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Preparation method for glyphosate dimethylamine salt active compound

A technology of glyphosate dimethylamine salt and glyphosate, which is applied in the field of preparation of glyphosate dimethylamine salt technical material, can solve the problem of severe exothermic reaction, which is very difficult to control and requires very strict sealing conditions for equipment and other problems, to overcome the effect of greatly reducing the reaction area, good quality of the original drug, and increasing the reaction area

Active Publication Date: 2016-09-21
SHANDONG RUNBO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as the reaction progresses, the pressure of the reaction system will be very high, and the sealing conditions of the equipment are very strict; and

Method used

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  • Preparation method for glyphosate dimethylamine salt active compound

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0033] Example 1

[0034] Put 1000 g of glyphosate technical material (95% content) into the kneader, add 50 g of water at 5°C and mix evenly, and add 253 g of pure liquid dimethylamine (99.9% content) dropwise under sealed conditions, The dropwise addition time was 5 h. Due to the vaporization of dimethylamine and the increase in temperature, the reaction pressure gradually increased, up to 0.1 MPa. After the dropwise addition, the temperature was raised to 50 °C and the reaction was continued for 30 min. The excess dimethylamine was put into the absorption tower, and then discharged, and the obtained wet material was dried for 0.5 hours at a pressure of -0.08 MPa and 30°C to obtain a content of 96.1% (the content was determined by HPLC method, the same below). Glyphosate dimethylamine salt 1242.9 g, the yield (yield is calculated as glyphosate, the same below) is 99.2%.

Example Embodiment

[0035] Example 2

[0036] Put 1000 g of glyphosate technical material (content 95%) into the kneader, add 50 g of water at 70°C and mix evenly, add 253 g of pure liquid dimethylamine (content 99.9%) dropwise under sealed conditions, The dropwise addition time is 2 h. Due to the gasification of dimethylamine and the increase of temperature, the reaction pressure gradually increases, up to 0.1 MPa. The absorption tower was then discharged, and dried at a pressure of -0.08 MPa and 70°C for 0.5 hours to obtain 1245.7 g of glyphosate dimethylamine salt with a content of 95.9% and a yield of 99.4%.

Example Embodiment

[0037] Example 3

[0038] Put 1000 g of glyphosate technical material (content 95%) into the kneader, add 100 g of water at 80°C and mix evenly, add 253 g of pure liquid dimethylamine (content 99.9%) dropwise under sealed conditions, The dropwise addition time is 1 h. Due to the gasification of dimethylamine and the increase of temperature, the reaction pressure gradually increases, up to 0.1 MPa. The absorption tower was then discharged, and dried at a pressure of -0.08 MPa and 80°C for 1 hour to obtain 1244.7 g of glyphosate dimethylamine salt with a content of 95.8% and a yield of 99.3%.

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Abstract

The invention discloses a preparation method for a glyphosate dimethylamine salt active compound. The method comprises the following steps: adding a glyphosate solid into a reactor; dropwise adding liquid dimethylamine into glyphosate under a sealed condition; continuously reacting after dropwise adding to obtain glyphosate dimethylamine salt. The liquid dimethylamine is taken as a raw material, the dimethylamine is added dropwise rather than be added at a time, the pressure in the reaction is lowered greatly, and the airtightness requirement of equipment is lower; in the dropwise adding process, the temperature does not need to be kept constant and is easy to control, and high operability is achieved; the preparation method has the advantages of no need of any organic solvent, simple process, adoption of readily-available raw materials, continuous production, no three-waste discharge, low equipment requirement, low production energy consumption, high safety, high environmental friendliness, high production efficiency, high product quality and high application value.

Description

technical field [0001] The invention relates to a preparation method of glyphosate dimethylamine salt technical, in particular to a simple and environment-friendly preparation method of glyphosate dimethylamine salt technical field, which belongs to the technical field of pesticide chemical industry. Background technique [0002] Glyphosate is a herbicide developed by the Monsanto Company of the United States, also known as glyphosate, roundup, glyphosate, and phosphonic acid. Its pure product is a non-volatile white solid that melts at about 230°C and Accompanied by decomposition, non-flammable, non-explosive, stable at room temperature storage. The solubility of glyphosate in water at 25°C is 1.2%, and it is insoluble in general organic solvents, but its ammonium salt, potassium salt, sodium salt, dimethylamine salt, and isopropylamine salt have relatively high solubility, so its soluble salt It is a commonly used form of pharmaceutical active ingredients. [0003] Glyph...

Claims

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Application Information

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IPC IPC(8): C07F9/38
CPCC07F9/3813
Inventor 孙国庆侯永生吴勇曹月辉孙鹏
Owner SHANDONG RUNBO BIOTECH CO LTD
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