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New preparation method of herbicide glyphosate

A glyphosate and solvent technology is applied in the new field of preparation of herbicide glyphosate, which can solve the problems of increasing production cost and polluting the environment, and achieve the effects of reducing production cost, reducing waste water discharge and reducing exhaust gas discharge.

Inactive Publication Date: 2015-07-01
李坚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Put paraformaldehyde, methanol and triethylamine into the reaction kettle. After the paraformaldehyde is dissolved, put in dry glycine. When the reaction solution is transparent, add dimethyl phosphite dropwise. After the reaction reaches the end point, add a large amount of hydrochloric acid aqueous solution for The hydrolysis reaction produces glyphosate. In order to recover methanol and triethylamine, two processes of methanol tower recovery and triethylamine recovery must be configured. In these two processes, a large amount of sodium chloride waste brine is produced, especially organic phosphorus in wastewater The compound content is as high as 2-4%. Since the sodium chloride content in the wastewater is as high as 15%, the biochemical wastewater treatment cannot be carried out by the method of active bacteria, and other treatment methods have greatly increased the production cost. Therefore, there are currently many glyphosate Phosphine production enterprises directly discharge these wastewater into rivers, seriously polluting the environment

Method used

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  • New preparation method of herbicide glyphosate
  • New preparation method of herbicide glyphosate
  • New preparation method of herbicide glyphosate

Examples

Experimental program
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Effect test

Embodiment 1

[0060] Molecular ratio: glycine: formaldehyde: hydrochloric acid: phosphorus trichloride = 1:2:2:1.02~1.05

[0061] Put 100 grams of 95% glycine and 304 grams of 30% hydrochloric acid into a four-necked reaction bottle at one time, start stirring, control the temperature at about 60°C, and add 211 grams of 36% formaldehyde dropwise. Turn on the vacuum and distill water, hydrochloric acid and formaldehyde as much as possible at 60°C. The distillation substrate is hydroxymethylglycine hydrochloride. Then, add 30 grams of N, N-dimethylformamide solvent at room temperature, and add Slowly add 181 grams of 98% phosphorus trichloride dropwise, control the temperature at about 74°C and keep it warm for 2 hours, then under high vacuum, try to distill off the solvent and excess phosphorus trichloride, and the distillation substrates are I and II Then, slowly add 80 grams of pure water under normal pressure, control the temperature at 90-110°C, hydrolyze for 4 hours, turn on the vacuum ...

Embodiment 2

[0063] Molecular ratio: sodium hydroxymethylglycine: phosphorus trichloride = 1: 1 ~ 1.02

[0064] Put 100 grams of 98% phosphorus trichloride and 145 grams of N,N-dimethylformamide into the reaction bottle at one time, start stirring, control the temperature at about 25°C, and slowly add anhydrous sodium hydroxymethylglycinate solid 165 gram, heat preservation reaction for 1 to 2 hours, then, at about 20 ° C, the NaCl solid generated is filtered out, the filtered mother liquor is returned to the reactor, the vacuum is turned on, and the N, N-dimethylolformamide solvent and excess Phosphorus trichloride, the distillate can be applied mechanically, and the distillation substrate is the new compound mixture of W and G. Then, under normal pressure, add 100 grams of water to the distillation substrate, control the temperature at 60-110°C, and perform the hydrolysis reaction for 2 ~8 hours, then, turn on the vacuum, distill hydrochloric acid and water as far as possible, the distil...

Embodiment 3

[0066] Molecular ratio: glycine: formaldehyde: HCl: phosphorus trichloride = 1:2~4:0~1:1

[0067] Put 100 grams of 95% glycine and 100 grams of pure water into the reaction bottle at one time, start stirring, control the temperature at about 60°C, and observe the transparency of the reaction system, then slowly add 317 grams of 36% formaldehyde dropwise, and keep the temperature for 4 hours. Turn on the vacuum, steam out water as much as possible, steam out excess hydrochloric acid and excess formaldehyde, and the distillation substrate is N, N——dimethylolglycine. Then, add 50 grams of anhydrous ethyl acetate to the distillation substrate, control the temperature at about 40°C, slowly add 177 grams of 98% phosphorus trichloride dropwise, keep the reaction for 1 hour, and then under high vacuum, try to distill out Solvent and excess phosphorus trichloride, the distillation substrate is the new compound mixture of C and D, 280 grams of 60% methanol aqueous solution is added to t...

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Abstract

The invention relates to a new preparation method of herbicide glyphosate by using phosphorus trichloride and hydroxymethyl glycinate or sodium hydroxymethylglycinate, or phosphorus trichloride and N,N-dihydroxymethylglycinate or iminodiacetonitrile as raw materials. In the method, the glyphosate or glyphosine is prepared by using a new compound produced by the mutual reaction among the raw materials as an intermediate through a further hydrolysis reaction. Compared with the traditional process for producing the glyphosate or the glyphosine, the production cost is reduced by more than 15%, and the whole production process can reach a clean production process standard with ultra low discharge of waste water.

Description

technical field [0001] The present invention relates to a method that uses phosphorus trichloride and hydroxymethylglycine hydrochloride or sodium hydroxymethylglycine, or phosphorus trichloride and N,N-dimethylolglycine or iminodiacetonitrile as raw materials A new method for preparing the herbicide glyphosate, the present invention particularly relates to a new compound synthesized by the mutual reaction of these raw materials as an intermediate, and then, glyphosate or bisglyphosate is prepared through a one-step hydrolysis reaction, which is compatible with the existing glyphosate Or compared with the production process of bisglyphosate, not only the production cost is reduced by more than 15%, but also the whole production process can meet the clean production process standard of ultra-low discharge of waste water. Background technique [0002] Regarding hydroxymethylglycine hydrochloride, it is recorded in the invention patent filed by the applicant for the patent of t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/42C07F9/06C07F9/40C07F9/38A01N57/20A01P13/00
Inventor 李坚
Owner 李坚