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Preparation method of N-(phosphonomethyl) iminodiacetic acid

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

Inactive Publication Date: 2014-03-05
CHONGQING UNISPLENDOUR CHEM
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  • Abstract
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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

Method used

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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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[0030] The embodiment of the present invention discloses a preparation method of bisglyphosate, comprising the following steps:

[0031] (A) react disodium iminodiacetic acid, phosphorus trichloride with water to obtain a solution containing monosodium iminodiacetic acid and sodium chloride;

[0032] (B) Concentrating the solution containing monosodium iminodiacetic acid and sodium chloride, then heating and filtering to obtain sodium chloride solid and filtrate;

[0033] (C) Mix and heat the filtrate with phosphorus trichloride, then add formaldehyde to react to obtain diglyphosate.

[0034] 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 foll...

Embodiment 1

[0046] 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 dropwise 98% phosphorus trichloride (20.8 g) Neutralize to pH 5.0, concentrate under reduced pressure and distill 82g of water, heat up to 80°C and filter while hot, wash the filter cake with 20mL of hot water, and dry to obtain 14.6g of product, wherein the content of iminodiacetic acid monosodium salt is 0.10%, the rest is sodium chloride.

[0047]The filtrate was transferred to a four-necked bottle equipped with a reflux condenser, a thermometer, a stirrer, and a constant pressure dropping funnel, and 109.1 g of phosphorus trichloride was added dropwise, and 47.0 g of formaldehyde (content 37%, 0.58mol) after adding, keep it warm for 2h, cool down to 10°C, keep warm for 2h to crystallize, filter, wash the filter cake with 10mL water, dry to get 97.0g of white solid, content 98.5%, chloride ion 0.04%,...

Embodiment 2

[0051] 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 98% phosphorus trichloride dropwise under stirring condition 46.8g was neutralized to a pH value of 5.2, concentrated under reduced pressure to distill 228g of water, heated to 85°C and filtered while hot, the filter cake was washed with 20mL of hot water and dried to obtain 19.9g of product, wherein the content of iminodiacetic acid monosodium salt was 0.11%, the rest is sodium chloride.

[0052] The filtrate was transferred to a four-necked bottle equipped with a reflux condenser, a thermometer, a stirrer, and a constant pressure dropping funnel, and 248.8 g of 98% phosphorus trichloride was added dropwise, and 105.4 g of formaldehyde was added dropwise at a temperature controlled between 115-120°C (Content 37%, 1.3mol) After the addition, keep it warm for 2 hours, cool dow...

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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 and phosphorus trichloride to react with water 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 phosphorus trichloride and formaldehyde for 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 phosphorus trichloride is firstly separated, so that the content of sodium chloride in a reaction system 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 and sodium chloride; iminodiacetic acid is mixed with phosphorous acid and hydrochloric acid, heated, and then formaldehyde is added dropwise, The condensation reaction yields bi...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 丁永良刘佳游欢屈洋张飞李静程益何咏梅李双龙刘欢
Owner CHONGQING UNISPLENDOUR CHEM
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