Method for preparing glyphosate by PMIDA catalytic oxidation

A technology of catalytic oxidation and glyphosate, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of inconvenient production operation, difficult post-processing, difficult preparation, etc., to improve the utilization rate of oxygen , Product quality is stable, and the effect of accelerating the reaction rate

Active Publication Date: 2011-09-21
SHANDONG WEIFANG RAINBOW CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of the catalyst is relatively complicated, the cost is high, and it is difficult to prevent the loss of the catalyst and precious metals during the production process.
[0005] CN101386627A discloses the method for preparing glyphosate by oxidizing diglyphosate with molecular oxygen-containing gas and dilute nitric acid under the catalytic condition of active carbon loaded with transition metal or its salt. The method has low production cost and stable product quality, but the production Nitric acid is used in raw materials, which brings inconvenience to production
[0006] As can be seen from the above, these methods are either low in production efficiency, difficult to carry out after-treatment, or inconvenient in production operation, or unstable in production quality, or high in cost, and the catalyst containing precious metals is not easy to prepare

Method used

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  • Method for preparing glyphosate by PMIDA catalytic oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation method of 5A molecular sieve loaded with nanometer nickel oxide:

[0023] Grind 200g of 5A molecular sieve with a mortar and sieve, take 40g of 20-100 mesh molecular sieve, add it to the mixed solution of 70g NiSO4 6H2O and 50g 30% NaOH and reflux for 2h, at a stirring speed of 300r / min at 30℃ Evaporate to dryness, wash with deionized water until neutral, dry and age in an oven at 100 °C for 15 hours, then put the sample in a muffle furnace at 450 °C for 3 hours, press into tablets and pulverize, take 40-70 mesh The sample acts as a co-oxidant.

Embodiment 2

[0025] The preparation method of 5A molecular sieve loaded with nanometer nickel oxide doped with manganese dioxide:

[0026] The 5A molecular sieve of 200g is ground and sieved with a mortar, take 40g of molecular sieve of 20-100 mesh, add 81gMn (NO 3 ) 2 , 119g NiSO4 6H2O and 80g 30% NaOH mixture were refluxed for 4h, evaporated to dryness at 60°C at a stirring speed of 300r / min, washed with deionized water until neutral, dried and aged in an oven at 110°C for 18h, and then The samples were placed in a muffle furnace and calcined at 500 °C for 5 hours. After tableting, they were pulverized. A 40-70 mesh sample was taken as a co-oxidant.

Embodiment 3

[0028] Preparation method of 5A molecular sieve loaded with nanometer nickel oxide:

[0029] Grind 200g of 5A molecular sieve with a mortar and sieve, take 40g of molecular sieve of 20-100 mesh, add it to the mixed solution of 50g NiSO4 6H2O and 120g 30% NaOH and reflux for 3h, at a stirring speed of 300r / min at 50℃ Evaporate to dryness, wash with deionized water until neutral, dry and age in an oven at 115 °C for 19 hours, then put the sample in a muffle furnace at 450 °C for 4 hours, press into tablets and pulverize, take 40-70 mesh The sample acts as a co-oxidant.

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Abstract

The invention discloses a method for preparing glyphosate by PMIDA catalytic oxidation, comprising the following steps: 100-110 parts of PMIDA, 5-12 parts of activated carbon and 0.25-1.80 parts of pro-oxidants are added in 300 parts of water by mass part, the mixture is stirred, and then oxygen-containing gas with 70-100 percent of oxygen mass fraction is vented to the mixture to carry out catalytic oxidation reaction, the reaction temperature is 50-100 DEG C, the reaction pressure is 0.5-2.0MPa and the reaction time is 1-2h; after the reaction is finished, the solution is cooled and filtered to obtain filtrated mother liquid and a filter cake 1, the filtrated mother liquid is utilized in a circulating way, the filter cake 1 is hot-melted after water is added and then is filtered to obtain hot filtrate and a filter cake 2, the hot filtrate is cooled and crystallized to obtain solid glyphosate, and the filter cake 2 is recycled and used repeatedly. The method has stable product quality, can greatly improve utilization rate of oxygen and speed up the reaction rate; the production cost is low, formaldehyde can be effectively degraded, thereby meeting the industrial production requirements.

Description

technical field [0001] The invention relates to a method for preparing glyphosate, in particular to a method using glyphosate as a raw material, using a specific activated carbon as a catalyst, using a gas containing molecular oxygen as an oxidant, and using a nanometer nickel oxide supported or doped with dioxide Method for preparing glyphosate using manganese nanometer nickel oxide and 5A molecular sieve as prooxidant. technical background [0002] The chemical name of glyphosate is N-phosphonomethylglycine (PMG), which is an efficient, broad-spectrum, low-toxicity and safe organic phosphine post-emergent herbicide. It is one of the most widely used herbicides. There are two main glyphosate production processes for industrialization. One is the IDA route developed by Monsanto Corporation in the United States with hydrocyanic acid or diethanolamine as the starting material; Dialkyl phosphate route. The air oxidation method of glyphosate has been proposed as an advanced lo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38B01J21/18
Inventor 李志清孙国庆袁良国陈琦赵广理朱红涛王之波
Owner SHANDONG WEIFANG RAINBOW CHEM
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