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Hydrolysis process in the process of preparing glyphosate by glycine method

A technology of glyphosate and glycine, applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of difficult wastewater treatment, consumption of hydrochloric acid and liquid alkali, etc., and achieve easy recycling , Reduce the amount of alkali used and improve the efficiency of use

Active Publication Date: 2012-02-01
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 removes the solvent methanol and the catalyst triethylamine through vacuum distillation and steam distillation, which solves the problem of the large consumption of hydrochloric acid and liquid caustic soda in the hydrolysis process and post-treatment of triethylamine, and the generation of salt at the same time makes the waste water difficult to treat. problems, and the use of vacuum recovery also saves a lot of steam

Method used

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  • Hydrolysis process in the process of preparing glyphosate by glycine method
  • Hydrolysis process in the process of preparing glyphosate by glycine method
  • Hydrolysis process in the process of preparing glyphosate by glycine method

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Take 870g of methanol, 270g of triethylamine, 160g of paraformaldehyde, 200g of glycine, and 350g of dimethyl phosphite to obtain 1850g of condensation liquid, and directly carry out vacuum distillation at a temperature of 65-70°C and a pressure of -0.085-0.090 Mpa, get 895ml distillate, distillate is condensed and with 3A 0 Molecular sieve (K 72 Na 48 [(AlO 2 ) 12 (SiO 2 ) 12 ]·XH 2 (2) 55g after drying, obtain methyl alcohol and triethylamine mixed solution 843.8g (wherein methyl alcohol 826.5g is 95% of feeding intake; Triethylamine 17.3g is 6.4% of charging amount)

[0027] Transfer the residual liquid in the separator to a four-necked reaction flask for steam distillation, inject saturated water vapor with a pressure of 0.03MPa, and distill for 48 minutes at a temperature of 80-83°C in the reaction flask to obtain 350ml of distillate Add 10ml of 30% sodium hydroxide solution to the distillate and transfer it to a separatory funnel, let it stand for 5 hours, ...

Embodiment 2

[0031] Take 1740kg of methanol, 540kg of triethylamine, 320kg of paraformaldehyde, 400kg of glycine, and 700kg of dimethyl phosphite to react to obtain 3700kg of condensation liquid at a temperature of 58°C. Pass into the flash tank for distillation, the pressure is -0.082, control the amount of steam in the flash tank and the amount of condensed liquid entering the flash tank, so that the temperature in the flash tank is 70±2°C, and the pressure is lower than -0.08 MPa. Distillation under reduced pressure took 92 minutes to obtain 1786L distillate, which was condensed and purified with 4A 0 Molecular sieve (molecular sieve type 10X) 120Kg after drying, obtain methanol and triethylamine mixed solution 1681Kg (wherein methanol 1655Kg, is 95.1% of feed intake; Triethylamine 25.7Kg, is 4.8% of feed intake)

[0032] The residual liquid was transferred to a 3000L reactor for steam distillation, and saturated water vapor with a pressure of 0.12MPa was introduced, and the temperatur...

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Abstract

The invention relates to a hydrolysis process in the process of preparing glyphosate by a glycine method, which is to directly carry out vacuum distillation and separation of the condensate mixture containing condensate triethylamine salt, methanol and a small amount of unsalted triethylamine, and distillate The product is reused after being condensed and dehydrated by molecular sieves, the residual liquid is subjected to steam distillation, and the distillate is adjusted to pH 8-9 with sodium hydroxide solution, left to stand, separated to obtain triethylamine, and directly reused after drying. The distilled raffinate is then hydrolyzed by adding hydrochloric acid to obtain glyphosate product. The invention solves the problem that triethylamine consumes a large amount of hydrochloric acid and liquid caustic soda in the hydrolysis process and post-treatment, and generates salt at the same time, resulting in difficult wastewater treatment; and adopting vacuum recovery not only greatly improves the recovery rate of methanol and triethylamine, but also A large amount of steam is saved, and the hydrolysis efficiency is high, the reaction time can be reduced from 8 hours to 2-4 hours, and the total yield of solid glyphosate reaches 74%.

Description

technical field [0001] The invention relates to a hydrolysis process in the process of preparing glyphosate by a glycine method. Background technique [0002] Glyphosate is an environmentally friendly broad-spectrum herbicide that can effectively remove 76 of the 78 most harmful weeds in the world. With my country's accession to the WTO and the improvement of people's living environment requirements, glyphosate is in line with the development direction of the world's pesticide industry because of its high efficiency, low toxicity, broad spectrum, and no residue. It is the most brilliant chemical pesticide in the world in the 20th century. With the rapid promotion of global glyphosate-resistant transgenic crops in the 21st century, their market prospects will be even broader. The glycine method occupies a dominant position in the production of glyphosate in China. The most critical link affecting the yield in the preparation route of the glycine method is the hydrolysis of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 姜永红周建强
Owner SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD