A kind of process method of synthesizing paraquat by cyanamide method
A process method, paraquat technology, applied in the field of pesticide synthesis, can solve the problems of affecting dimer synthesis, increasing production cost, affecting the yield of paraquat, etc., to achieve the effect of increasing yield, reducing production cost, and avoiding thermal decomposition
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Embodiment 1
[0019] A process for synthesizing paraquat by cyanamide method, the concrete steps are:
[0020] (1) Synthesis of N-picoline chloride (MPC), add 4500kg pyridine and 1700kg methanol respectively into the high-pressure reaction kettle, heat up to 60°C, and then use a rotameter to control the slow introduction of methyl chloride gas, and then The speed is 30m 3 / h, when reacting until there is no pyridine stench, it is regarded as the end of the reaction, and the reaction product is pumped into the drying kettle in batches by vacuum, then the methanol is steamed out, recovered and recycled after condensation and reflux, and 7000kg MPC is obtained through drying;
[0021] (2) Synthesis of the intermediate 1,1'-dimethyl-4,4'-dihydrobipyridine, adding the MPC obtained in (1) into the autoclave, and then adding 48kg of sodium cyanide as a catalyst, Then vacuumize, then add liquid ammonia to the autoclave, stir to make it react, control the temperature to 30°C, stir at 40r / min, and t...
Embodiment 2
[0024] A process for synthesizing paraquat by cyanamide method, the concrete steps are:
[0025] (1) Synthesis of N-picoline chloride (MPC), add 4500kg pyridine and 1700kg methanol respectively into the high-pressure reaction kettle, heat up to 65°C, and then use a rotameter to control the slow introduction of methyl chloride gas, and then The speed is 70m 3 / h, when reacting until there is no pyridine stench, it is regarded as the end of the reaction, and the reaction product is pumped into the drying kettle in batches by vacuum, then the methanol is evaporated, recovered and recycled after condensation and reflux, and 7350kg MPC is obtained through drying;
[0026] (2) Synthesis of the intermediate 1,1'-dimethyl-4,4'-dihydrobipyridine, adding the MPC obtained in (1) into the autoclave, and then adding 50kg of sodium cyanide as a catalyst, Then vacuumize, then add liquid ammonia to the autoclave, stir to make it react, control the temperature to 45°C, stir at 50r / min, and th...
Embodiment 3
[0029] A process for synthesizing paraquat by cyanamide method, the concrete steps are:
[0030] (1) Synthesis of N-picoline chloride (MPC), add 4500kg of pyridine and 1700kg of methanol into the high-pressure reaction kettle, heat up to 70°C, and then use a rotameter to control the slow introduction of methyl chloride gas. The speed is 100m 3 / h, when reacting until there is no pyridine stench, it is regarded as the end of the reaction, and the reaction product is sucked into the drying kettle in batches by vacuum, then the methanol is steamed out, recovered and recycled after condensation and reflux, and 6997kg MPC is obtained through drying;
[0031](2) Synthesis of the intermediate 1,1'-dimethyl-4,4'-dihydrobipyridine, adding the MPC obtained in (1) into the autoclave, and then adding 47kg of sodium cyanide as a catalyst, Then vacuumize, then add liquid ammonia to the autoclave, stir to make it react, control the temperature at 55°C, stir at 60r / min, and the reaction time...
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