Method for preparing iminodiacetic acid by using raw material of hydroxy acetonitrile
A technology of iminodiacetic acid and hydroxyacetonitrile, which is applied in the preparation of cyanide reaction, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of potential safety hazards, poor reaction selectivity, and low ammonia recovery rate, and achieve easy Transport and storage, mild reaction conditions, easy preparation and purification
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Embodiment 1
[0021] Add hydroxyacetonitrile (50%) 500 grams (4.39mol) in the reaction bottle of 1000 milliliters, add ammonium chloride 38.5 grams (0.72mol) under stirring, give system heating then, when being heated to 110 ℃, start to add ammoniacal liquor, Control the drip rate of ammonia water to ensure that the pH value of the reaction solution is between 5 and 8, and at the same time control the temperature of the reaction system between 110 and 130°C. After adding 158 grams (2.3 mol) of ammonia water (25%), the dropwise addition can be stopped, and the temperature is kept at 110-130° C. for 2 hours, and the reaction solution is transferred to a 2000 ml reaction flask. Add 865 grams (8.53mol) of 36% concentrated hydrochloric acid. After the hydrochloric acid is added, keep it warm at 80-150°C for 4 hours, then cool it down. 484.8 grams of the mixture of acid salt and ammonium chloride, the material yield is 75%. The reaction mother liquor is used mechanically, and the crude product c...
Embodiment 2
[0024] Add hydroxyacetonitrile (50%) 500 grams (4.39mol) in the reaction bottle of 1000 milliliters, add ammonium chloride 38.5 grams (0.72mol) under stirring, give system heating then, when being heated to 110 ℃, start to add ammoniacal liquor, Control the drip rate of ammonia water to ensure that the pH value of the reaction solution is between 5 and 8, and at the same time control the temperature of the reaction system between 110 and 130°C. After adding 158 grams (2.3 mol) of ammonia water (25%), the dropwise addition can be stopped, and the temperature is kept at 110-130° C. for 2 hours, and the reaction solution is transferred to a 2000 ml reaction bottle.
[0025] Add 865 grams (8.53mol) of 36% concentrated hydrochloric acid prepared by mixing and absorbing hydrochloric acid gas from the previous batch of mother liquor and water; At 10° C., 568.8 grams of a mixture of iminodiacetic acid hydrochloride and ammonium chloride were obtained by suction filtration, and the yie...
Embodiment 3
[0028] Add hydroxyacetonitrile (50%) 500 grams (4.39mol) in the reaction bottle of 1000 milliliters, add ammonium chloride 38.5 grams (0.72mol) under stirring, give system heating then, when being heated to 110 ℃, start to add ammoniacal liquor, Control the drip rate of ammonia water to ensure that the pH value of the reaction solution is between 5 and 8, and at the same time control the temperature of the reaction system between 110 and 130°C. After adding 158 grams (2.3 mol) of ammonia water (25%), the dropwise addition can be stopped, and the temperature is kept at 110-130° C. for 2 hours, and the reaction solution is transferred to a 2000 ml reaction bottle.
[0029] Add 865 grams (8.53mol) of 36% concentrated hydrochloric acid prepared by mixing and absorbing hydrochloric acid gas from the previous batch of mother liquor and water; At 10° C., 568.8 grams of a mixture of iminodiacetic acid hydrochloride and ammonium chloride were obtained by suction filtration, and the yie...
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