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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0018] Example 1 640g IDA disodium salt was added to a 1L flask equipped with a stirrer, and 166g of sulfuric acid with a mass percentage concentration of 50% was added dropwise, and 802g IDA sodium salt solution was obtained by filtration, and the IDA mass percentage concentration was 25.54%.

[0019] Add 802g of the IDA sodium salt solution prepared in the above steps into a 1L flask equipped with reflux device and stirring. Add 165g sulfuric acid with a mass percentage concentration of 50% within 1 hour, keep it for 2 hours, control the temperature at 34°C, and filter and separate , Drying to obtain 186g solid IDA (IDA mass percentage concentration is 95.20%, the yield from IDA monosodium salt solution to solid IDA is 86.45%) and 750g mother liquor, the mother liquor is added with a mass percentage concentration of 32% liquid caustic soda 65g for neutralization , Concentrated to remove 170g of water, cooled and crystallized, filtered and separated at 2℃ to obtain 520g of Na 2 S...

Example Embodiment

[0021]Example 2 640g IDA disodium salt was added to a 1L flask equipped with a stirrer, and 166g of sulfuric acid with a mass percentage concentration of 50% was added dropwise to obtain 799g of an IDA sodium salt solution with a mass percentage concentration of 25.63%.

[0022] Add 799g of IDA monosodium salt solution prepared in the above steps and 121g of IDA concentrated mother liquor prepared in Example 1 into a 1L flask equipped with a reflux device and stirring. Add 190g of sulfuric acid with a mass percentage concentration of 50% in 1 hour, and keep crystallizing. For 2 hours, control the temperature at 36°C, filter and dry to obtain 205g solid IDA (IDA mass percentage concentration is 96.58%, the yield from IDA sodium salt solution to solid IDA is 96.68%) and 875g mother liquor. The mother liquor is added with a mass percentage concentration of 80g of 32% liquid caustic soda is neutralized, 220g of water is removed by concentration, cooled and crystallized, filtered and s...

Example Embodiment

[0024] Example 3 640g IDA disodium salt was added to a 1L flask equipped with stirring, and 166g of sulfuric acid with a mass percentage concentration of 50% was added dropwise, and 800g of IDA sodium salt solution was obtained by filtration, and the IDA mass percentage concentration was 25.58%.

[0025] Add 800g of IDA monosodium salt solution prepared in the above steps and 150g of IDA concentrated mother liquor prepared in Example 2 into a 1L flask equipped with reflux device and stirring. Add 190g of sulfuric acid with a mass percentage concentration of 50% in 1 hour, and keep crystallizing. For 2 hours, control the temperature at 38°C, filter and dry to obtain 208g solid IDA (IDA mass percentage concentration is 95.08%, the yield from IDA monosodium salt solution to solid IDA is 96.64%) and 921g mother liquor, the mother liquor plus 80g mass percentage concentration Neutralize with 32% liquid caustic soda, concentrate to remove 270g of water, cool down and crystallize, filter...

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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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