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
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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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