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Method for hydrolyzing glyphosate acid

A technology of glyphosate acid and hydrolysis reaction, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as inaccurate ingredients, affecting production efficiency and output, damage, etc.

Active Publication Date: 2011-09-14
SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is necessary to cool down the high-temperature reaction kettle before each new feed, which not only causes a great waste of energy, but also causes a large amount of steam valve water to be effectively utilized due to the poor quality of the cooled circulating water, and is released in vain.
At the same time, the reaction time is greatly prolonged, and the reactor is also vulnerable to damage during the frequent hot and cold changes. If the two materials are directly mixed into the reactor, it is often prone to inaccurate ingredients or even wrong feeding.
On the other hand, although the injected two hydrolyzed materials are fed according to the specified load of the reactor, since the materials and solvents in the reaction system are all volatile components, as the temperature rises and the reaction proceeds, the materials in the kettle The amount will gradually decrease, so that the upper empty space in the reactor will continue to increase, resulting in an increase in the ineffective heating ratio of the heating jacket to these empty spaces, resulting in the phenomenon of upper heating and lower cooling of the reactor
According to the current feeding method, this problem is common but cannot be solved
This is not only another factor that increases energy waste, but also reduces reactor utilization, affecting production efficiency and output

Method used

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  • Method for hydrolyzing glyphosate acid
  • Method for hydrolyzing glyphosate acid
  • Method for hydrolyzing glyphosate acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 1000 grams of the mixed acid synthesis solution formed by mixing the synthesis solution of the precursor compound of glyphosate acid and 30% hydrochloric acid in a molar ratio of 1:3.2 into a 1000ml three-necked bottle, heat up to 80°C, part of the organic solvent and After the water is removed, add 400 grams of the mixed acid synthesis solution dropwise, and the time for adding is 10-20 minutes. After dropping, continue to heat up to 120°C to complete the hydrolysis reaction. The solid glyphosate content and the glyphosate content in the mother liquor were detected, and the total yield calculated as glycine was 81.5%.

Embodiment 2

[0017] 1000 grams of the mixed acid synthesis solution formed by mixing the synthesis solution of the precursor compound of glyphosate acid with 32% hydrochloric acid in a molar ratio of 1:3.3 is added to a 1000ml three-necked flask; the temperature is raised to 90°C, and part of the organic solvent After detaching from water, add 500 grams of the same mixed acid synthetic solution dropwise, and the dropwise addition time is 10-20 minutes. After dropping, continue to heat up to 120°C to complete the hydrolysis reaction. The solid glyphosate content and the glyphosate content in the mother liquor were detected, and the total yield calculated as glycine was 81.2%.

Embodiment 3

[0019] 6,200 kilograms of the mixed acid synthetic solution formed by mixing the synthetic solution of the precursor compound of glyphosate acid with 30% hydrochloric acid in a molar ratio of 1:3.2 is injected into the 6300KL hydrolysis kettle, and 2,200 kilograms are injected into the elevated tank. The temperature of the mixed acid synthetic solution in the hydrolysis tank is raised to 80°C, and after part of the organic solvent and water are released, the mixed acid synthetic solution in the high level tank is added dropwise to the hydrolysis tank, the dropping time is 1-2 hours, and the dropping temperature does not exceed 80°C . Continue to heat up the material in the kettle to 120°C to complete the hydrolysis reaction. The solid glyphosate content and the glyphosate content in the mother liquor were detected, and the total yield calculated as glycine was 80.8%.

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Abstract

The invention relates to a method for hydrolyzing glyphosate. It comprises following steps: mixing prosoma of glyphosate with chlorhydric acid solution, feeding the mixture according to required amount into autoclave, heating for hydrolysis; or feeding the mixture, heating not more than 100 Deg. C, and dropping said mixture into autoclave until meets the required amount, heating again for hydrolysis. The method is characterized by shortened hydrolysis time, increased utilizing rate of autoclave and heat, increased yeild and decreased energy consumption. It aslo solves the damage to autoclave caused by stop- and- go heating in traditional method.

Description

technical field [0001] The invention relates to a hydrolysis reaction operation method in the production process of glyphosate. Background technique [0002] Glyphosate is a widely used herbicide. Since its commercialization in the mid-1970s, its range of applications has continued to expand due to its excellent herbicidal performance. [0003] The industrialized production of glyphosate acid is mainly by two kinds of methods at present: a kind of is the IDA method generally adopted by companies such as U.S. Monsanto, uses diethanolamine as starting raw material production; Another kind of method is as disclosed in document DEOLSNO.P2942898. The alkyl ester method is to heat and dissolve paraformaldehyde or formaldehyde in a methanol solvent containing triethylamine, and then add glycine and dimethyl phosphite (or trimethyl phosphite) for condensation reaction to generate intermediate The triethylamine salt (II) of the body compound dimethyl glyphosate, and then hydrochlor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 刘德亮
Owner SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD