Novel process for producing chlopyrifos from pyridone by using aqueous phase method
A technology of pyridone and chlorpyrifos, applied in the field of preparation of chlorpyrifos, can solve the problems of no increase in yield, large amount of solvent used, serious loss, etc.
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Embodiment 1
[0014] Add 200g of newly distilled trichloroacetyl chloride, 87g of acrylonitrile, 566g of solvent, and 0.66g of cuprous chloride into a 1000ml flask, react at 90-120°C, and remove the produced hydrogen chloride by operating under reflux Gas, generating 2,2,4-trichloro-4-cyanobutyryl chloride dilute solution.
[0015] The 2,2,4-trichloro-4-cyanobutyryl chloride mixed solution is subjected to vacuum distillation, unreacted raw materials (mainly acrylonitrile, trichloroacetyl chloride and part of the solvent) are recovered, the catalyst is filtered out, and the filtrate is 2,2,4-Trichloro-4-cyanobutyryl chloride concentrated solution.
[0016] Add an appropriate amount of solvent to the concentrated solution of 2,2,4-trichloro-4-cyanobutyryl chloride, react under the action of a gauge pressure of 30-150KPa, a temperature of 30-100°C and a catalyst to form a pyridone solution. The pyridone solution is cooled to crystallize and separated to obtain dry pyridone.
[0017] In a 500...
Embodiment 2
[0019] Add 990kg of newly distilled trichloroacetyl chloride, 435kg of acrylonitrile, 2830g of solvent, and 3.3kg of cuprous chloride into a 5000L reactor, react at 90-120°C, and remove the produced Hydrogen chloride gas produces a dilute solution of 2,2,4-trichloro-4-cyanobutyryl chloride.
[0020] The 2,2,4-trichloro-4-cyanobutyryl chloride mixed solution is subjected to vacuum distillation, unreacted raw materials (mainly acrylonitrile, trichloroacetyl chloride and part of the solvent) are recovered, the catalyst is filtered out, and the filtrate is 2,2,4-Trichloro-4-cyanobutyryl chloride concentrated solution.
[0021] Add an appropriate amount of solvent to the concentrated solution of 2,2,4-trichloro-4-cyanobutyryl chloride, react under the action of a gauge pressure of 30-150KPa, a temperature of 30-100°C and a catalyst to form a pyridone solution. The pyridone solution is cooled to crystallize and separated to obtain dry pyridone.
[0022] Add 3000kg of water, 784kg ...
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