Production method of N-phosphono methyliminodiacetic acid

A technology of phosphonomethyliminodiacetic acid and iminodiacetic acid, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. , many pollutants, etc., to achieve the effect of improving yield, reducing energy consumption, and reducing the discharge of three wastes

Inactive Publication Date: 2008-10-15
捷马化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above methods, at the end of the reaction, it is necessary to add alkali (preferably NaOH) to neutralize or dehydrate to separate out diglyphosate, and then separate and wash to obtain the finished product, which has the disadvantages of large alkali consumption, many pollutants, large amount of waste water and biochemical Poor performance and other disadvantages; and the composition of the reaction mother liquor is complex, containing a large amount of useful components such as inorganic acids, salts, formaldehyde, residual bis-glyphosate, IDA, etc. are not separated and recycled, and the number of times the mother liquor is recycled or even cannot be applied mechanically
These deficiencies make the production of bisglyphosate face more and more serious environmental protection problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1 In a 1L flask equipped with stirring, add 640g of IDA disodium salt, add dropwise a mass percentage concentration of 50% sulfuric acid 166g, and filter to obtain 802g of IDA monosodium salt solution, with an IDA mass percentage concentration of 25.54%.

[0019] Add 802g of the IDA-sodium salt solution prepared in the above steps to a 1L flask equipped with a reflux device and stirring, add dropwise 165g of sulfuric acid with a mass percentage concentration of 50% within 1 hour, keep it warm for 2 hours, control the temperature at 34°C, and filter and separate , dry to get 186g solid IDA (IDA mass percent concentration is 95.20%, is 86.45% from IDA-sodium salt solution to solid IDA yield) and 750g mother liquor, and mother liquor adds mass percent concentration and is that 32% liquid caustic soda 65g is neutralized , Concentrate and remove 170g of water, cool down and crystallize, filter and separate at 2°C to obtain 520g Na 2 SO 4 10H 2 0 and 121g concentrat...

Embodiment 2

[0021]Example 2 In a 1L flask equipped with stirring, add 640g of IDA disodium salt, dropwise add 166g of sulfuric acid with a mass percentage concentration of 50%, and filter to obtain 799g of IDA monosodium salt solution, with an IDA mass percentage concentration of 25.63%.

[0022] In a 1L flask equipped with reflux device and stirring, add 799g of the IDA-sodium salt solution prepared by the above steps and the concentrated mother liquor of 121g of IDA prepared in Example 1, add dropwise 190g of sulfuric acid with a mass percentage concentration of 50% in 1 hour, and insulate and crystallize 2 hours, control temperature 36 ℃, filter, dry to get 205g solid IDA (IDA mass percent concentration is 96.58%, from IDA-sodium salt solution to solid IDA yield is 96.68%) and 875g mother liquor, mother liquor adds mass percent concentration of 80g of 32% liquid caustic soda was neutralized, concentrated to remove 220g of water, cooled and crystallized, filtered and separated at 4°C to ...

Embodiment 3

[0024] Example 3 In a 1L flask equipped with stirring, add 640g of IDA disodium salt, add dropwise a mass percent concentration of 50% sulfuric acid 166g, and filter to obtain 800g of IDA monosodium salt solution, with an IDA mass percent concentration of 25.58%.

[0025] In a 1L flask equipped with reflux device and stirring, add 800g of the IDA-sodium salt solution prepared by the above steps and the concentrated mother liquor of 150g of IDA prepared in Example 2, and add dropwise 190g of sulfuric acid with a mass percentage concentration of 50% in 1 hour, and heat preservation and crystallization 2 hours, control temperature 38 ℃, filter, dry to get 208g solid IDA (IDA mass percent concentration is 95.08%, from IDA-sodium salt solution to solid IDA yield is 96.64%) and 921g mother liquor, mother liquor adds 80g mass percent concentration Neutralize 32% liquid caustic soda, concentrate and remove 270g of water, cool down and crystallize, filter and separate at 6°C to obtain 5...

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PUM

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Abstract

The invention discloses a method for manufacturing N-phosphonomethyliminodiacetic acid (PMIDA). The method comprises the following steps: (1) IDA disodium salt source is reacted with sulphuric acid to obtain IDA monosodium salt solution; (2) the IDA monosodium salt solution is then reacted with sulphuric acid to separate out iminodiacetic acid (IDA), and reaction mother liquor is treated by liquid alkali to obtain Na2SO4 after evaporated dehydration; moreover, the mother liquor is treated as the raw material of the step (2); (3) the IDA is mixed with phosphorous acid and formaldehyde to generate PMIDA through reaction under the condition of sulphuric acid, wherein the PMIDA is obtained through cooling crystallization and filtration after formaldehyde-containing waste water is separated through evaporation; the mother liquor is treated as the raw material of PMIDA; the formaldehyde-containing waste water separates concentrated and reclaimed concentrated formaldehyde through a pervaporation membrane separating device, and the separated concentrated formaldehyde is treated as formaldehyde raw material; and discharged water is used for reclaimed water recovery after resin treatment. The invention reclaims the byproduct of Na2SO4 and makes effective use of resources such as PMIDA, IDA, formaldehyde, sulphuric acid and water in the production waste water of PMIDA.

Description

technical field [0001] The present invention relates to a kind of production method of N-phosphonomethyliminodiacetic acid, more specifically, diglycoside in the waste water produced in the production process of N-phosphonomethyliminodiacetic acid (bisglyphosate) Phosphine, sulfuric acid, formaldehyde, water, incompletely reacted iminodiacetic acid (IDA) and by-product sodium sulfate are recycled. Background technique [0002] Diglyphosate is a precursor to the production of the broad-spectrum herbicide glyphosate. There are three main production methods at present: one is to add phosphorus trichloride dropwise to iminodiacetic acid disodium salt as in the CN1132838C patent, and then react with formaldehyde to generate diglyphosate. The second is to react iminodiacetic acid disodium salt with inorganic acid to directly obtain the intermediate iminodiacetic acid disodium salt inorganic acid salt as in the CN1221557C patent, and then react with phosphorous acid source and for...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 徐国明邱晖刘小华郑端镛刘景伟翁建新吴冬莲王国光雷华军冯琼蕾
Owner 捷马化工股份有限公司
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