Continuous production method of multi-kettle serial triazine herbicide

Abstract

The invention relates to a continuous production method of a multi-kettle serial triazine herbicide. A metered cyanuric chloride solution is pre-cooled and mixed with alkylamine R1 in a mixer to entera first-stage reaction kettle, continuous discharging is conducted, after a heat exchanger is passed, the cyanuric chloride solution is neutralized with alkali in the mixer and enters a first-stage neutralization kettle, after a reaction is completed, the cyanuric chloride solution passes through a continuous water separator and the heat exchanger and is mixed with alkylamine R2 in the mixer to enter a second-stage reaction kettle, the continuous discharging is conducted, after the cyanuric chloride solution passes through the heat exchanger, the cyanuric chloride solution is mixed with the alkali in the mixer to enter a second-stage neutralization kettle, after the neutralization, a aqueous phase is separated by a continuous layerer, a solvent is removed, and drying is conducted to obtain a triazine product. The production method has the advantages of high productivity, good production stability, high efficiency, high product quality and the like, is particularly suitable for technical transformation of existing production enterprises, has a low transformation cost, basically does not add novel reaction equipment, and is easily mastered by existing enterprises.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for continuously producing triazine herbicides in series with multiple reactors. Background technique [0002] Triazine herbicides are one of the traditional herbicides introduced in the 1950s, and their herbicidal activity was discovered in 1952 by the Swiss company Geigy. It acts by inhibiting photosynthesis of plants by targeting D1 protein through photosynthetic system II (PSII). After years of experimentation, a series of triazine herbicides have been developed. Among them, zinc herbicides are used in large amounts. Two chlorine atoms in trimeric chlorine are replaced by two alkylamine groups to form zinc herbicides. Usually, these alkylamine groups include ethylamine, isopropylamine, cyclic Propylamino, tert-butylamino, etc. Representative zinc herbicides include atrazine (atrazine), simazine, terbuthine, permethazine, and the like. This kind of he...

AI Technical Summary

Problems solved by technology

The inventors have found that the problems of the existing technology are: one, the reaction temperature is not easy to control, because the heat transfer area of ​​the jacket is relatively small and the heat of reaction is relatively large, so the reaction drop rate cannot be fast, otherwise the side reactions will be aggravated; the other is the low production capacity , due to the limitation of the drop rate, it takes about 18-24 hours for the sequencing batch reaction to complete the whole process; the third is that there are many side reactions, because the temperature cannot be accurately controlled, operating factors, local overconcentration and other factors cause many side reactions, and the product purity Poor; Fourth, there are many intermittent production equipment, complicated operation, and low labor efficiency. It is inevitable that there will be quality fluctuations caused by manual operation errors

[0004] The process of using microreactors to synthesize triazine herbicides reported in China, due to the low load of a single set of microreactors, will cause a large investment and low cost performance for this 10,000-ton product

[0005] In CN201710663765.7, a mixer and a tubular reactor are used to synthesize the triazine herbicide atrazine. Although it can be produced continuously, there is no back-mixing process in the reaction process. The best effect may not be achieved; in addition, the water phase of the first stage of reaction is not separated between the first stage of reaction and the second stage of reaction in the whole process, and the impurities and unreacted materials in it are easy to be carried into the next stage, resulting in the increase of impurities

Images