Preparation method of N-(phosphonomethyl) iminodiacetic acid

A technology of bisphosphonate and monosodium iminodiacetate, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. Reaction and other problems, to achieve the effect of reducing sodium chloride, reducing sodium chloride content and improving reaction yield

Inactive Publication Date: 2014-03-05
CHONGQING UNISPLENDOUR CHEM
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Problems solved by technology

If sodium chloride is precipitated in the later stage of the reaction, it will inevitably wrap iminodiacetic acid, which will affect the reaction and reduce the yield; moreover, when diglyphosate is crystallized, it needs to be washed with a large amount of water to remove salt, thus increasing the amount of waste water produced

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  • Preparation method of N-(phosphonomethyl) iminodiacetic acid
  • Preparation method of N-(phosphonomethyl) iminodiacetic acid
  • Preparation method of N-(phosphonomethyl) iminodiacetic acid

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[0029] The embodiment of the present invention discloses a preparation method of bisglyphosate, comprising the following steps:

[0030] (A) react disodium iminodiacetic acid with hydrochloric acid to obtain a solution containing monosodium iminodiacetic acid and sodium chloride;

[0031] (B) Concentrating the solution containing monosodium iminodiacetic acid and sodium chloride, then heating and filtering to obtain sodium chloride solid and filtrate;

[0032] (C) Mix the filtrate with hydrochloric acid and phosphorous acid, heat, then add formaldehyde, and react to obtain bisglyphosate.

[0033] The invention uses disodium iminodiacetate as a starting material to prepare diglyphosate. The source of the disodium iminodiacetate is not particularly limited, and it can be obtained commercially or preferably obtained by hydrolysis of iminodiacetonitrile or oxidation of diethanolamine. The method for obtaining disodium iminodiacetonitrile by hydrolyzing iminodiacetonitrile is as ...

Embodiment 1

[0043] Put 179.6g (0.45mol) of 44.5% iminodiacetic acid disodium salt produced after dehydrogenation of diethanolamine into a four-neck flask, heat to 70°C to dissolve, and add 31% hydrochloric acid dropwise under stirring to neutralize to the pH value 5.0, concentrated under reduced pressure to distill 90g of water, raised the temperature to 80°C and filtered while hot, washed the filter cake with 20mL of hot water, dried to obtain 14.3g of solid, of which the mass content of iminodiacetic acid monosodium salt was 0.10%, and the rest was chlorinated sodium.

[0044] The filtrate was transferred to a four-necked bottle equipped with a reflux condenser, a thermometer, an agitator, and a constant pressure dropping funnel, and 45.7 g of phosphorous acid (97% by mass, 0.54mol), 111.9 g of hydrochloric acid (97% by mass) were added. 31%, 0.95mol), temperature control between 115-120℃, add 47.0g formaldehyde (content 37%, 0.58mol) dropwise, keep warm for 2h after adding, cool down t...

Embodiment 2

[0048]Put 426.5 g (content 41.5%, 1 mol) of iminodiacetonitrile disodium salt generated after hydrolysis of iminodiacetonitrile sodium hydroxide solution into a four-neck flask, heat to dissolve, and add 36% hydrochloric acid dropwise under stirring conditions to neutralize to The pH value is 5.2, concentrated under reduced pressure to distill 250g of water, heated to 85°C and filtered while hot, the filter cake was washed with 20mL of hot water, and dried to obtain 19.8g of solid, of which the mass content of iminodiacetic acid monosodium salt was 0.11%, and the rest was Sodium chloride.

[0049] The filtrate was transferred to a four-necked bottle equipped with a reflux condenser, a thermometer, an agitator, and a constant pressure dropping funnel, and 97.2 g of phosphorous acid (97% by mass, 1.15mol), 294.5 g of hydrochloric acid (31% by mass) were added. , 2.15mol), add 105.4g formaldehyde dropwise between 115-120°C (content 37%, 1.3mol) and keep warm for 2h, cool down to ...

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Abstract

The invention provides a preparation method of N-(phosphonomethyl) iminodiacetic acid. The preparation method comprises the steps of enabling disodium iminodiacetate to react with hydrochloric acid to obtain a solution containing monosodium iminodiacetate and sodium chloride; concentrating the solution containing monosodium iminodiacetate and sodium chloride, heating and filtering to obtain a sodium chloride solid and filtrate; mixing the filtrate with hydrochloric acid and phosphorous acid, heating, then adding formaldehyde and reacting to obtain N-(phosphonomethyl) iminodiacetic acid. As monosodium iminodiacetate has relatively large solubility in water and the changes in solubility of sodium chloride along with the temperature are not obvious, sodium chloride obtained by acidification of disodium iminodiacetate by hydrochloric acid is firstly separated, so that the content of sodium chloride is reduced, the precipitation of sodium chloride in the subsequent reaction is avoided, and the reaction yield is improved; meanwhile, the viscosity of raw materials is reduced, so that the mixing of the raw materials becomes more uniform. Secondary, as sodium chloride in the system is reduced, wastewater produced by washing during separation of N-(phosphonomethyl) iminodiacetic acid is reduced. Experimental results show that the yield of N-(phosphonomethyl) iminodiacetic acid prepared by the method provided by the invention can be up to above 93%.

Description

technical field [0001] The invention relates to the field of diglyphosate production, in particular to a preparation method of diglyphosate. Background technique [0002] Diglyphosate (N-phosphoromethyliminodiacetic acid) is a precursor used to synthesize glyphosate, and is also the main raw material for the production of broad-spectrum destructive post-emergence herbicides. Its formula for synthesizing glyphosate is: [0003] [0004] The one-pot method for preparing bisglyphosate is usually divided into two types: neutralization with hydrochloric acid and neutralization with phosphorus trichloride. [0005] Among them, the hydrochloric acid neutralization method is specifically as follows: first, neutralize iminodiacetic acid disodium salt with hydrochloric acid to generate iminodiacetic acid; iminodiacetic acid is mixed with phosphorous acid and hydrochloric acid, heated, and then formaldehyde is added dropwise for condensation reaction to obtain bisaminodiacetic acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 丁永良张飞吴传隆刘佳屈洋李静游欢何咏梅李双龙程益刘欢
Owner CHONGQING UNISPLENDOUR CHEM
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