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Clean production method for preparing N-(phosphonomethyl)iminodiacetic acid

A technology of clean production and diglyphosate, which is applied in the chemical industry, can solve the problems of no mention of diglyphosate wastewater treatment methods, no good wastewater treatment methods, etc., and achieve the effects of reducing hydrolysis costs, simple composition, and low salt content

Active Publication Date: 2011-10-05
SHANDONG WEIFANG RAINBOW CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Above-mentioned technique consumes a large amount of alkali or acid, (the mol ratio of consumption liquid caustic soda or hydrochloric acid amount and iminodiacetonitrile is 2.1-2.3: 1) a lot of waste water (mainly being the waste water containing diglyphosate, 1 ton of bisglyphosate produces about 5 tons of high-salt wastewater), especially for the process of alkaline hydrolysis of iminodiacetonitrile, there is currently no good wastewater treatment method
[0005] Patents CN101392276A, CN101429532A introduce the method of utilizing biological enzymes to catalyze the production of iminodiacetic acid solution, but it only obtains a solution with the highest IDA content of 7%, such a low-concentration solution cannot be directly used in the synthesis of diglyphosate. It did not mention the treatment method of the wastewater generated in the production process of bisglyphosate

Method used

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  • Clean production method for preparing N-(phosphonomethyl)iminodiacetic acid
  • Clean production method for preparing N-(phosphonomethyl)iminodiacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Those skilled in the art know that there are many kinds of enzymes that can make nitrile hydrolysis, and the enzymes used in the following examples here are genetically engineered Escherichia coli BL21 (DE3) / Pet-NiT (LuoHui, et al.Appl Biochem Biotechnol.DOI10.1007 / s12010-008-8324-y).

[0025] enzyme cell culture

[0026] Medium:

[0027] 1# medium composition: tryptone 1%, yeast powder 0.5%, sodium chloride 1%, glycerol 0.3%, 20mM lactose, kanamycin 50uM / L, PH7.0

[0028] 2# medium composition: 5% corn steep liquor, 0.017M KH 2 PO 4 , 0.07M K 2 HPO 4 , 0.4% glucose, 20mM lactose, 50uM / L kanamycin, pH7.5

[0029] nourish:

[0030] In medium 1#, 35°C, 180r / min, cultivate genetically engineered Escherichia coli BL21(DE3) / Pet-NiT for 12h, inoculate 5% inoculum into medium 2#, 30°C, 200r / min , cultivated for 14h.

[0031] Collect bacteria:

[0032] 10000r / min, centrifuge for 5min, and harvest the bacteria.

[0033] Immobilized enzyme preparation:

[0034] First...

Embodiment 2

[0039] Nitrilase was immobilized on the carrier obtained by mixing sodium periodate and starch, then added to the evaporated solution in Example 1, and added water to 1450 g. Slowly add iminodiacetonitrile between PH6-9 at 35°C to maintain the concentration of diacetonitrile. After 14 hours of dosing, stop the dosing and add 100 g of iminodiacetonitrile (92%) in total, (during which it is used to adjust the pH Consume liquid caustic soda 27g) filter after insulation 1h, get filtrate 1531.8g, IDA content 8.24%, get the diglyphosate mother liquor 300g among the embodiment 1 and mix with filtrate after adjusting pH to 6-7 with 7g tablet alkali. Then carry out membrane concentration to obtain concentrated solution 790.4g, concentrated solution is evaporated again, take embodiment 1 middle membrane concentrated light solution 300g absorb ammonia gas, obtain concentrated solution 489.3g, IDA content 26.13%. Get the concentrated solution and add 152g (99%) phosphorus trichloride drop...

Embodiment 3

[0041]Take the immobilized enzyme filtered in Example 1 and add some unused immobilized enzyme, dissolve in the aqueous solution of pH=7, a total of 1100g, the enzyme cell concentration is 40g / L. Slowly add iminodiacetonitrile at 40°C, pH 6-9, maintain the concentration of diacetonitrile at 0.05mol / L-0.1mol / L, stop adding after 18 hours of reaction, and add iminodiacetonitrile (92%) 100g, (during this period, 22g of liquid caustic soda is used for adjusting PH) is incubated for 1h and then filtered to obtain 1198.3g of filtrate with an IDA content of 10.51%. After evaporation, 435.3 g of concentrated liquid was obtained, and 263.6 g of evaporated liquid was obtained. Take the concentrated solution and add 155g (99%) phosphorus trichloride dropwise in a 1000ml flask, then raise the temperature and add dropwise 101.9g (37%) formaldehyde, after the reaction is completed, 140g of deacidification, add 62g of liquid caustic soda (32%) to adjust the pH, and filter with suction , 100...

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Abstract

The invention relates to a clean production method for preparing N-(phosphonomethyl)iminodiacetic acid, comprising the following steps: first using nitrilase to catalytically hydrolyze iminodiacetonitrile to obtain low concentration solution of iminodiacetic acid, and using the nitrilase indiscriminately; carrying out film condensation and multi-effect evaporation on the low concentration iminodiacetic acid solution to obtain iminodiacetic acid feed liquid with content between 25% and 35%; and reacting the feed liquid with a hydrochloric acid source, a phosphorous acid source and methanol to obtain N-(phosphonomethyl)iminodiacetic acid wet feed and mother liquid. Thin liquid after film condensation is used for absorbing ammonia overflowing during multi-effect evaporation. Evaporated liquid obtained through multi-effect evaporation is reused for enzymolysis of the iminodiacetonitrile, and partial N-(phosphonomethyl)iminodiacetic acid mother liquid is mixed with the low concentration iminodiacetic acid solution and is used in the next N-(phosphonomethyl)iminodiacetic acid synthesis indiscriminately through concentration and recovery. The process greatly reduces the consumption of hydrochloric acid and liquid alkali, simultaneously improves the yield of N-(phosphonomethyl)iminodiacetic acid by about 1-2% and reduces the wastewater.

Description

technical field [0001] The invention relates to a clean production method for preparing diglyphosate, which belongs to the technical field of chemical industry. Background technique [0002] Glyphosate (glyphosate, N-phosphonomethylglycine) is a destructive organophosphine herbicide commercialized by Monsanto in 1974. Because of its excellent herbicidal performance, coupled with the widespread planting of glyphosate-resistant transgenic crops, glyphosate has become the world's largest herbicide in sales. [0003] The synthesis techniques of domestic glyphosate mainly include glycine method (Gly method) and iminodiacetic acid method (IDA method). Among them, the IDA method was developed in the late 1990s and realized industrial production. This process mainly uses the iminodiacetonitrile method (IDAN) in China. Due to the advantages of cheap and easy-to-obtain raw materials such as iminodiacetonitrile, good catalyst selectivity and higher yield for glyphosate oxidation, the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C12P13/00C07F9/38
Inventor 孙国庆陈琦陈桂元侯永生
Owner SHANDONG WEIFANG RAINBOW CHEM