CN105622666A - Glyphosate synthesis technology - Google Patents

Abstract

The invention discloses a glyphosate synthesis technology. The glyphosate synthesis technology comprises a depolymerization reaction process, an addition reaction process, a condensation reaction process, a hydrolysis reaction process and a crystallization process. The glyphosate synthesis technology solves the problem that the glyphosate synthesis condensation reaction cannot occur under the waterless conditions. In the addition reaction and condensation reaction processes, the reaction liquid is dehydrated through a dehydration device so that reaction product moisture is reduced, dimethyl phosphite consumption is reduced, a reaction yield is improved, raw materials are saved and a cost is reduced.

Description

The synthesis technique of glyphosate

Technical field

The invention belongs to technical field of chemical synthesis, be specifically related to the synthesis technique of a kind of glyphosate.

Background technology

Glyphosate reaches also known as glyphosate, agriculture, careless dry phosphine, the sweet acid of phosphine. Sterling is non-volatile white solid, and proportion is 0.5, is approximately in about 230 DEG C fusings, and with decomposing. When 25 DEG C, the dissolubility in water is 1.2%, and insoluble in common organic solvents, its isopropyl amine salt is dissolved completely in water. Glyphosate is non-combustible, do not explode, and storage at normal temperature is stable, and medium carbon steel, tin plate (tinplate) are had corrosiveness. Glyphosate is usually used in preventing and kill off the weeds in apple orchard, vineyard and tea place. In current glyphosate synthesis process approach, technological process is not easy to implement, and the glyphosate finished product purity of generation is low, and reactant conversion per pass is low, and manufacturing process is complicated, and production efficiency is low and cost high, is not suitable for large-scale production.

Summary of the invention

For the above-mentioned technical problem overcoming prior art to exist, it is an object of the invention to, it is provided that the synthesis technique of a kind of glyphosate, the present invention not only manufacturing process is simple, improve work efficiency, and the glyphosate products purity generated is greatly, is suitable for industrialized production.

The synthesis technique of glyphosate provided by the invention, comprises the following steps:

(1) depolymerization reaction: methanol, triethylamine and paraformaldehyde are carried out depolymerization reaction 55-70 minute at 35-40 DEG C, obtains depolymerization liquid;

(2) additive reaction: after being cooled to 32-52 DEG C, adds glycine in depolymerization liquid and carries out additive reaction, react 15-25 minute and clarify to additive reaction liquid at 42-44 DEG C, solids disappeared;

(3) dehydration cycle processes the regeneration with dehydrant: while the additive reaction liquid of clarification is proceeded additive reaction, processes with 3A or 4A molecular sieve dehydration cycle, obtains dehydration addition liquid; The nitrogen of 100-350 DEG C of 3A or 4A molecular sieve carries out Regeneration Treatment, the condensed recovery methanol of nitrogen after process and triethylamine, tail gas emptying process;

(4) condensation reaction: add dimethylphosphite in dehydration addition liquid, condensation reaction is carried out at 52-54 DEG C, condensation reaction solution is carried out the dehydration cycle described in step (3) simultaneously and processes the regeneration with dehydrant by reaction, react 50-100 minute, condensation reaction completes, and obtains dehydrating condensation liquid;

(5) hydrolysis; Adding mass fraction content after dehydrating condensation liquid is cooled to less than 25 DEG C is the hydrochloric acid of 28-32%;

(6) crystallization: temperature is down to less than 30 DEG C, spontaneous nucleation at least 4 hours, filters, washing, dry obtains glyphosate.

The synthesis technique of glyphosate provided by the invention, it has the beneficial effects that, overcoming prior art, to prepare operation in glyphosate technical process more, and the problem that workload is big improves work efficiency; Improve the conversion per pass of reactant and the productivity of product.

Detailed description of the invention

Below in conjunction with an embodiment, the synthesis technique of glyphosate provided by the invention is described in detail.

Embodiment

The synthesis technique of the glyphosate of the present embodiment, comprises the following steps:

(1) depolymerization reaction: methanol, triethylamine and paraformaldehyde are carried out depolymerization reaction 55 minutes at 40 DEG C, obtains depolymerization liquid;

(2) additive reaction: after being cooled to 52 DEG C, adds glycine in depolymerization liquid and carries out additive reaction, react 25 minutes and clarify to additive reaction liquid at 42 DEG C, solids disappeared;

(3) dehydration cycle processes the regeneration with dehydrant: while the additive reaction liquid of clarification is proceeded additive reaction, processes with 3A or 4A molecular sieve dehydration cycle, obtains dehydration addition liquid; 3A or 4A molecular sieve carries out Regeneration Treatment with the nitrogen of 250 DEG C, the condensed recovery methanol of nitrogen after process and triethylamine, tail gas emptying process;

(4) condensation reaction: add dimethylphosphite in dehydration addition liquid, carrying out condensation reaction at 54 DEG C, condensation reaction solution is carried out the dehydration cycle described in step (3) simultaneously and processes the regeneration with dehydrant by reaction, reacts 100 minutes, condensation reaction completes, and obtains dehydrating condensation liquid;

(5) hydrolysis; Be cooled to by dehydrating condensation liquid after 20 DEG C adding mass fraction content is the hydrochloric acid of 32%;

(6) crystallization: temperature is down to 20 DEG C, spontaneous nucleation 4 hours, filters, washing, dry obtains glyphosate.

The synthesis technique of glyphosate, it is not necessary to loaded down with trivial details post-reaction treatment, operation simple possible, and also environmentally friendly pollution-free, technological process is easy to implement, it is achieved that the industrialized production of product.

Claims (1)

1. the synthesis technique of a glyphosate, it is characterised in that: said method comprising the steps of:

(1) depolymerization reaction: methanol, triethylamine and paraformaldehyde are carried out depolymerization reaction 55-70 minute at 35-40 DEG C, obtains depolymerization liquid;

(2) additive reaction: after being cooled to 32-52 DEG C, adds glycine in depolymerization liquid and carries out additive reaction, react 15-25 minute and clarify to additive reaction liquid at 42-44 DEG C, solids disappeared;

(3) dehydration cycle processes the regeneration with dehydrant: while the additive reaction liquid of clarification is proceeded additive reaction, processes with 3A or 4A molecular sieve dehydration cycle, obtains dehydration addition liquid; The nitrogen of 100-350 DEG C of 3A or 4A molecular sieve carries out Regeneration Treatment, the condensed recovery methanol of nitrogen after process and triethylamine, tail gas emptying process;

(4) condensation reaction: add dimethylphosphite in dehydration addition liquid, condensation reaction is carried out at 52-54 DEG C, condensation reaction solution is carried out the dehydration cycle described in step (3) simultaneously and processes the regeneration with dehydrant by reaction, react 50-100 minute, condensation reaction completes, and obtains dehydrating condensation liquid;

(5) hydrolysis; Adding mass fraction content after dehydrating condensation liquid is cooled to less than 25 DEG C is the hydrochloric acid of 28-32%;

(6) crystallization: temperature is down to less than 30 DEG C, spontaneous nucleation at least 4 hours, filters, washing, dry obtains glyphosate.