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Process for preparing iminodiacetonitrile

A technology of iminodiacetonitrile and preparation process, applied in the field of preparing iminodiacetonitrile, can solve the problems of complex reaction product, unstable product, low product yield, etc., and achieves high conversion rate, inhibition of polymerization and decomposition, high Yield effect

Active Publication Date: 2007-08-15
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, whether it is produced by batch method or continuous method, due to the complex reaction products and easy polymerization, the product is unstable. Although the product conversion rate is high, the product yield is low, and the product content is low and the quality is poor.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: Under the condition of no preheating, the hydroxyacetonitrile with the concentration of 40% by weight and the ammoniacal liquor with the concentration of 26.5% by weight are then entered into the continuous reactor with the metering pump respectively according to the theoretical ratio, and the flow rate of the hydroxyacetonitrile is 2m 3 / hour, the reaction temperature is controlled at 165 ° C ~ 180 ° C, the reaction pressure is 0.4Mpa, the residence time of the material in the reactor is 1 minute, the mixed liquid at the outlet of the reactor is analyzed by high performance liquid chromatography, the conversion rate is 78.7%, and the continuous reaction is 24 Obtain 9680 kilograms of black solid iminodiacetonitrile product in 1 hour, content 88.1%, yield 53.4%.

Embodiment 2

[0025] Embodiment 2: the hydroxyacetonitrile that is 40% by weight percentage concentration is preheated to 80 ℃ respectively, and the ammoniacal liquor that is 26.5% by weight percentage concentration is preheated to 175 ℃, enters continuous reactor with metering pump respectively according to theoretical ratio, and hydroxyl Acetonitrile flow rate is 2m 3 / hour, the reaction temperature is controlled at 165 ° C ~ 170 ° C, the reaction pressure is 0.7Mpa, the residence time of the material in the reactor is 1 minute, the mixed liquid at the outlet of the reactor is analyzed by high performance liquid chromatography, and the conversion rate is 95.7%. Obtain 13356 kilograms of black solid iminodiacetonitrile products in 1 hour, content 92.6%, yield 77.3%.

Embodiment 3

[0026] Embodiment 3: add stabilizer aluminum oxide in the hydroxyacetonitrile that weight percent concentration is 20%, its add-on is 0.1% of the weight percent of hydroxyacetonitrile, stir and mix at room temperature, preheat to 60 ℃; Preheat 25% ammonia water to 170°C; respectively use metering pumps to enter the continuous reactor, control the reaction temperature at 120°C-140°C, and the reaction pressure at 0.5Mpa, the residence time of the material in the reactor is 3 minutes; the outlet of the reactor The mixed solution was analyzed by high performance liquid chromatography, the conversion rate was 94.9%, and 7122 kg of brown-black solid iminodiacetonitrile product was obtained, the content was 94.8%, and the yield was 84.4%.

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Abstract

A process for preparing iminodiacetonitrile from hydroxy acetonitrile and ammonia water includes such steps as respective pre-heating, mixing and reacting.

Description

technical field [0001] The invention relates to a process for preparing iminodiacetonitrile, in particular to a process for preparing iminodiacetonitrile with hydroxyacetonitrile and ammonia source. Background technique [0002] Iminodiacetonitrile, light brown to off-white crystalline powder, melting point 75-76 ° C, is an important fine chemical intermediate, widely used in pesticides, dyes, medicines, synthetic resins, water treatment, electronics and other fields . [0003] U.S. Patent 5187301 discloses the method for preparing iminodiacetonitrile with hydroxyacetonitrile and ammonia source, and its principle is as follows: [0004] Main response: [0005] NH 3 +2HOCH 2 CNNH(CH 2 EN) 2 +2H 2 o [0006] side effects: [0007] NH 3 +HOCH 2 CNNH 2 CH 2 CN+H 2 o [0008] NH 3 + 3 HOCH 2 CNN(CH 2 EN) 3 +3H 2 o [0009] In the above reaction, side reactions also include dimers, trimers and multimers of the above products themselves and polymers between...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/30C07C255/61
Inventor 龙晓钦甘永昌周垂龙
Owner CHONGQING UNISPLENDOUR CHEM
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