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Method for preparing iminodiacetic acid by using raw material of hydroxy acetonitrile

A technology of iminodiacetic acid and hydroxyacetonitrile is applied in the preparation of cyanide reaction, chemical instruments and methods, preparation of organic compounds, etc., which can solve the problems of potential safety hazards, poor reaction selectivity, easy generation of tar, etc., and achieve easy transportation. The effect of storage, mild reaction conditions, and cost reduction of raw materials

Active Publication Date: 2009-11-11
BEIJING ZIGUANG YINGLI CHEM TECH 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 catalysts, and there are potential safety hazards, and the raw material diethanolamine is affected by the price of crude oil, resulting in high production costs. At the same time, there are economic, technical and environmental factors such as three wastes and catalyst deactivation. The competitiveness of this process Not strong
[0003] The hydrocyanic acid method is generally favored at home and abroad. U.S. Patent No. 5,187,301 reports the preparation of iminodiacetonitrile by the batch method of hydroxyacetonitrile, followed by hydrolysis with sodium hydroxide, acidification, crystallization, separation, and the method for preparing iminodiacetic acid , has been widely favored or adopted by relevant manufacturers at present, but this method has poor reaction selectivity, serious decomposition and polymerization in the process, easy to produce tar, complex post-processing, too many times of solid-liquid separation, and a small amount of hydrocyanic acid when there is solid-liquid separation And the safety and environmental protection of ammonia escape, the waste water produced by aminoacetonitrile and iminodiacetonitrile is difficult to deal with, and must be treated with high-investment and high-energy-consuming incineration devices; low ammonia recovery rate, large investment, low ammonia concentration, and poor use value ; The yield of iminodiacetic acid p-hydroxyacetonitrile is only about 60%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add hydroxyacetonitrile (50%) 500 grams (4.39mol) in the reaction bottle of 1000 milliliters, add ammonium chloride 38.5 grams (0.72mol) under stirring, give system heating then, when being heated to 110 ℃, start to add ammoniacal liquor, Control the drip rate of ammonia water to ensure that the pH value of the reaction solution is between 5 and 8, and at the same time control the temperature of the reaction system between 110 and 130°C. After adding 158 grams (2.3 mol) of ammonia water (25%), the dropwise addition can be stopped, and the temperature is kept at 110-130° C. for 2 hours, and the reaction solution is transferred to a 2000 ml reaction bottle. Add 865 grams (8.53mol) of 36% concentrated hydrochloric acid. After the hydrochloric acid is added, keep it warm at 80-150°C for 4 hours, then cool it down. 484.8 grams of the mixture of acid salt and ammonium chloride, the material yield is 75%. The reaction mother liquor is used mechanically, and the crude product ...

Embodiment 2

[0024] Add hydroxyacetonitrile (50%) 500 grams (4.39mol) in the reaction bottle of 1000 milliliters, add ammonium chloride 38.5 grams (0.72mol) under stirring, give system heating then, when being heated to 110 ℃, start to add ammoniacal liquor, Control the drip rate of ammonia water to ensure that the pH value of the reaction solution is between 5 and 8, and at the same time control the temperature of the reaction system between 110 and 130°C. After adding 158 grams (2.3 mol) of ammonia water (25%), the dropwise addition can be stopped, and the temperature is kept at 110-130° C. for 2 hours, and the reaction solution is transferred to a 2000 ml reaction flask.

[0025] Add 865 grams (8.53mol) of 36% concentrated hydrochloric acid prepared by mixing and absorbing hydrochloric acid gas from the previous batch of mother liquor and water; At 10° C., 568.8 grams of a mixture of iminodiacetic acid hydrochloride and ammonium chloride were obtained by suction filtration, and the yiel...

Embodiment 3

[0028] Add hydroxyacetonitrile (50%) 500 grams (4.39mol) in the reaction bottle of 1000 milliliters, add ammonium chloride 38.5 grams (0.72mol) under stirring, give system heating then, when being heated to 110 ℃, start to add ammoniacal liquor, Control the drip rate of ammonia water to ensure that the pH value of the reaction solution is between 5 and 8, and at the same time control the temperature of the reaction system between 110 and 130°C. After adding 158 grams (2.3 mol) of ammonia water (25%), the dropwise addition can be stopped, and the temperature is kept at 110-130° C. for 2 hours, and the reaction solution is transferred to a 2000 ml reaction flask.

[0029] Add 865 grams (8.53mol) of 36% concentrated hydrochloric acid prepared by mixing and absorbing hydrochloric acid gas from the previous batch of mother liquor and water; At 10° C., 568.8 grams of a mixture of iminodiacetic acid hydrochloride and ammonium chloride were obtained by suction filtration, and the yiel...

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PUM

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Abstract

The invention provides a method for preparing and separating iminodiacetic acid by using hydroxyacetonitrile as a raw material through a one-pot cooking method. The method has high yield, less three wastes, and the obtained product is easy to prepare and purify.

Description

technical field [0001] The invention relates to a method for preparing iminodiacetic acid and its salts by using hydroxyacetonitrile as a raw material, in particular to a method for synthesizing and separating iminodiacetic acid by using hydroxyacetonitrile as a raw material through one-step acidolysis. Background technique [0002] The domestic industrial production methods of iminodiacetic acid mainly include hydrogen cyanide method, chloroacetic acid method and diethanolamine method. The chloroacetic acid method is a mature process, but the process is long, the product purity is low, the cost is high, and the "three wastes" are serious, so it is already an obsolete process. Diethanolamine method is a new technology developed in foreign countries in the 1990s. This method uses diethanolamine as the main raw material, under the presence of high temperature (170°C), high pressure (0.8Mp) and Cu-Ni alloy catalyst and sodium hydroxide, oxidative dehydrogenation , to generate ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/16C07C227/12
Inventor 李星尹应武顾爱宏郭钰来田金平罗志刚冯倩闫惠娟石春光张华沙伊娜
Owner BEIJING ZIGUANG YINGLI CHEM TECH CO LTD