Industrial preparation process for 3,4-difluorobenzonitrile
A technology of difluorobenzonitrile and preparation process, applied in 3 fields, can solve the problems of inability to meet industrial production needs, strict reaction requirements, complex preparation process, etc., and achieves the possibility of reducing fluorine loss and coking, short reaction process flow, and improved performance. Effect of Reaction Yield
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[0030] Example one
[0031] 1. Add 456Kg of solvent and 150L of toluene from the solvent DMI high tank and toluene high tank to the 2000L fluorination kettle with distillation tower;
[0032] 2. Turn on the fluorination kettle and stir, open the feeding port and put 139.2Kg of anhydrous potassium fluoride and 20Kg of the catalyst into the fluorination kettle, close the feeding port, and check whether the seal is intact;
[0033] 3. Turn on the vacuum system to make the gauge pressure of the fluorination kettle -0.1Mpa. After the vacuum is stable, turn on the cooling water system of the top condenser of the fluorination kettle, start the hot oil pump, and slowly increase the temperature; when the temperature in the kettle rises to 110°C When the rectification tower is in a state of full reflux, the discharge flow rate is controlled at 55kg / h, the discharging is finished, and the detoluene of the distillate is clear, and the discharge valve is closed to make the tower in a state of fu...
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[0039] Example two
[0040] 1. Add 342Kg of solvent and 150L of toluene from the solvent DMI high tank and toluene high tank to the 2000L fluorination kettle with distillation tower;
[0041] 2. Turn on the fluorination kettle and stir, open the feeding port and put 127.6Kg of anhydrous potassium fluoride and 12.5Kg of catalyst into the fluorination kettle, close the feeding port, and check whether the seal is intact;
[0042] 3. Turn on the vacuum system to make the gauge pressure of the fluorination kettle -0.1Mpa. After the vacuum is stable, turn on the cooling water system of the top condenser of the fluorination kettle, start the hot oil pump, and slowly increase the temperature; when the temperature in the kettle rises to 110°C When the rectification tower is in a state of full reflux, the discharge flow rate is controlled at 55kg / h, the discharging is finished, and the detoluene of the distillate is clear, and the discharge valve is closed to make the tower in a state of full...
Example Embodiment
[0048] Example three
[0049] 1. Add 912Kg of solvent and 150L of toluene from the solvent DMI high-position tank and toluene high-position tank to the 2000L fluorination kettle with distillation tower;
[0050] 2. Turn on the fluorination kettle and stir, open the feeding port and put 232Kg of anhydrous potassium fluoride and 25Kg of catalyst into the fluorination kettle, close the feeding port, and check whether the seal is intact;
[0051] 3. Turn on the vacuum system to make the gauge pressure of the fluorination kettle -0.1Mpa. After the vacuum is stable, turn on the cooling water system of the top condenser of the fluorination kettle, start the hot oil pump, and slowly increase the temperature; when the temperature in the kettle rises to 110°C When the rectification tower is in a state of full reflux, the discharge flow rate is controlled at 55kg / h, the discharging is finished, and the detoluene of the distillate is clear, and the discharge valve is closed to make the tower i...
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