Preparation technique of iminodiacetonitrile

A technology of iminodiacetonitrile and hydroxyacetonitrile, which is applied in the field of preparation technology of iminodiacetonitrile, can solve the problems of many reaction by-products, great safety hazards, difficulty in realizing industrialization, etc., achieves the improvement of yield and content, and prevents the production of nitriles Polymerization, avoiding the effect of side reactions

Inactive Publication Date: 2010-04-07
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. US 2794044 discloses a method for preparing iminodiacetonitrile with formaldehyde, hydrogen cyanide and ammonia as raw materials. The pH is adjusted by adding sulfuric acid. After 20 hours of reaction, cooling and crystallization obtains iminodiacetonitrile, but there are many by-products in this reaction , the yield is low, and the highly toxic raw material hydrogen cyanide is used, which has great potential safety hazards
[0005] 2. US5187301 discloses a method for preparing iminodiacetonitrile with hydroxyacetonitrile and ammonia source. The method includes batch and continuous methods. Although ammonium sulfate is added as a buffer, the occurrence of polymerization cannot be effectively avoided. Therefore, whether it is intermittent or continuous, Because the reaction product is relatively complicated, the product is unstable, although the conversion rate of the product is high, the yield is low, and the product quality is low, it is difficult to realize industrialization
[0006] 3. CN1830953 discloses the use of hydroxyacetonitrile and ammonia water as raw materials to prepare iminodiacetonitrile. Although aluminum oxide is used as a stabilizer, the process is unstable, and the three wastes are large and difficult to handle
[0007] 4. CN101050191A discloses that hydroxyacetonitrile and ammonia are used as raw materials, and trimethylhydroquinone is added as a polymerization inhibitor to react to obtain iminodiacetonitrile, although the yield of iminodiacetonitrile obtained by using the polymerization inhibitor And the quality has been greatly improved, but the occurrence of side reactions is still unavoidable at a higher reaction temperature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Be that in the hydroxyacetonitrile of 50% by mass percent, add composite type polymerization inhibitor (by mass ratio, hydroquinone: N, N'-dialkyl-p-phenylenediamine=5: 1) and ammonium sulfate respectively, wherein The addition amount of the polymerization inhibitor is 0.5% of the pure hydroxyacetonitrile mass, the ammonium sulfate addition is 15% of the pure hydroxyacetonitrile mass, stirred and mixed evenly at room temperature, acidified with dilute sulfuric acid to a pH value of 2, preheated to 100 ° C, Liquid ammonia (mass percentage composition 99.3%) under room temperature is squeezed into continuous reactor with metering pump and ammonia pump respectively, and the hydroxyacetonitrile flow rate is 2.5m 3 / hour, the reaction temperature is controlled at 140-160°C, the reaction pressure is 0.8-1.0Mpa, the residence time of the material in the reactor is 3 minutes, and then the reaction mixture from the reactor is quenched and then enters the crystallization tank, an...

Embodiment 2

[0030] Be that in the hydroxyacetonitrile of 50% by mass percent, add composite type polymerization inhibitor (by mass ratio, hydroquinone: N, N'-dialkyl-p-phenylenediamine=5: 1) and ammonium sulfate respectively, wherein The amount of polymerization inhibitor added is 1% of the mass of pure hydroxyacetonitrile, the amount of ammonium sulfate added is 20% of the mass of pure hydroxyacetonitrile, stirred and mixed evenly at room temperature, acidified to pH 3 with dilute sulfuric acid, preheated to 100 ° C, Liquid ammonia (mass percentage composition 99.3%) under room temperature is squeezed into continuous reactor with metering pump and ammonia pump respectively, and the hydroxyacetonitrile flow rate is 2.5m 3 / hour, the reaction temperature is controlled at 140-160°C, the reaction pressure is 0.8-1.0Mpa, the residence time of the material in the reactor is 5 minutes, and then the reaction mixture from the reactor is quenched and then enters the crystallization tank, and sulfu...

Embodiment 3

[0032] In the hydroxyacetonitrile of 60% by mass percentage, add composite inhibitor (according to mass ratio, hydroquinone: alkylbenzene sulfonic acid tertiary amine salt=5: 1) and ammonium sulfate, wherein inhibitor adds The amount is 1% of the mass of pure hydroxyacetonitrile, the amount of ammonium sulfate added is 15% of the mass of pure hydroxyacetonitrile, stirred and mixed evenly at room temperature, acidified with dilute sulfuric acid to a pH value of 3, preheated to 110 ° C, and the rest are the same as in Example 2 , 9132 kg of off-white crystal iminodiacetonitrile was obtained, the content was 98.1%, and the yield was 91.3%.

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PUM

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Abstract

The invention discloses a preparation technique of iminodiacetonitrile, belonging to the field of chemical engineering. In the technique, glycolic acid nitrile reacts with ammonia, a compound polymerization inhibitor is added, and reaction is carried out to obtain iminodiacetonitrile. The iminodiacetonitrile prepared by the invention has higher yield and content, side reaction under higher reaction temperature is avoided, and the reaction is more stable.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a preparation process of iminodiacetonitrile using a composite polymerization inhibitor. Background technique [0002] Iminodiacetonitrile (CAS 628-87-5), light yellow to brown powder, melting point 75-78°C, soluble in water (solubility 6-7g, 25°C), soluble in organic solvents such as acetone. It is mainly used to synthesize the herbicide glyphosate. In addition, as an important fine chemical intermediate, it is widely used in the fields of dyes, electroplating, water treatment, and synthetic resins. [0003] There are many existing methods for the preparation of iminodiacetonitrile. [0004] 1. US 2794044 discloses a method for preparing iminodiacetonitrile with formaldehyde, hydrogen cyanide and ammonia as raw materials. The pH is adjusted by adding sulfuric acid. After 20 hours of reaction, cooling and crystallization obtains iminodiacetonitrile, but there are many by-products i...

Claims

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Application Information

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IPC IPC(8): C07C255/24C07C253/30C07C253/32
Inventor 王红明李家栋李健葛九敢周典海
Owner ANHUI COSTAR BIOCHEM CO LTD
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