Method and device for producing N-phosphono methyl glycine

A technology of phosphonomethylglycine and production method, applied in the field of N-phosphonomethyliminodiacetic acid, can solve the problems of affecting the productivity of equipment, blockage of fixed bed, poor heat transfer effect of fixed bed and the like

Active Publication Date: 2013-06-26
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is deficiency in this method equally, at first, 1) when using fixed bed as continuous reactor, catalyst is piled up in fixed bed, and after oxygen enters fixed bed, forms big bubble to occupy catalyst surface space, causes diglyphosate feed liquid in catalyst The uneven distribution on the surface results in incomplete conversion of diglyphosate or increased side reactions; 2) the heat transfer effect of the fixed bed is poor, and the heat released during the catalytic oxidation of diglyphosate is difficult to transfer in time, so the temperature is too high and there are by-products The generation of aminomethyl phosphoric acid reduces the reaction yield
3) There is a requirement for the particle size of the carbon catalyst supported in the fixed bed reactor, and the carbon catalyst with small particles will generate a large pressure drop, which will eventually lead to the blockage of the fixed bed
However, after choosing a carbon catalyst with large particles, its catalytic efficiency will decrease, and the cost of the catalyst will be higher; 4) due to the short service life of the carbon catalyst used, usually within 20 days, large-scale production equipment adopts fixed-bed reactors. , the filling and unloading of the catalyst is heavy, and the production equipment needs to be shut down, which affects the production capacity of the equipment

Method used

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  • Method and device for producing N-phosphono methyl glycine
  • Method and device for producing N-phosphono methyl glycine
  • Method and device for producing N-phosphono methyl glycine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Under the temperature of 100~110 ℃ and the pressure of 0.1~0.5MPa, put 98% PMIDA and deionized water into the feed mixer according to a certain proportion and be mixed with the aqueous solution of 3% bisglyphosate in concentration by weight, Squeeze into the tubular reactor that 3Kg gac catalyst is housed after metering with pump then. Pure oxygen gas was metered into the tubular reactor at a rate of 7.3 g / min. The reactor pressure was maintained at about 0.3 MPa. Experiments were performed at various temperatures and liquid feed rates. The reaction results are shown in Table 1.

[0063] Table 1

[0064]

Embodiment 2

[0066] Example 2-1, Step 1: Repeat the operation in Example 1, other operating conditions remain unchanged, inject the diglyphosate aqueous solution into the tubular reactor at a liquid feed rate of 430 g / min. The reaction temperature was maintained at about 110°C. Step 2: The obtained glyphosate feed liquid is discharged and concentrated in the concentration tank. The processed feed liquid is fully crystallized, filtered and separated, and the filtrate is the glyphosate mother liquid, weighing 184Kg. After recovery, it is recycled to the concentration section, wet After drying the powder, glyphosate crystals were obtained, weighing 16Kg, with a measured content of 97.5% and a yield of 85%.

[0067] Example 2-2, repeat the operation in Example 2-1, after the glyphosate feed liquid obtained in step 2 is discharged into the concentration tank, add the glyphosate mother liquor obtained in Example 2-1 together to concentrate in the concentration tank , the treated feed liquid is ...

Embodiment 3

[0070] Under the temperature of 120~140 ℃ and the pressure of 0.2~0.4MPa, put 98% PMIDA and deionized water into the feed mixer according to a certain proportion and be mixed with the aqueous solution of 6% diglyphosate in weight percent concentration, Then push into the tubular reactor that 4.5Kg activated carbon catalyst is housed after metering with a pump. Pure oxygen gas was metered into the tubular reactor at a rate of 6.4 g / min. The reactor pressure was maintained at about 0.5 MPa. Experiments were performed at various temperatures and liquid feed rates. The reaction results are shown in Table 2.

[0071] Table 2

[0072]

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Abstract

The invention relates to a method for continuously producing N-phosphono methyl glycine. The method comprises the following steps of: inputting reaction feed liquor into a reactor under the condition of oxidizing PMIDA into glyphosate to make an activated carbon catalyst suspend in the reaction feed liquor in the reactor; fully contacting the PMIDA with molecular oxygen; continuously oxidizing the PMIDA into the glyphosate under a selected reaction condition; and performing a PMIDA oxidizing reaction. The invention also relates to a device for continuously producing the N-phosphono methyl glycine. The device mainly comprises a power generator, a tubular reactor and a gas-liquid separator. The device is characterized in that: the power generator is connected with the bottom of the tubular reactor through a pipeline; the gas-liquid separator is connected with the top of the tubular reactor; the lower part of the tubular reactor is provided with an oxygen containing gas feed tube orificeand is connected with a gas distributor in the tube; and the power generator is connected with a feed tube of the PMIDA feed liquor and catalyst activated carbon or a feed tube of the mixed liquor ofthe PMIDA feed liquor and catalyst activated carbon through pipelines.

Description

technical field [0001] The present invention relates to a method and device for preparing glyphosate by catalytic oxidation continuous reaction of N-phosphonomethyliminodiacetic acid, i.e., bisglyphosate (PMIDA), which belongs to N-phosphonomethylglycine, i.e. grass The field of preparation of glycine (PMG). Background technique [0002] Glyphosate is a systemic conductive broad-spectrum herbicide with the advantages of high efficiency, broad-spectrum, low toxicity and no residue. In recent years, due to the expansion of global planting of genetically modified crops, the recovery and modernization of global agriculture, especially in developing countries, and the production of renewable energy, the market demand for glyphosate has grown rapidly, and the sales volume has increased by nearly 15% per year. , has occupied the first place in the world's pesticide sales for many years, and has become the fastest growing pesticide variety. [0003] There are currently two product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38B01J21/18A01N57/20A01P13/00
Inventor 王伟任不凡周曙光吴嘉陈静屠民海林少耕杨旭张海良叶志凤韩鑫
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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