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Method for preparing glyphosate

A technology of glyphosate and bisglyphosate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., to reduce energy consumption, realize automatic control, and reduce reaction pressure

Inactive Publication Date: 2012-09-26
SICHUAN DIMEITE BIOLOGICAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses a single-pot internal circulation crystallization tank, which uses multiple circulation pumps for circulation, which requires high technical requirements for refrigeration equipment and will increase energy consumption.
And CN101139262A adopts 2~3 crystallization kettles connected in series, the mode section cooling crystallization that material is transported to the external heat exchanger by circulating pump, this method has increased equipment investment, has increased energy consumption, and the crystallization after crystallization There is no corresponding treatment plan for glyphosate mother liquor

Method used

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  • Method for preparing glyphosate
  • Method for preparing glyphosate
  • Method for preparing glyphosate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] see figure 1 , figure 2 , 100g of bisglyphosate, 6.6g of activated carbon, and 893g of water were made into a suspension and dropped into the pressure reactor 1. The water is deionized water, the mass fraction of bisglyphosate is greater than 98%, and the specific surface area of ​​activated carbon is 1200m 2 / g. Close the pressure reactor, start stirring, heat, and raise the temperature to 75°C at a stirring speed of 700r / min, feed oxygen at a flow rate of 0.3L / min, control the pressure of the reactor to 0.3MPa, and the reaction time to 90min. Release the pressure to normal pressure, take a sample to detect the diglyphosate, and stop the oxygen flow after the diglyphosate is completely converted. The reaction material is heated to 90° C. and filtered through the first microporous filtration device 2 to obtain filter cake I and mother liquor I. Filter cake I activated carbon was used as a catalyst for the next oxidation reaction. The mass fraction of glyphosate wa...

Embodiment 2

[0041] see figure 1 , figure 2 100g bisglyphosate, 893g water and embodiment 1 reclaim filter cake I activated carbon (add 5% fresh activated carbon of activated carbon consumption percentage in embodiment 1) to be made into suspension, drop in the pressure reaction kettle; Wherein water adopts to remove Ionized water, the mass fraction of bisglyphosate is greater than 98%, and the specific surface area of ​​activated carbon is 1200m 2 / g. Close the pressure reactor, start stirring, heat, and raise the temperature to 75°C at a stirring speed of 700r / min, feed oxygen at a flow rate of 0.3L / min, control the pressure of the reactor to 0.3MPa, and the reaction time to 90min. Release the pressure to normal pressure, take a sample to detect the diglyphosate, and stop the oxygen flow after the diglyphosate is completely converted. The reaction material is heated to 90° C. and then filtered through the first microporous filter device to obtain filter cake I and mother liquor I. ...

Embodiment 3

[0044] see figure 1 , figure 2 , with 100g bisglyphosate, 893g glyphosate crystallization mother liquor (after the mother liquor II of embodiment 1 is used as the refrigerant of embodiment 2) and the recovery filter cake I activated carbon of embodiment 2 (adding 5% of the active carbon consumption percentage in embodiment 2 fresh Activated carbon) is made into a suspension and put into a pressure reactor; the mass fraction of bisglyphosate is greater than 98%, and the specific surface area of ​​activated carbon is 1200 m 2 / g. Close the pressure reactor, start stirring, heat, and control the stirring speed at 700r / min to raise the temperature to 75°C, feed oxygen at a flow rate of 0.3L / min, control the pressure of the reactor to 0.3MPa, and the reaction time to 90min. Release the pressure to normal pressure, take a sample to detect the diglyphosate, and stop the oxygen flow after the diglyphosate is completely converted. The reaction material is heated to 90° C. and then...

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Abstract

The invention discloses a method for preparing glyphosate, and the method comprises the following steps: 1) mixing raw material water, a N-Phosphonomethyl aminodiacetic acid and active carbons in certain proportion so as to obtain a suspension, adding the obtained suspension into a pressure reaction kettle, and closing the pressure reaction kettle to carry out oxidation reaction on the suspension, so as to rapidly oxidize the N-Phosphonomethyl aminodiacetic acid; and carrying out sampling analysis on the mass fraction of the N-Phosphonomethyl aminodiacetic acid in reaction liquid, when the N-Phosphonomethyl aminodiacetic acid is completely transformed, stopping feeding oxygen into the reaction kettle, and carrying out pressure relief until the reaction kettle is at ordinary pressure; 2) raising the temperature of the materials subjected to reaction to 80-100 DEG C, filtering the materials by using a microporous filtering device so as to obtain a filter cake I mainly containing the activated carbons and a mother solution I; and 3) carrying out continuous multi-effect crystallization on the mother solution I, separating solids from the mother solution I by using the microporous filtering device so as to obtain a filter cake II and a mother solution II, and drying the filter cake II so as to obtain a glyphosate chemical. The method disclosed by the invention is safe in operation, short in reaction period, high in production efficiency, low in production cost, low in energy consumption, and less in emission of'three wastes'.

Description

Technical field: [0001] The invention relates to a method for preparing glyphosate. Background technique: [0002] Glyphosate is a high-efficiency, broad-spectrum, low-toxic organic phosphine post-emergence herbicide successfully developed by Monsanto Chemical Company in the 1960s. Its chemical name is N-phosphonomethylglycine (PMG). The most widely used herbicide. [0003] The synthesis process of glyphosate is mainly divided into two categories, namely the alkyl ester method and the iminodiacetic acid method (IDA method). The alkyl ester method is to prepare glyphosate through hydrolysis after condensation of glycine, paraformaldehyde and alkyl phosphite. The iminodiacetic acid method uses iminodiacetic acid, formaldehyde, and phosphorous acid as raw materials to prepare the intermediate bisglyphosate (PMIDA), and then catalyzes the oxidation to obtain glyphosate. [0004] The catalytic oxidation of diglyphosate to prepare glyphosate mainly includes hydrogen peroxide ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38C07D487/18
Inventor 王国成杨华詹源文陈松梁晓禽
Owner SICHUAN DIMEITE BIOLOGICAL SCI & TECH
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