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
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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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