Synthetic method of chlorpyrifos

Abstract

The invention discloses a synthetic method of chlorpyrifos, which comprises the following steps of: enabling trichloro-acetic chloride, acrylonitrile, o-dichlorobenzene and a CuCl catalyst to react to obtain a crude product; adding the crude product into a reaction kettle containing water, a catalyst and alkali, raising the temperature and backwardly flowing for 3-4 hours, standing and separating out a solvent, cooling and crystallizing a water phase, centrifuging to obtain a trichloropyridine alcohol potassium tide product and drying to obtain a trichloropyridine alcohol potassium finished product; and adding the trichloropyridine alcohol potassium finished product into the reaction kettle, adding water, boric acid and a catalyst, agitating, raising the temperature to 75-80 DEG C, maintaining the pH to be equal to 9-10, dripping ethyl chloride, maintaining for 3-5 hours, standing and phase separation, separating out an oil phase, adding the oil phase into absolute ethyl alcohol for recrystallization, filtering and air-drying to obtain a chlorpyrifos finished product. The synthetic method has the advantages of easiness in operation, high yield and reduced environment pollution and provides guarantee for sustainable development.

Description

technical field [0001] The invention relates to a synthesis method of chlorpyrifos. Background technique [0002] At present, the intermediate sodium clopyridinate is mostly used in the synthesis of chlorpyrifos in China. Sodium clopyridinate has the problems of many process control points, high toxicity of raw materials, poor product quality and low yield in the synthesis process. [0003] The process of synthesizing sodium triclopyridinate is as follows: put trichloroacetyl chloride, acrylonitrile, nitrobenzene, and catalyst cuprous chloride into the reactor, heat up, stir at 120-140°C for 8-16h, and remove low boiling Throw in dry HCl gas, stir for 3-10h, cool down, add NaOH solution, stir at room temperature for 5-12 hours, and centrifuge to obtain sodium clopyridinate. [0004] The synthesis of sodium clopyridinate uses nitrobenzene as a solvent, which is highly toxic and has great potential safety hazards in actual production; the finished product sodium clopyridinat...

AI Technical Summary

Problems solved by technology

Sodium clopyridinate has many process control points in the synthesis process, the toxicity of raw materials is large, the product quality is poor, and the problem of low yield

In practice, this kind of high-salt wastewater cannot be discharged directly because the COD exceeds the standard, so this wastewater also has treatment problems