Production process for catalytic synthesis of chlorfenapyr with mixed catalyst

Abstract

The invention provides a production process for catalytic synthesis of chlorfenapyr with a mixed catalyst. The production process comprises steps of material addition, chloric ether dropping, heat-preservation reactions and solid-liquid separation. 4-bromine and chloric ether are adopted as main raw materials, acetonitrile is adopted as a reaction solvent, potassium carbonate and solid caustic soda are adopted as a mixed catalyst for catalytic synthesis of chlorfenapyr, after reactions are completed, solid-liquid separation is carried out, a reaction solvent is evaporated off, a refining solvent is further used to carry out refining, and thus the chlorfenapyr is prepared. A small dosage of the mixed catalyst is used in the production process, the amount of the catalyst is reduced by 60% when being compared with that of a conventional process, a small amount of solid wastes is generated, the solid wastes are reduced by 55% when being compared with those of a conventional process, the cost is reduced by 15-20% when being compared with that of conventional process, the solvent can be circulated and mechanically applied, pollution and waste can be reduced, and very good economical efficiency and environment-friendliness can be achieved.

Description

technical field [0001] The invention relates to a method for preparing an insecticidal and acaricidal agent of arylpyrrole compounds with a novel structure, in particular to a production process for synthesizing chlorfenapyr catalyzed by a mixed catalyst, and belongs to the technical field of chemical synthesis. Background technique [0002] Chlorfenapyr, the English name is Chlorfenapyr, the trade name is Chujin Suspending Agent, and the Chinese common name is Chlorfenapyr. It is a new type of heterocyclic insecticide, acaricide and nematicide successfully developed by American Cyanamid Company. With the promulgation of the national highly toxic pesticide substitution policy and the improvement of people's awareness of environmental protection, as a representative of the recommended pesticide varieties for pest control of pollution-free agricultural products, the application of low-toxicity and high-efficiency chlorfenapyr is becoming more and more extensive. Chlorfenapyr ...

AI Technical Summary

Problems solved by technology

[0005] CN102617439A discloses a preparation method of chlorfenapyr, using 4-bromo and chloromethyl ethyl ether as raw materials, alkali metal carbonate or organic amine as acid-binding agent, and ester as solvent to prepare chlorfenapyr, which discloses Sodium carbonate and potassium carbonate are acid-binding agents, which have the disadvantage of large solid waste. At the same time, when the reaction temperature drops below 55°C, the reaction time must be extended to 2 hours, and the product yield can reach 91%. At the same time, the catalyst and solvent Consumption is also larger, the mass ratio of catalyst and raw material 4-bromine is 0.39:1, and the mass ratio of solvent and raw material 4-bromine is 5.7:1 (embodiment 2)

[0007] The shortcomings of this patent are: after the reaction is finished and the temperature is lowered, a large amount of water needs to be added, and dilute hydrochloric acid needs to be added to adjust the pH, which wastes a lot of water resources, complicates the operation process, and increases the production cost.

At the same time, the patent discloses that the yield of the crude product of chlorfenapyr is 99%, but after refining, the yield of the finished product is reduced to below 85% (Example 1)

Images