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Continuous synthesis of glyphosate by dimethyl ester

A technology of dimethyl ester and glyphosate, which is applied in the field of continuous production of glyphosate by dimethyl ester method, can solve the problems of lack of coherence in production, small capacity of a single device, unreasonable energy utilization, etc., and achieves continuous hydrolysis. The effect of reducing the difficulty of recycling and effectively utilizing thermal energy

Active Publication Date: 2009-12-09
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, our country basically adopts the kettle-type intermittent dimethyl ester method with stirring, which has a low degree of automation, and the capacity of a single set of equipment is small, the reaction time is long, the production before and after the lack of continuity, and the production is easily affected by human factors and sometimes has Unstable phenomenon occurs, and the production efficiency is low, and the energy utilization is unreasonable

Method used

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  • Continuous synthesis of glyphosate by dimethyl ester
  • Continuous synthesis of glyphosate by dimethyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The mol ratio of synthetic liquid (in terms of glycine) and hydrochloric acid is the acidified synthetic liquid of 1: 3.1, enters the hydrolysis reaction zone with the feed rate of 1.28 tons / h, and the hydrolysis reactor adopts the combination reactor of one tower two stills, will acidify The synthetic liquid is fed continuously from the top of the tower, and the temperature in the tower is controlled at 90-100°C for preliminary hydrolysis. At the same time, the solvent methanol comes out from the top of the tower, and the generated hydrolyzate, unreacted synthetic liquid and intermediate reaction mixture enter continuously from the bottom of the tower. The first-stage tank-type hydrolysis reactor conducts continuous hydrolysis, and the temperature is controlled at 100-110°C, and then continues to enter the second-stage tank-type reactor for hydrolysis, and the temperature is controlled at 124-128°C, and the material is continuously discharged to neutralize and crystalliz...

Embodiment 2

[0051] The mol ratio of synthetic liquid (in terms of glycine) and hydrochloric acid is the acidified synthetic liquid of 1: 3.4, enters the hydrolysis reaction zone with the feed rate of 1.28 tons / h, and the hydrolysis reactor adopts the combined reactor of one tower two stills, will acidify The synthetic liquid is fed continuously from the middle of the tower, and the temperature in the tower is controlled at 90-100°C for preliminary hydrolysis. At the same time, the solvent methanol comes out from the top of the tower, and the generated hydrolyzate, unreacted synthetic liquid and intermediate reaction mixture enter continuously from the bottom of the tower. The first-stage tank-type hydrolysis reactor conducts continuous hydrolysis, and the temperature is controlled at 100-110°C, and then continues to enter the second-stage tank-type reactor for hydrolysis, and the temperature is controlled at 124-128°C, and the material is continuously discharged to neutralize and crystalliz...

Embodiment 3

[0053] The molar ratio of the synthetic solution (in terms of glycine) and hydrochloric acid is pumped into the circulation mixer with a constant flow metering pump in the ratio of 1:3.4, the total flow rate is 1.28 tons / h, and the circulation flow rate is 10 tons / h. After the condenser, enter the hydrolysis combination device (one tower and two kettles) for hydrolysis. The temperature at the top of the tower is controlled at 92°C, the temperature of the first-stage hydrolysis tower is 110°C, and the temperature of the second-stage hydrolysis tower is 120°C. The residence time is 35 minutes, and the hydrolyzate is added with alkali to crystallize for 8 hours to obtain the product glyphosate, and the total yield of glyphosate is 84.5%.

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Abstract

The invention provides a method for the continuous synthesis of glyphosate by the dimethyl ester method, which comprises the steps of acidifying and mixing the synthesis solution prepared from paraformaldehyde, glycine and dimethyl ester with hydrochloric acid and then entering the hydrolysis reaction zone. The reactor maintains a continuous state; the acidified synthetic solution is continuously hydrolyzed in the hydrolysis reaction zone to form glyphosate salt, and the raw glyphosate powder is obtained by continuously discharging and neutralizing crystallization. Among them, the preferred embodiments of the hydrolysis reaction zone include "one tower with two tanks" and "three tanks in series". The invention realizes the continuous hydrolysis of glyphosate, simplifies the process and realizes large-scale production.

Description

technical field [0001] The invention relates to the research field of continuous production of glyphosate by dimethyl ester method. Background technique [0002] Glyphosate is a low-toxicity, high-efficiency, broad-spectrum herbicide. It was first successfully developed by Monsanto Company of the United States in 1974 and has applied for patent protection in many countries around the world. In the mid-to-late 1990s, with the successive expiration of its patent protection in various countries in the world and the widespread planting of glyphosate-resistant transgenic crops, the application of glyphosate has developed rapidly, becoming the largest and fastest-growing pesticide variety. [0003] There are many synthetic methods of glyphosate, but currently only two industrialized process routes are used, namely the IDA process and the alkyl ester process. The alkyl ester process is the process route adopted by most of the production enterprises in our country. Alkyl ester pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 王伟任不凡来虎钦周曙光蔡鹏詹波王林辉李丽娟胡江邵振威佘慧玲吴涛周瑛黄重水
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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