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Method for preparing glyphosate by continuous oxidation

A glyphosate and oxygen technology, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve problems such as many side reactions, and achieve the effects of short reaction time, high purity, and uniform internal mass transfer.

Active Publication Date: 2019-11-12
NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The invention overcomes the disadvantages of many side reactions in the existing process, and provides a method for preparing glyphosate by oxidation with less reaction impurities and continuous reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1, adopt microchannel reactor to prepare glyphosate, this scheme comprises batching operation, microchannel reaction procedure and crystallization powder-taking operation; The microchannel reactor that adopts in the microchannel reaction procedure has preheating module, reaction module, reacts The module has a slurry inlet, an oxygen inlet and a reaction product outlet;

[0031] (1) Batching process: at a certain temperature, mix bisglyphosate with batching water and catalyst evenly, so that the solid is suspended in the solution to form a slurry.

[0032] (2) Microchannel reaction process: The slurry prepared in (1) enters the preheating module of the microchannel reactor through the slurry metering pump, and the preheated material enters the reaction module through the slurry inlet. Oxygen is input into the oxygen inlet, and the reaction pressure in the reaction module is 1.2~1.5Mpa. The reaction liquid is discharged from the reaction product outlet after b...

Embodiment 2

[0036] The three procedures in Example 1 were used.

[0037] Then, weigh 233.0 g of bisglyphosate solid, 45.0 g of activated carbon catalyst, and 4382 g of batching water, stir, heat up to 70° C., and mix uniformly to form a raw material slurry. A diaphragm pump is used to beat the slurry into a group of preheating modules of the microchannel reactor at a speed of 40 g / min, and the slurry is weighed with a balance. The preheated material enters the reaction module. Oxygen and slurry are fed at the same time, the intake speed is set to 113ml / min, and the temperature of the reaction module is set to 90°C. After passing through 6 reaction modules, the liquid phase is collected by the gas-liquid separator, and the clear liquid is obtained by heat preservation and filtration, and the temperature is crystallized. , filtered to obtain glyphosate solid 163.7g, content 98.7%, yield 96.1%.

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Abstract

The invention discloses a method for preparing glyphosate by continuous oxidation. According to a scheme of the invention, the method adopts a microchannel reactor to prepare the glyphosate, and comprises a batching procedure, a microchannel reaction procedure and a crystallization powder preparation procedure. In the microchannel reaction procedure, the feeding speed of oxygen is changed from high to low; a temperature is stabilized at 60 DEG C and then raised to 90 DEG C; and a pressure is changed from positive pressure to negative pressure. The method provided by the invention adopts the microchannel reactor for a reaction; a glyphosate product obtained by using the method provided by the invention has high purity and high yield; and the method can realize precise feeding, has short reaction time, and generates few side reactions.

Description

technical field [0001] The invention relates to a synthesis method of glyphosate herbicide. Background technique [0002] Glyphosate (N-phosphonomethylglycine) is a herbicide with low toxicity, high efficiency and systemic conductivity. It has been popular all over the world since the 1980s, especially in transgenic glyphosate-resistant crops. One of the most widely used herbicides at present. Its production process mainly includes glycine method and iminodiacetic acid method (IDAN method). The key step of the IDAN method is the oxidation of diglyphosate to glyphosate. [0003] In the traditional tank-type process, the material in the reactor is a solid-liquid-gas three-phase reaction. Due to the large volume and poor stirring effect, it is necessary to increase the conversion rate of diglyphosate by prolonging the reaction time. This makes the glyphosate generated in the reaction process inevitably have side reactions. First, glyphosate will continue to react with exces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38B01J19/00
CPCB01J19/0093C07F9/3813
Inventor 董垒杜辉沈书群孙亚峰孙春楼徐伟
Owner NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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