Preparing method for glyphosate

A technology of glyphosate and glyphosate, applied in the chemical industry, can solve the problems of complexity, high energy consumption, difficult disposal of by-products and mother liquor, etc., and achieve the effects of changing electron distribution, improving catalytic activity, and low formaldehyde content

Active Publication Date: 2016-08-03
ANHUI YINONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the glycine method is the mainstream method for preparing glyphosate in China, but the glycine method uses glycine as a raw material to prepare glyphosate through reaction. This process equipment is relatively complicated, energy consumption is also high, and by-products and mother liquor are difficult to handle.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method of glyphosate includes the following steps:

[0022] (1) Synthesis of iminodiacetic acid: reacting hydrocyanic acid, formaldehyde and hexamethylenetetraammonium under the action of oxygen for 10h at a temperature of 40℃ to obtain iminodiacetonitrile, and then iminodiacetonitrile Prepare iminodiacetic acid by hydrolysis and acidification;

[0023] (2) Preparation of Glyphosate: react iminodiacetic acid, formaldehyde and phosphorus trichloride at 50°C for 2h to obtain Glyphosate;

[0024] (3) Preparation of glyphosate: add the glyphosate prepared in step (2) into the reaction kettle, pass an oxygen flow into the reaction kettle at a flow rate of 2L / min, and add activated carbon supported titanium dioxide catalyst and water in the reaction kettle Set the visible light source to irradiate, gradually heat the reactor to 80°C, stir, the reaction pressure in the reactor is 0.2~0.4MPa, and react for 3h;

[0025] Among them, the specific surface area of ​​the origi...

Embodiment 2

[0029] A preparation method of glyphosate includes the following steps:

[0030] (1) Synthesis of iminodiacetic acid: reacting hydrocyanic acid, formaldehyde and hexamethylenetetraammonium under the action of oxygen for 12h at a temperature of 45℃ to obtain iminodiacetonitrile, and then iminodiacetonitrile Prepare iminodiacetic acid by hydrolysis and acidification;

[0031] (2) Preparation of Glyphosate: react iminodiacetic acid, formaldehyde and phosphorus trichloride at 55°C for 3 hours to obtain Glyphosate;

[0032] (3) Preparation of glyphosate: add the glyphosate prepared in step (2) into the reactor, and pass an oxygen flow into the reactor at a flow rate of 1.8L / min, and add activated carbon-supported titanium dioxide catalyst and water to the reactor. Set visible light source to irradiate, gradually heat the reactor to 80°C, stir, the reaction pressure in the reactor is 0.2~0.4MPa, and react for 3h;

[0033] Among them, the specific surface area of ​​the original activated ca...

Embodiment 3

[0037] A preparation method of glyphosate includes the following steps:

[0038] (1) Synthesis of iminodiacetic acid: reacting hydrocyanic acid, formaldehyde and hexamethylenetetraammonium under the action of air for 8h at a temperature of 50℃ to obtain iminodiacetonitrile, and then iminodiacetonitrile Prepare iminodiacetic acid by hydrolysis and acidification;

[0039] (2) Preparation of Glyphosate: react iminodiacetic acid, formaldehyde and phosphorus trichloride at 45°C for 2 hours to prepare Glyphosate;

[0040] (3) Preparation of glyphosate: add the glyphosate prepared in step (2) into the reactor, and pass an oxygen flow into the reactor at a flow rate of 2.3 L / min, and add activated carbon-supported titanium dioxide catalyst and water to the reactor. Set visible light source to irradiate, gradually heat the reactor to 80°C, stir, the reaction pressure in the reactor is 0.2~0.4MPa, and react for 4h;

[0041] Among them, the specific surface area of ​​the original activated carb...

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Abstract

The invention relates to a preparing method for glyphosate and belongs to the technical field of chemical engineering. The preparing method specifically comprises the four steps of synthesis of iminodiacetic acid, preparation of pmida, preparation of glyphosate and solid and liquid separation. According to the preparing method, firstly, precious metal silver is loaded on titanium dioxide, the surface nature of titanium dioxide is influenced, electron distribution is changed, and catalytic activity is improved; then, titanium dioxide loaded with silver is loaded into activated carbon and irradiated with an ultraviolet source. The selectivity of glyphosate is greatly improved, the oxidization process of pmida is greatly shortened, the yield of glyphosate is increased to 96.3%, and the product purity can reach 97.6%; besides, the content of methyl aldehyde is low, fewer products are generated, and the requirement of the nation for environment friendliness is met.

Description

Technical field [0001] The invention belongs to the technical field of chemical engineering, and specifically relates to a preparation method of glyphosate. Background technique [0002] Glyphosate is a highly effective and low-toxic post-emergence herbicide, and it is currently the largest herbicide in China. The herbicidal mechanism of glyphosate is to kill weeds through systemic conduction, so it is non-toxic and harmless to humans and animals. In addition, glyphosate is easily degraded by microorganisms after entering the soil, and will not pollute the soil and groundwater. Therefore, glyphosate is an efficient, broad-spectrum, low-toxic and environmentally friendly biocidal herbicide. Based on the above many advantages, glyphosate has been widely promoted and used once it came out, especially the large-scale planting of genetically modified crops, which has made the global demand for glyphosate continue to grow. [0003] There are currently two main industrial production met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
CPCC07F9/3813
Inventor 徐益峰方冉
Owner ANHUI YINONG CHEM
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