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Method for preparing glyphosate by PMIDA of catalytic oxidizing by gas containing molecular oxygen

A technology of gas catalysis and glyphosate, applied in chemical instruments and methods, botany equipment and methods, organic chemistry, etc., can solve the problems of difficult operation, high cost, and no practical production significance, etc. Concentration, stable product quality, and cost reduction effects

Inactive Publication Date: 2010-01-06
李欣荣
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the oxidant in this method adds a large amount of hydrogen peroxide with a high ratio in addition to oxygen, the cost will remain high, and the operation is difficult. Even if the yield is good, there is no practical production significance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Diglyphosate 400g (1.73mol) water 500g, the specific surface is 1200m 2 50g of powdered activated carbon per gram is put into a stainless steel low-pressure reactor, and the temperature is raised to 70°C at a stirring speed of 1500 rpm by using inclined blades, and an oxygen-enriched gas with an oxygen volume concentration of 98% is introduced, and the inlet gas is controlled. The pressure is used to adjust the pressure of the reactor, and the pressure is controlled at about 0.2Mpa, and the flow rate of the incoming gas is controlled through the reactor exhaust valve, and the flow rate is controlled at 5m 3 / h·kmol bisglyphosate and measure the oxygen content at the exhaust outlet online. When the oxygen concentration increases rapidly and reaches more than 10% in 10 minutes, the reaction is over, and the reaction liquid is cooled and frozen to -5°C. When the crystals are folded out, they are separated to remove the mother liquor containing formaldehyde and other harmfu...

Embodiment 2

[0024] Diglyphosate 400g (1.73mol) water 500g, specific surface area is 1500m 2 40g of powdered activated carbon per gram is put into a stainless steel low-pressure reactor, using a flat plate slurry, heating up to 30°C at a stirring speed of 800 rpm, and feeding oxygen-enriched air with an oxygen volume concentration of 92%, by controlling the inlet gas pressure To adjust the reactor pressure, the pressure is controlled at about 0.2Mpa, and the flow rate of the gas is controlled through the reactor exhaust valve, and the flow rate is controlled at 5m 3 / h·kmol bisglyphosate and measure the oxygen content at the exhaust outlet online. When the oxygen concentration increases rapidly and reaches more than 15% in 10 minutes, the reaction is over, and the reaction solution is cooled and frozen to -8°C. When the crystals are folded out, they are separated, and the mother liquor containing formaldehyde and other harmful impurities is separated, filtered and waited for treatment.

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Abstract

This invention relates to a method of using gas containing molecular oxygen to catalytic oxidate double-gan phosphine for preparing glyphosate. The steps:(1) mix double-gan phosphine, water and activated carbon, at condition of speed of agitator 800 to 1500 r / m , inlet oxygen enrichment gas to carry out reaction, reactant liquor for refrigeration, glyphosate seed out, collect glyphosate and activated carbon blending press cake, divide mother solution with deleterious impurities such as formaldehyde; (2) plunge glyphosate and activated carbon admixture press cake to glyphosate saturation solution, after glyphosate dissolving take filtration while hot, filtrate recooling, glyphosate seedout, cake drying, then gain glyphosate solid; or plunge press cake to water, cooling, drop isopropylamine or inlet alkaline air, directly prepare isopropylamine salt or ammonium salt water solution.

Description

technical field [0001] The invention relates to a preparation method of glyphosate, in particular to a method for preparing glyphosate by catalytically oxidizing diglyphosate with a gas containing molecular oxygen. Background technique [0002] Glyphosate, also known as phosphonomethylglycine, is an important pesticide variety, and it is currently the herbicide with the largest output and the widest application range in the world. [0003] Diglyphosate, also known as phosphonomethyliminodiacetic acid, has many methods to prepare glyphosate by catalytic oxidation of gas containing molecular oxygen. Glyphosate is oxidized into a method for glyphosate. The content of glyphosate in the synthesis solution of this method is relatively ideal, and the cost is also low. However, the by-product formaldehyde of this method is easy to react with the finished product glyphosate to generate N-methyl glyphosate Phosphine, resulting in poor stability of glyphosate, rapid decline in product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38A01N57/12
Inventor 李欣荣
Owner 李欣荣
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