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
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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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