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Cleaning production method for iminodiacetonitrile

A technology of iminodiacetonitrile and hydroxyacetonitrile, which is applied in the chemical industry, can solve problems affecting product quality, complicate production, limit the scope of use, etc., and achieve the effect of improving product appearance

Active Publication Date: 2016-01-27
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But adding sulfuric acid can cause the urotropine produced in the reaction process to decompose and generate ammonium sulfate and formaldehyde, and formaldehyde can react with iminodiacetonitrile to generate impurity I compound (structural formula as shown in formula I), which affects product quality and limits its scope of use
Therefore, in order to obtain high-content iminodiacetonitrile, impurity removal and purification must be carried out, which complicates production and increases production cost

Method used

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  • Cleaning production method for iminodiacetonitrile
  • Cleaning production method for iminodiacetonitrile
  • Cleaning production method for iminodiacetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Take 1000 g of iminodiacetonitrile reaction solution produced by Xinjiang Ziguang Yongli Chemical Industry Co., Ltd., which is brown-black, with an iminodiacetonitrile content of 25%, quickly cool down to 45°C, feed sulfur dioxide gas until the reaction solution pH=3.0, and cool down to 10-15°C. ℃, stirred and crystallized for 6.0 h, filtered, washed the solid with a small amount of water, and dried to obtain 238.6 g of white iminodiacetonitrile product, the content of iminodiacetonitrile was 98.3%, and the impurity content of compound I was 0.38%.

Embodiment 2

[0085] Take 1000 g of iminodiacetonitrile reaction solution produced by Xinjiang Ziguang Yongli Chemical Industry Co., Ltd., which is brown-black, with an iminodiacetonitrile content of 25%, quickly cool down to 45°C, feed sulfur dioxide gas until the pH of the reaction solution is 2.0, and cool down to 10-15°C. ℃, stirred and crystallized for 6.0 h, filtered, washed the solid with a small amount of water, and dried to obtain a white iminodiacetonitrile product 236.8, with an iminodiacetonitrile content of 98.9% and an impurity content of 0.15% in Compound I.

Embodiment 3

[0087] Take 1000 g of iminodiacetonitrile reaction solution produced by Xinjiang Ziguang Yongli Chemical Industry Co., Ltd., which is brown-black, with an iminodiacetonitrile content of 25%, quickly cool down to 45°C, feed sulfur dioxide gas until the reaction solution pH=4.0, and cool down to 10-15°C. ℃, stirred and crystallized for 6.0 h, filtered, washed the solid with a small amount of water, and dried to obtain 233.5 g of white iminodiacetonitrile product, the content of iminodiacetonitrile was 97.9%, and the impurity content of compound I was 0.52%.

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Abstract

The invention belongs to the chemical field, and concretely relates to a cleaning production method for preparing iminodiacetonitrile from hydroxy acetonitrile and an ammonia source as raw materials. The method is concretely as follows: hydroxy acetonitrile and an ammonia source are reacted, a reaction solution containing iminodiacetonitrile is obtained, sulfurous acid or a substance or a system which can generate sulfurous acid is added to adjust the pH value to 0-7, then crystallization, separation and drying are carried out, and an iminodiacetonitrile product is obtained. Sulfurous acid is employed and is helpful to stabilize hydroxy acetonitrile in an acidic condition, polymerization and decomposition reactions are avoided, sulfurous acid can react with formaldehyde generated in the acidifying process, the situation that formaldehyde and iminodiacetonitrile react to generate impurities is prevented, the content of the obtained product iminodiacetonitrile is more than 97.0%, and the impurity content is less than 3%.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a clean production method for preparing iminodiacetonitrile by using hydroxyacetonitrile as a raw material. Background technique [0002] Iminodiacetonitrile, white or light gray needle crystal, melting point 74-76°C, soluble in water (solubility 6-7g, 25°C), easily soluble in organic solvents such as methanol, ethanol, acetone and chloroform, is a kind of An important chemical intermediate, mainly used in the production of pharmaceuticals, rubber, metal cleaning agents, complexes, especially the herbicide glyphosate, etc. [0003] Existing preparation method about iminodiacetonitrile is more, as adopting hydrocyanic acid, hexamethylenetetramine and formaldehyde as the method for raw material, aminoacetonitrile heating generation disproportionation reaction generates the method for iminodiacetonitrile, hydroxyacetonitrile and A method for preparing iminodiacetonitril...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C253/34C07C255/25
Inventor 丁永良郑道敏尹应武刘佳杨少梅张泉森夏兵金海琴柳亚玲翁帮荣刘乃逻何彪
Owner CHONGQING UNISPLENDOUR CHEM
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