Application of phosphine or hypophosphite or phosphate in preparation of glyphosate

A technology of glyphosate and phosphorous acid, applied in application, organic chemistry, herbicides and algicides, etc., can solve the problems of large wastewater discharge, many by-products, increased production costs, etc., and achieve the goal of reducing wastewater discharge Effect

Inactive Publication Date: 2010-09-08
李坚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 2. Combining the three main raw materials of iminodiacetic acid, formaldehyde, and phosphorous acid to produce glyphosate. These two routes have been used for nearly 20 years, and there are defects such as large waste water discharge and many by-products. The first route must be To produce equimolar methylal and chloromethane, the second route must produce equimolar acetic acid. Because the recovery of these by-products increases production costs, most production companies do not recycle these by-products at present, causing serious environmental problems. Pollution, the above two production routes are increasingly unable to meet the requirements of environmental protection in the future

Method used

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  • Application of phosphine or hypophosphite or phosphate in preparation of glyphosate
  • Application of phosphine or hypophosphite or phosphate in preparation of glyphosate
  • Application of phosphine or hypophosphite or phosphate in preparation of glyphosate

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Molecular ratio: phosphine: hydroxymethylglycine hydrochloride = 1: 0.5 ~ 1

[0035] Use N,N-dimethylformamide as a solvent, prepare about 40% hydroxymethylglycine salt solution, put it into the reaction kettle, start stirring, control the temperature below 40°C, and slowly introduce the calculated amount of phosphine Gas, after reacting to the end point, A compound is generated, and the reaction yield is 94%.

[0036] Then control the temperature between 40 and 80°C, and slowly introduce air into the oxidation reaction for 2 to 8 hours. Gradually, solid glyphosate hydrochloride will precipitate out of the solvent. After the reaction reaches the end, filter and dry to obtain glyphosate. Hydrochloride solid. The filtrate is recovered and applied mechanically, and the reaction yield of this step is 98%.

[0037] Below 0°C, slowly add glyphosate hydrochloride into 20% ammonia solution to neutralize to form glyphosate and ammonium chloride, adjust the pH value to 1-3, and...

Embodiment 2

[0039] Molecular ratio: sodium hypophosphite: hydroxymethylglycine hydrochloride = 1:1

[0040] Use butanol as a solvent, prepare about 40% hydroxymethylglycine hydrochloride solution, put it into the reaction kettle, start stirring, control the temperature below 60°C, slowly add the calculated amount of sodium hypophosphite solid, and keep warm for 2~ After 8 hours, after the reaction reached the end point, the new compound B was generated, and the reaction yield was 94%.

[0041] Subsequent process is identical with the subsequent process of embodiment 1.

Embodiment 3

[0043] Put 20g of 98% glycine and 21.8g of 98% phosphorous acid into a 500ml reaction bottle at one time, start stirring, and slowly add 82.4g of 30% NaOH solution dropwise below 40°C, then control the temperature at 40-110°C, slowly Add 21.4g of 36.5% formaldehyde solution dropwise, keep warm for 1 to 2 hours, cool to about 2°C, and stand at this temperature for 18 hours to crystallize, a large amount of solids precipitate, filter, and dry to obtain the disodium of the new compound C Salt solid 48.8g, the filtrate is recovered and used mechanically.

[0044] Pass hydrochloric acid gas into the N,N-dimethylformamide solvent to form a saturated solution of hydrochloric acid, control the temperature below 10°C, slowly add the disodium salt solid of the new compound C into the saturated solution, and generate a large amount of compound C and Solid mixture of sodium chloride, control the temperature at 80-150°C, keep warm for 2-8 hours, compound C isomerized into glyphosate gradua...

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Abstract

The invention relates to a novel method for preparing glyphosate herbicide by adopting a phosphine or hypophosphite or phosphate compound as a raw material, in particular to the usage of the compounds in the production field of glyphosate. One-step reaction between the compounds and sodium hydroxymethylaminoacetate or hydroxymethylaminoacetate hydrochloride produces a tervalent organic phosphoruscompound, and then further oxidation or isomerization produces glyphosate.

Description

technical field [0001] The present invention relates to a kind of new method that is raw material preparation glyphosate herbicide with phosphine or hypophosphite or phosphite compound, relate in particular to the purposes of these compounds in the field of glyphosate production, these compounds and hydroxymethyl The one-step reaction of sodium glycinate or hydroxymethylglycine hydrochloride can first synthesize trivalent organic phosphorus compounds, and then further oxidize or isomerize to synthesize glyphosate. Background technique [0002] Phosphine or hypophosphite or phosphite is a traditional inorganic phosphorus chemical raw material, widely used in electroplating industry, food industry, pharmaceutical industry, coating industry and other fields, phosphine itself is a traditional pesticide fumigant, widely used It is used in the sterilization of grain storage, but there is still no literature report on the application of glyphosate in the production field. Glyphosa...

Claims

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Application Information

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IPC IPC(8): C07F9/141C07F9/48C07F9/50C07F9/38A01N57/12A01N57/20A01P13/00
Inventor 李坚
Owner 李坚
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