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Hydrolyzation post-processing technique during preparation of glyphosate through glycin method

A technology of glycine and glyphosate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of increasing the total amount of mother liquor, difficult waste water treatment, and high energy consumption, Achieve the effect of increasing surface area, reducing time and reducing energy consumption

Active Publication Date: 2010-03-17
SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process separates the hydrolyzate after hydrolysis by vacuum distillation, recycles and utilizes the excess hydrochloric acid after hydrolysis, and does not add alkali during crystallization, thus solving the problem of increasing the total amount of mother liquor caused by adding liquid alkali solution, high energy consumption, and Problems such as the harm caused by excessive sodium salt to soil and crops, etc., and also solve the problem that the waste water is not easy to treat due to the generation of salt

Method used

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  • Hydrolyzation post-processing technique during preparation of glyphosate through glycin method
  • Hydrolyzation post-processing technique during preparation of glyphosate through glycin method
  • Hydrolyzation post-processing technique during preparation of glyphosate through glycin method

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Effect test

Embodiment 1

[0024] While stirring, add 280g of methanol, 85g of triethylamine, 49.5g of paraformaldehyde, 62.5g of glycine, and 109.5g of dimethyl phosphite into the four-necked reaction flask in order to complete the depolymerization, addition, and condensation reactions. Obtain the condensed liquid, directly add 330g of 31% hydrochloric acid (the mol ratio of glycine and hydrochloric acid is 1: 3.4) under agitation and carry out hydrolysis, control temperature when adding acid and be not higher than 45 ℃, treat that after hydrochloric acid adds, begin to slowly heat up, gas phase Condensation was collected in a flask. First, the temperature was raised to 80°C in 140 minutes, and then to 117°C in 130 minutes, and kept for 20 minutes to obtain a hydrolyzed solution.

[0025] Distill the hydrolyzate under reduced pressure, the pressure is 0.025-0.03Mpa, the temperature drops rapidly to 80±3°C, and then rises slowly, it takes 30 minutes, the temperature rises back to 110±2°C, and 150ml of d...

Embodiment 2

[0027] Get methanol 2800kg, triethylamine 850kg, paraformaldehyde 495kg, glycine 625kg, dimethyl phosphite 1095kg reaction to obtain condensation liquid, directly add 30% hydrochloric acid 330g under stirring (the mol ratio of glycine and hydrochloric acid is 1: 3.34) Carry out hydrolysis, control the temperature not higher than 45°C when adding acid, and start to slowly heat up after adding hydrochloric acid. First, the temperature was raised to 80°C in 140 minutes, and then to 117°C in 130 minutes, and kept for 20 minutes to obtain a hydrolyzed solution.

[0028] Pass the hydrolyzate into the flash tank for distillation, control the amount of steam in the flash tank and the amount of hydrolyzate entering the flash tank, so that the temperature in the flash tank is not lower than 80±2°C, and the pressure is 0.08-0.085 MPa. The vacuum distillation took 60 minutes to obtain 1650L of condensed distillate and a mixed solution of hydrochloric acid. The content of hydrochloric aci...

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Abstract

The invention relates to a hydrolyzation post-processing technique during preparation of glyphosate through a glycin method, which includes the steps of implementing reduced pressure distillation andseparation to a hydrolyzation liquor under the temperature between 80 and 110 DEG C and the pressure equal to or less than 0.05MPa after the condensation reaction and hydrolysis reaction for preparingglyphosate through the glycin method are finished, depickling and then crystallizing to obtain the glyphosate products. The hydrolyzation post-processing technique during preparation of glyphosate through the glycin method recovers hydrochloric acid by reducing the pressure, which can lead the recovery rate of hydrochloric acid to be more than 4 percent; and hot water is added for crystallizing after the hydrochloric acid is removed, thus effectively improving the availability factor of a crystallization kettle; and meanwhile, as no caustic soda liquor is added during hydrolyzation, the totalamount of a mother liquor and the content of sodium chloride are reduced as well, the energy consumption for recovering triethylamine through rectifying the mother liquor is reduced, and the total yield of the finally obtained solid glyphosate reaches 73-75 percent.

Description

technical field [0001] The invention relates to a post-hydrolysis treatment process in the process of preparing glyphosate by a glycine method. technical background [0002] Glyphosate is a high-efficiency, broad-spectrum, low-toxic and safe organophosphorus herbicide, which can effectively remove 76 of the 78 most harmful weeds in the world. The application is very extensive. With my country's entry into WTO and the improvement of people's living environment requirements, as well as the rapid promotion of global glyphosate-resistant transgenic crops in the 21st century, its market prospect will be even broader. There are two synthetic methods: IDA method and glycine method. [0003] At present, the commonly used method in domestic production enterprises is the glycine method, which is obtained by addition, condensation and hydrolysis of glycine, dialkyl phosphite and paraformaldehyde as raw materials, and the original glyphosate is obtained after crystallization, solid-li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 肖艳姜永红何耀宏
Owner SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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