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Process for preparing N-(phosphonomethyl) iminodiacetic acid by hydroxyacetonitrile continuous method

A technology of hydroxyacetonitrile and diglyphosate, which is applied in the field of diglyphosate preparation, can solve the problems of many side reactions, high catalyst requirements, and low purity, and achieve the reduction of by-products and polymers, simple and easy steps, and improved purity Effect

Active Publication Date: 2012-12-12
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high requirements on equipment and catalyst, and the catalyst is easily deactivated. The price of the raw material diethanolamine is unstable, and it is difficult to treat the three wastes.
[0006] Taking hydroxyacetonitrile as raw material through ammonolysis, alkaline hydrolysis, steps such as condensation to synthesize diglyphosate, there are also reports at home and abroad, CN101092430A synthesizes diglyphosate by the method of one-pot cooking, but this method has many side reactions in the ammonolysis process, and will simultaneously A large amount of tar polymer is generated, which seriously affects the subsequent alkali hydrolysis and condensation reactions, and the yield of diglyphosate is low, and the purity is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In the hydroxyacetonitrile solution of 51% in 274g concentration, add 0.96g methyl hydroquinone, 27.4g ammonium chloride, be warming up to 90 ℃ under the condition of stirring, dropwise concentration is the ammoniacal liquor 86.3g of 26%, control rate of addition, Keep the pH value of the hydroxyacetonitrile solution at 4.5, complete the dropwise addition in 20 minutes, raise the temperature to 102°C, keep it warm for 20 minutes, filter while it is hot, add 2.2 g of stabilizer aluminum oxide to the filtrate, adjust the pH value to 3 with hydrochloric acid, filter, and cool to 50°C, drop into 416g of 70°C sodium hydroxide solution with a concentration of 30%, and start to release ammonia gas, absorb the ammonia gas with water, maintain the temperature of the sodium hydroxide solution system at 75-80°C during the dropwise addition, and drop for 30 minutes After the addition, raise the temperature to 102°C, keep it warm for 2 hours, until no ammonia gas is generated, finish...

Embodiment 2

[0030] Add 0.45g N-nitrosodiphenylamine and ammonium chloride in 140g of hydroxyacetonitrile solution with a concentration of 51%. The molar ratio of hydroxyacetonitrile and ammonia water is 1:0.8, add ammonia water with a concentration of 26%, and control the rate of addition, so that the pH value of the hydroxyacetonitrile solution is 5. After 25 minutes, the dropwise addition is completed, and the temperature is raised to 105° C., kept for 20 minutes, and filtered while it is hot. , add 1.2g of stabilizer aluminum oxide to the filtrate, adjust the pH value to 5 with hydrochloric acid, cool to 50°C, drop into 210g of 25% sodium hydroxide solution at 60°C, and start to release ammonia gas, ammonia gas Absorb with water, maintain the temperature of the sodium hydroxide solution system at 75-80°C during the dropwise addition, complete the dropwise addition in 35 minutes, raise the temperature to 104°C, keep it warm for 2.5 hours, finish the reaction and cool to 50°C to obtain th...

Embodiment 3

[0032] Adding benzoquinone in the hydroxyacetonitrile solution of 51% in 420g concentration, the add-on is 1% of the consumption of hydroxyacetonitrile, 41.4g ammonium phosphate, the add-on is 50% of hydroxyacetonitrile, and it is heated up to 92 ℃ under the condition of stirring, According to the molar ratio of hydroxyacetonitrile and ammonia water as 1:0.3, add ammonia water with a concentration of 26% dropwise, and control the dropping speed so that the pH value of the hydroxyacetonitrile solution is at 5. The dropwise addition is completed in 35 minutes, and the temperature is raised to 101° C., kept for 18 minutes, and kept warm. Filter, add stabilizer aluminum oxide 3.6g to the filtrate, and adjust the pH value to 4 with hydrochloric acid, cool to 50°C, drop into 630g of 75°C concentration of 50% sodium hydroxide solution, and start to release ammonia, ammonia Absorb the gas with water, keep the temperature of the sodium hydroxide solution system at 75-80°C during the dro...

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Abstract

The invention discloses a process for preparing N-(phosphonomethyl) iminodiacetic acid by a hydroxyacetonitrile continuous method; in the method, hydroxyacetonitrile and ammonia which are used as raw materials are ammonolyzed, hydrolyzed with alkalis and condensed to obtain the N-(phosphonomethyl) iminodiacetic acid. The process is characterized in that iminodiacetonitrile is synthesized under the action of a polymerization inhibitor and a pH buffering agent in the ammonolysis step, wherein the amount of the polymerization inhibitor is 0.06-2.5% of the mass of the hydroxyacetonitrile, and theamount of the buffering agent is 1-50% of the weight of the hydroxyacetonitrile. The process has the characteristics that the iminodiacetonitrile prepared from the hydroxyacetonitrile and the ammoniadoes not need to be crystallized for separation and can be directly hydrolyzed with alkalis to produce iminodiacetic acid disodium salts, and the iminodiacetic acid disodium salt solution is directlyused for synthesizing the N-(phosphonomethyl) iminodiacetic acid; and the prepared N-(phosphonomethyl) iminodiacetic acid has the advantages of high purity and yield.

Description

technical field [0001] The invention provides a process for preparing diglyphosate, which uses hydroxyacetonitrile and ammonia as initial raw materials, and undergoes ammonolysis, alkali hydrolysis and condensation steps to obtain a diglyphosate product with a purity greater than 98%. Background technique [0002] Diglyphosate is mainly formed by condensation of iminodiacetic acid, phosphorous acid, phosphorus trichloride and formaldehyde under certain conditions in industry. Traditional synthesis techniques can be divided into the following categories: [0003] 1. Hydrocyanic acid method This method has strict requirements on equipment and safety, and the synthesis of hydrocyanic acid is restricted by the origin of natural gas resources, so the scope of promotion is limited. And there is a large amount of cyanide-containing waste water, which is not easy to deal with. It is treated by incineration, which consumes a lot of energy. [0004] 2. Chloroacetic acid method Chlor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 薛谊岳瑞宽李健葛九敢周典海
Owner ANHUI COSTAR BIOCHEM CO LTD
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