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Synthetic process for glyphosate

A synthesis process, glyphosate technology, applied in the compound of periodic table group 5/15 elements, chemical instruments and methods, organic chemistry, etc., can solve the problem of shortening the reaction time, to improve the purity and efficiency, production cycle The effect of shortening and improving the conversion rate of finished products

Inactive Publication Date: 2017-12-29
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although this production method increases the condensation reaction temperature, shortens the reaction time, and increases the yield of the product, the yield is only partially improved on the existing basis, and the reaction time is only partially shortened.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] After adding methanol, paraformaldehyde and triethylamine in sequence to the condensation kettle, the temperature was raised to 35-50°C, and the reaction was performed for 45-55 minutes. After the material was transparent, the temperature was lowered to 30-40°C; React for 55-68 minutes, after the material is transparent, cool down to 35-40°C; add dimethyl phosphite, heat up to 45-55°C, react for 70-85 minutes, after the material is transparent, cool down to 30-45°C; inject Acidification kettle, add hydrochloric acid, the temperature is controlled below 45 ℃, after adding, stir for 3-8 minutes, carry out temperature increase dealcoholization, deacidification, heat up to 80 ℃ ~ 117 ℃, dealcoholization to 117 ℃, wait for the material to turn yellow and keep warm for 15- 25 minutes; add water, put it into the final kettle, and after discharging, slowly add liquid caustic soda, adjust the pH to 0.6 to 1.0, continue to cool down to 25 to 30 °C for centrifugation, and the centr...

Embodiment 2

[0029] After adding methanol, paraformaldehyde and triethylamine in sequence to the condensation kettle, the temperature is raised to 35-50°C, and the reaction is carried out for 45-55 minutes. After the material is transparent, the temperature is lowered to 30-40°C. 50-55 ℃, heat preservation reaction for 2-3 hours, steam out by-products and excess formaldehyde; add glycine, heat up to 50-60 ℃, react for 55-68 minutes, after the material is transparent, cool down to 35-40 ℃; Dimethyl phosphate, heat up to 45-55 ℃, react for 70-85 minutes, after the material is transparent, cool down to 30-45 ℃; put it into the acidification kettle, add hydrochloric acid, control the temperature below 45 ℃, stir after adding for 3- 8 minutes, carry out temperature increase dealcoholization, deacidification, heat up to 80 ℃ ~ 117 ℃, dealcoholization to 117 ℃, wait for the material to turn yellow and keep warm for 15-25 minutes; add water, put it into the final kettle, after discharging, slowly a...

Embodiment 3

[0033] After adding methanol, paraformaldehyde and triethylamine in sequence to the condensation kettle, the temperature is raised to 35-50°C, and the reaction is carried out for 45-55 minutes. After the material is transparent, the temperature is lowered to 30-40°C. 50-55 ℃, heat preservation reaction for 2-3 hours, steam out by-products and excess formaldehyde; add glycine to the treated solution, heat up to 50-60 ℃, react for 55-68 minutes, after the material is transparent, cool down to 35- 40°C; add dimethyl phosphite, heat up to 45-55°C, react for 70-85 minutes, after the material is transparent, cool down to 30-45°C; put it into the acidification kettle, add hydrochloric acid, control the temperature below 45°C, add After completion, stir for 3-8 minutes, carry out temperature increase dealcoholization, deacidification, heat up to 80 ℃ ~ 117 ℃, dealcoholization to 117 ℃ and keep warm for 15-25 minutes until the material turns yellow; add water for hydrolysis, and the hyd...

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PUM

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Abstract

The invention relates to a synthetic process for glyphosate. The synthetic process comprises the following steps: 1) adding methyl alcohol, paraformaldehyde and triethylamine into a condensation kettle in turn; 2) adding glycine; 3) adding dimethyl phosphite, rising temperature, reacting and cooling after the material is transparent; 4) pump into acidizing kettle, adding hydrochloric acid, stirring after completely adding, rising temperature and dealcoholizing, deacidifying, rising temperature, dealcoholizing and keeping the temperature till the material becomes yellow; 5) adding water, putting into a product kettle, discharging, slowly adding liquid caustic soda, regulating PH, cooling and centrifuging, thereby acquiring the centrifuging solid, namely, a glyphosate raw drug. The invention solves the problems of long production period and low yield, namely, the production period is shortened and the yield is increased; the yield is lower and the purity is lower in the prior art; the yield according to the invention is 1.5 times of the prior art and the purity is increased to 96.90%.

Description

technical field [0001] The invention relates to the field of pesticide processing, in particular to a synthesis process of glyphosate. Background technique [0002] As a broad-spectrum herbicide, glyphosate has become the most widely used and most productive pesticide product in the world due to its special herbicidal effect. In recent years, with the development of transgenic glyphosate-resistant crops, the amount of glyphosate has increased year by year. At present, the synthesis and production of glyphosate mainly pass through two routes: IDA route and glycine route. Foreign glyphosate manufacturers mainly follow the IDA route to produce glyphosate; domestic glyphosate manufacturers mostly use the glycine production route independently developed by my country. The production process of glycine route mainly includes: depolymerization, addition, condensation, hydrolysis and crystallization. Due to the diversity and complexity of its synthesis reactions and some uncontroll...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
CPCC07F9/3813
Inventor 黄中桂蔡小林袁晓林付志平史正光朱凯明黄锋杨镭郑宏亮刘心龙
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD