Method for preparing N-(phosphonomethyl) iminodiacetic acid and glyphosate by using non-alkali metal

A technology of diglyphosate and glyphosate, applied in herbicides and algicides, chemical instruments and methods, chemicals for biological control, etc., can solve environmental pollution, waste of sodium hydroxide and hydrochloric acid raw materials, waste Resources and other issues

Inactive Publication Date: 2010-03-24
李坚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Up to now, for the preparation method of glyphosate, there have been many researches on the IDA route, such as VS5312973, VS5023369, ZL93120707, ZL96195765, 03147313X and other invention patents. These invention patents include the domestic production of diglyphosate and All glyphosate companies use a large amount of alkali metal sodium hydroxide. The main process feature is that iminodiacetonitrile or diethanolamine is used as raw material, and sodium hydroxide is used for hydrolysis to prepare iminodiacetic acid diacetate. Sodium salt, and then use hydrochloric acid to neutralize the disodium salt to prepare iminodiacetic acid, and then use this iminodiacetic acid to prepare diglyphosate and glyphosate. In this production process, sodium hydroxide and hydrochloric acid are repeatedly and alternately neutralized The reaction is the main source of industrial wastewater. The production of one ton of diglyphosate produces 4 to 6 tons of wastewater, and the production of one ton of glyphosate produces 8 tons of wastewater. The output of glyphosate produced by the IDA route in China is close to 200,000 tons / year, and the resulting waste brine alone exceeds 1.6 million tons / year. The main reason is that all production enterprises have adopted the process of converting nitrile groups into sodium carboxyl salts by hydrolysis with alkali metals. In order to convert sodium carboxyl The salt becomes carboxyl, and a large amount of hydrochloric acid must be used for neutralization, which not only produces a large amount of sodium chloride waste brine, but also wastes a large amount of sodium hydroxide and hydrochloric acid raw materials, which not only pollutes the environment, but also increases production costs. resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Molecular ratio: iminodiacetonitrile (or diethanolamine): formaldehyde: phosphorous acid: hydrochloric acid = 1:1~2:1~1.2:0~4.

[0026] Add 157 grams of 37% formaldehyde solution into a 1000ml four-necked reaction bottle, start stirring, control the temperature at 30-60°C, slowly add 100 grams of 92% iminodiacetonitrile (or diethanolamine), and react for 1-4 hours , when the content of iminodiacetonitrile in the analysis and test reaction system is ≤1%, it is the end of the reaction, and then under normal pressure or vacuum conditions, distill water and excess formaldehyde, and analyze and test when the water content in the distillation substrate is ≤4% , add 348 grams of 30% hydrochloric acid aqueous solution (or concentrated sulfuric acid 70 grams), control reaction temperature 30~150 ℃, reflux reaction 2~24 hours, preferably 4~6 hours, analyze and test the hydroxymethyl imino two in reaction system Then, steam hydrochloric acid water as much as possible under normal ...

Embodiment 2

[0028] Put 100 grams of 92% iminodiacetonitrile (or diethanolamine) into 348 grams of 30% hydrochloric acid aqueous solution (or 60% sulfuric acid), reflux for 4 to 16 hours, and try to distill the hydrochloric acid aqueous solution for the next time. Apply mechanically, put in 520 grams of anhydrous methanol, 98 grams of anhydrous triethylamine (or anhydrous acetic acid), 58 grams of paraformaldehyde, stir and react at 20-45°C for 0.5-3 hours, then cool down to normal temperature, and filter to separate chlorine Ammonium chloride solid, under high vacuum, try to distill out triethylamine and methanol in the mother liquor, in order to prepare for the next time, slowly add the calculated amount of water and phosphorous acid solid 95 grams to the filtered mother liquor, control the temperature 30 ~ 100 ℃, the reaction time is 1-6 hours, the temperature is lowered, left standing, filtered and dried to obtain 224 grams of bisglyphosate with a content of 98%.

Embodiment 3

[0030] Put 100 grams of 92% iminodiacetonitrile (or glycol amine) into 117 grams of 37% formaldehyde solution, add 100-200 grams of deionized water, start stirring, and slowly add 98% phosphorous acid solid 81-95 gram, control reaction temperature 30~100 ℃, reaction time 1~12 hours, steam solvent water and excess formaldehyde, in order to apply mechanically next time, add 400 grams of hydrochloric acid aqueous solution (or 250 grams of 60~80% sulfuric acid) of calculated amount) , at 67°C, add 122 grams of 27% hydrogen peroxide dropwise, control the temperature at 67-100°C, and react for 4-24 hours, then lower the temperature to 50°C, slowly add 22 grams of 10% ferrous sulfate solution, and react for 1-3 hours , the reaction is finished, then the pH value is adjusted to about 4 with ammonia water, the temperature is lowered to stand, filtered, and dried to obtain 145 grams of glyphosate, with a content of 96%. The aftertreatment of filtering mother liquor is the same as above-...

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PUM

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Abstract

The invention relates to a new method for preparing N-(phosphonomethyl) iminodiacetic acid and glyphosate by taking iminodiacetonitrile or diethanolamine as a raw material, and the whole reaction process does not use alkali metal; compared with the prior production process for preparing the N-(phosphonomethyl) iminodiacetic acid and the glyphosate, the new method can achieve the purposes of greatly reducing the energy consumption and reducing the emission of waste water.

Description

technical field [0001] The invention relates to a new method for preparing diglyphosate and glyphosate by using iminodiacetonitrile or diethanolamine as raw materials, and the whole reaction process does not need to use alkali metals to prepare diglyphosate and glyphosate. The process can achieve the purpose of greatly reducing energy consumption and reducing waste water discharge. Background technique [0002] Glyphosate is a new type, high efficiency, low toxicity, no residue, broad-spectrum herbicide, and can also be used as a plant growth regulator. In the route of glyphosate, diglyphosate is the most important intermediate. However, diglyphosate has developed into a very important export chemical product in my country, and many non-pesticide companies are producing and selling it. The inventor of the present invention has applied for an invention patent in 2008. Its name is "preparation method of glyphosate technical", and the application number is 200810131794X. The in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38A01P13/00
Inventor 李坚
Owner 李坚
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