Clean production method for preparing iminodiacetonitrile by taking hydroxy acetonitrile as raw material

A technology of iminodiacetonitrile and hydroxyacetonitrile, which is applied in the preparation of carboxylic acid nitriles, chemical instruments and methods, and the preparation of organic compounds. It can solve problems such as poor stability, difficult waste liquid treatment, and unstable process, and meet the reaction conditions. Mild, less treatment, lower cost effects

Active Publication Date: 2009-12-02
BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of this method is about 78% after recrystallization, but considering that the two starting materials all need to be prepared separately, especially aminoacetonitrile (NH 2 CH 2 CN) is difficult to prepare and has poor stability, making it difficult to realize industrialization
[0006] 4. Publication No. CN1830953A discloses that hydroxyacetonitrile and ammonia are used as raw materials to continuously prepare iminodiacetonitrile at 120-180°C, pressure 0.4-1MPa, and reaction time 0.5-3 minutes under the addition of alumina stabilizer. Unstable, uneven product quality, large amount of catalyst, large amount of three wastes, difficult to handle and can only be incinerated, which does not meet environmental protection requirements
At present, this method is mainly used in domestic production, but there are many problems such as large amount of catalyst added, low crystallization yield, dark color, and difficult treatment of waste liquid. The mother liquid is mostly treated by incineration, which does not meet the requirements of clean production and environmental protection.

Method used

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  • Clean production method for preparing iminodiacetonitrile by taking hydroxy acetonitrile as raw material

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add hydroxyacetonitrile (50%) 300 grams (2.63 moles) in the reaction flask of 500 milliliters, add ammonium chloride 23 grams (0.43 moles) under stirring, then give system heating, when being heated to 90 ℃, start to add ammoniacal liquor, Control the drip rate of ammonia water to ensure that the pH value of the reaction solution is between 5-8, and simultaneously control the temperature of the reaction system between 110-130°C. After adding 90 grams (1.32 moles) of ammonia water (25%), the dropwise addition can be stopped, and the heat preservation at 100-110° C. for half an hour is continued, the reaction solution is cooled to 20-25° C., kept stirring for 1 hour, and suction filtered to obtain 104 gram of iminodiacetonitrile wet product, yield 75%, obtain mother liquor 295 grams simultaneously.

[0028] Heat 295 grams of mother liquor obtained by suction filtration to 75°C for dehydration under reduced pressure, the vacuum degree of dehydration is -0.08~-0.09Mpa, afte...

Embodiment 2

[0030] Add hydroxyacetonitrile (50%) 300 grams (2.63 moles) in the reaction flask of 1000 milliliters, add 130 grams of mother liquors to be applied mechanically in Example 1 under stirring, then give system heating, when being heated to 90 ℃, start to add ammoniacal liquor, control The dropping speed of ammonia water is to ensure that the pH value of the reaction solution is between 5-8, and at the same time control the temperature of the reaction system between 100-130°C. After adding 88 grams (1.29 moles) of ammonia water (25%), the dropwise addition can be stopped, continue to be incubated at 100-110° C. for half an hour, and the reaction solution is cooled to 20-25° C., kept stirring for 1 hour, and suction filtered to obtain 125 gram of iminodiacetonitrile wet product, yield 88%, obtain mother liquor 380 grams simultaneously.

[0031] Heat 380 grams of mother liquor obtained by suction filtration to 75°C for dehydration under reduced pressure. The dehydration vacuum degr...

Embodiment 3

[0033] Add hydroxyacetonitrile (50%) 300 grams (2.63 moles) in the reaction bottle of 1000 milliliters, add embodiment 2 under stirring and wait to apply mechanically 160 grams of mother liquor, then give system heating, when being heated to 90 ℃, start to add ammoniacal liquor, control The dropping speed of ammonia water is to ensure that the pH value of the reaction solution is between 5-8, and at the same time, the temperature of the reaction system is controlled between 110-130°C. After adding 86 grams (1.26 moles) of ammonia water (25%), you can stop the dropwise addition, continue to keep warm at 100-110°C for half an hour, adjust the pH value of the reaction solution to 2-4, cool to 20-25°C, and keep stirring After 1 hour, 132 grams of iminodiacetonitrile wet product was obtained by suction filtration, with a yield of 91%, and 405 grams of mother liquor were obtained at the same time.

[0034] Heat 405 grams of mother liquor obtained by suction filtration to 75°C for dehy...

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Abstract

The invention provides a clean production method for preparing iminodiacetonitrile by taking hydroxy acetonitrile and ammonia as raw materials in the presence of catalysis of inorganic ammonium salt and circularly applying a mother solution instead of a catalyst after the mother solution is condensed. The method has small quantity of three wastes of atoms and easy industrialization and is a novel process with less investment, quick response, low production cost, remarkable economic benefit and strong market competitiveness.

Description

technical field [0001] The invention relates to a clean production method for preparing iminodiacetonitrile by using hydroxyacetonitrile as raw material. Background technique [0002] Iminodiacetonitrile (CAS 628-87-5), white or light gray needle crystal, melting point 74-76°C, soluble in organic solvents such as methanol, ethanol, and chloroform, is an important chemical intermediate, mainly used In medicine, rubber, metal cleaning agents, complexes, herbicides, etc. [0003] 1. Using hydrocyanic acid (HCN), hexamethylenetetramine ((CH 2 ) 6 N 4 ) and formaldehyde (HCHO) as raw materials. That is, under the conditions of temperature 150°C, pressure 1MPa, and residence time 1-2 minutes, the mixed aqueous solution of hydrocyanic acid, hexamethylenetetramine and formaldehyde enters the tubular reactor under certain pH conditions for reaction, thereby Iminodiacetonitrile was obtained. The reaction conditions are harsh, liquid hydrocyanic acid is required, and there is a g...

Claims

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Application Information

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IPC IPC(8): C07C255/30C07C253/30
Inventor 廖翠莺李星尹应武尹政清李建虹陈斌
Owner BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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