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Method for preparing diethylacetonitrile in imino group

A technology of iminodiacetonitrile and hydroxyacetonitrile, which is applied to the preparation of carboxylic acid nitriles, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of large amount of auxiliary raw material ammonium sulfate, harsh reaction conditions, and difficult handling, and achieve The preparation process is continuous and stable, the yield and quality are improved, and the stability is good

Inactive Publication Date: 2007-10-10
四川省天然气化工研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction conditions are harsh, liquid hydrocyanic acid is required, and there are large safety hazards. At the same time, the reaction yield is low, the cost is high, and the equipment efficiency is low.
[0005] 2. Publication No. CN1594281A discloses that under the action of catalyst replacing phenol and iron trihalide, ammonia is passed into the mixed system of hydroxyacetonitrile, and the pH value in the reaction process is controlled to obtain iminodiacetonitrile. This method has high yield , good quality, but this batch process has the disadvantages of unstable operation, low production capacity, excessive consumption of auxiliary raw material ammonium sulfate, etc.
[0006] 3. Publication No. CN1830953A discloses the continuous preparation of iminodiacetonitrile at 120-180°C, pressure of 0.4-1Mpa, and reaction time of 0.5-3 minutes using hydroxyacetonitrile and ammonia water as raw materials, with the addition of an alumina stabilizer. Higher, better quality, but the process is unstable, and the amount of three wastes is large, difficult to handle
[0007] 4. US5187301 discloses a method for preparing iminodiacetonitrile with hydroxyacetonitrile and ammonia source. The method is divided into continuous method and batch method. However, whether it is batch method or continuous method, it is difficult to realize industrialization due to its high requirements. Simultaneously reaction product is complicated, and product quality is not high, and yield is lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Hydroxyacetonitrile with a concentration of 400g / L and liquid ammonia (99.2% by mass) at room temperature are pumped into the tubular reactor with a metering pump and an ammonia pump at an equivalent ratio of 0.9:1, and the hydroxyl flow rate is 3000L / h, the reaction temperature is controlled at 170-180°C, the reaction pressure is 1.0-1.2Mpa, and the material residence time is 4 minutes. The reaction solution from the reactor is cooled rapidly by a plate heat exchanger and then enters the crystallization tank. The reaction is continued for eight hours to obtain Brown-red solid iminodiacetonitrile 7192kg, content 96.1%, yield 86.4%, by analyzing the reaction mother liquor, the conversion rate of this reaction is 97.2%, the mother liquor volume is 18.6m 3 .

Embodiment 2

[0023] Preheat the hydroxyacetonitrile with a concentration of 450g / L to 170°C, and liquid ammonia (99.2% by mass) at room temperature are pumped into the tubular reactor with a metering pump and an ammonia pump in an equivalent ratio of 1:1, respectively. , the hydroxyl flow rate is 2000L / h, the reaction temperature is controlled at 170-180°C, the reaction pressure is 1.0-1.2Mpa, and the material residence time is 3.5 minutes. The reaction continued for eight hours to obtain 5543kg of off-white solid iminodiacetonitrile, with a content of 96.5% and a yield of 89.2%. By analyzing the reaction mother liquor, the conversion rate of this reaction was 97.5%, and the volume of the mother liquor was 12.3m 3 .

Embodiment 3

[0025] Preheat the hydroxyacetonitrile with a concentration of 380g / L to 170°C, and liquid ammonia (98.7% by mass) at room temperature is pumped into the tubular reactor with a metering pump and an ammonia pump at an equivalent ratio of 1:1.1, respectively. , the hydroxyl flow rate is 500L / h, the reaction temperature is controlled at 170-180°C, the reaction pressure is 0.8-1.0Mpa, and the material residence time is 4 minutes. The reaction liquid from the reactor is cooled rapidly by a plate heat exchanger and enters the crystallization tank. Continuously reacted for eight hours to obtain 1119kg of brown-red solid iminodiacetonitrile, with a content of 96.4%, and a yield of 85.2%. By analyzing the reaction mother liquor, the reaction conversion rate was 98.1%, and the mother liquor volume was 3.1m3.

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Abstract

This invention provides a method for preparing iminodiacetonitrile. The method comprises: reacting hydroxyacetonitrile and 95-100 wt. % liquid ammonia to obtain iminodiacetonitrile. The method has such advantages as high yield, high product quality, and continuous and stable process.

Description

Technical field: [0001] The invention relates to a preparation method of iminodiacetonitrile, in particular to a method for preparing iminodiacetonitrile by reacting hydroxyacetonitrile with high-concentration liquid ammonia. Background technique: [0002] Iminodiacetonitrile (CAS 628-87-5), white or light gray needle-like crystalline powder, melting point: 74-76°C. Soluble in water, soluble in organic solvents such as methanol, ethanol and chloroform, flammable and toxic. It is mainly used in the manufacture of glyphosate and other pesticides, and also in the fields of pesticides, synthetic resins, water treatment and electronic appliances. [0003] Existing preparation methods about iminodiacetonitrile are more, but there are some weak points: [0004] 1. Use hydrocyanic acid, hexamethylenetetramine and formaldehyde as raw materials. That is, under the conditions of above 130°C, 1Mpa, and a residence time of 1-2 minutes, the mixed aqueous solution of hydrocyanic acid, h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/24C07C253/30
Inventor 龙志成唐劲松黄成太邹童
Owner 四川省天然气化工研究院
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