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 problems such as unreasonable energy utilization, lack of continuity in production, and small capacity of a single set of equipment, and achieve leakage points and Reduced contact points with the outside world, strong airtightness, and reduced equipment utilization

Active Publication Date: 2007-04-04
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

Continuous synthesis of glyphosate by dimethyl ester is carried out by taking paraformaldehyde, amino acetic acid and dimethyl ester as raw materials to obtain synthetic liquid, acidizing it with hydrochloric acid, mixing, entering into hydrolytic reactive zone, reacting in hydrolytic reactor continuously, acidizing synthetic liquid, hydrolyzing in hydrolytic reactive zone continuously, forming into glyphosate salt, batching continuously and neutralization crystallizing to obtain the final product. It realizes continuous hydrolysis and simplifies process and can be used in 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 Applications(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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