Synthesis method of dichloro tetrafluoroethoxy aniline
A technology of dichlorotetrafluoroethoxyaniline and a synthesis method, which is applied in the field of synthesis of dichlorotetrafluoroethoxyaniline, can solve the problems of prolonging the process route, waste of resources, strong alkalinity, etc., and achieve shortening of the process route, Effect of reducing waste water discharge and mild reaction
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Embodiment 1
[0024] First add 7 kg of solvent into the 10-liter reaction kettle through the hand hole, then add 2 kg of 3,5-dichloro-p-aminophenol into the reaction kettle, and finally add 220 grams of catalyst, and tighten the hand hole. Vacuumize, replace with nitrogen twice, and then evacuate to -0.09MPa. Start the hot water system, pass the hot water into the jacket of the addition kettle and circulate it, pass tetrafluoroethylene into the addition kettle, and control the pressure in the kettle to 0.15-0.2MPa. Sampling and analysis after 30 minutes, sampling and analysis once every 30 minutes, until the aminophenol reaction is complete, stop passing tetrafluoroethylene, stop passing hot water, and keep warm to continue the reaction for 30-60 minutes. Out of barrels.
[0025] The catalyst is a mixture of potassium carbonate and potassium bicarbonate with a weight ratio of 1:1; the solvent is mainly toluene, and DMSO, an aprotic solvent accounting for 2% of the total weight of the solve...
Embodiment 2
[0035] First add 6.6 kg of solvent into the 10-liter reaction kettle through the hand hole, then add 1.8 kg of 3,5-dichloro-p-aminophenol into the reaction kettle, and finally add 210 grams of catalyst, and tighten the hand hole. Vacuumize, replace with nitrogen twice, and then evacuate to -0.09MPa. Start the hot water system, pass the hot water into the jacket of the addition kettle and circulate it, pass tetrafluoroethylene into the addition kettle, and control the pressure in the kettle to 0.15-0.2MPa. Sampling and analysis after 30 minutes, sampling and analysis once every 30 minutes, until the aminophenol reaction is complete, stop passing tetrafluoroethylene, stop passing hot water, and keep warm to continue the reaction for 30-60 minutes. Out of barrels.
[0036] The catalyst is a mixture of potassium carbonate and potassium bicarbonate with a weight ratio of 1:3; the solvent is mainly toluene, and 3% of the total weight of the solvent is added with an aprotic solvent ...
Embodiment 3
[0040]First put 5.6 kg of solvent into the 10-liter reaction kettle through the hand hole, then add 1.5 kg of 3,5-dichloro-p-aminophenol into the reaction kettle, and finally add 200 grams of catalyst, and tighten the hand hole. Vacuumize, replace with nitrogen twice, and then evacuate to -0.09MPa. Start the hot water system, pass the hot water into the jacket of the addition kettle and circulate it, pass tetrafluoroethylene into the addition kettle, and control the pressure in the kettle to 0.15-0.2MPa. Sampling and analysis after 30 minutes, sampling and analysis once every 30 minutes, until the aminophenol reaction is complete, stop passing tetrafluoroethylene, stop passing hot water, and keep warm to continue the reaction for 30-60 minutes. Out of barrels.
[0041] The catalyst is a mixture of potassium carbonate and potassium bicarbonate with a weight ratio of 3:1; the solvent is mainly toluene, and DMSO, an aprotic solvent accounting for 2% of the total weight of the so...
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