in by the metering pump according to the volume flow ratio of 2:1, and it takes 4 hours to pump them all in, and the residence time in the microreactor is 5 minutes. Collect the system liquid at the outlet of the microreactor heat exchanger, add 516g of 30% hydrochloric acid, and steam distill to obtain 411g of oil layer. The composition of the oil layer detection system is: water 30%, pentafluorophenol 70%. Rectification and dehydration gave 288g of pentafluor...
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