Process for preparing hydantoin by one-step method
A hydantoin and process technology, applied in the field of one-step preparation of hydantoin, can solve problems such as lengthy route, discharge of waste acid solution, increased cost, etc., and achieve the effects of reducing cost, avoiding use, and reducing environmental pollution
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Embodiment 1
[0015] Prepare 500ml of hydroxyacetonitrile solution of 4mol / L, drop it into the trickle bed reactor from the top at a flow rate of 200mL / h, carbon dioxide and ammonia gas flow from the bottom of the bed at 0.04m 3 / h and 0.02m 3 The speed of / h is passed from the bottom, the bed is heated by the jacket, and the temperature is controlled at 70°C. After the reaction solution is exhausted, the solution obtained after the reaction is collected and concentrated to 1 / 3-1 / 4 of the original volume. , cooled and crystallized to obtain hydantoin, recrystallized and vacuum dried to obtain hydantoin 138g, the purity was 99.5%, and the yield was 68.66%.
Embodiment 2
[0017] Prepare 500ml of hydroxyacetonitrile solution of 4mol / L, drop it into the trickle bed reactor from the top at a flow rate of 200mL / h, carbon dioxide and ammonia gas flow from the bottom of the bed at 0.045m 3 / h and 0.02m 3 The speed of / h is passed from the bottom, the bed is heated by the jacket, and the temperature is controlled at 70°C. After the reaction solution is exhausted, the solution obtained after the reaction is collected and concentrated to 1 / 3-1 / 4 of the original volume. , cooled and crystallized to obtain hydantoin, recrystallized and vacuum dried to obtain hydantoin 142g, the purity was 99.7%, and the yield was 70.79%.
Embodiment 3
[0019] Prepare 500ml of hydroxyacetonitrile solution of 4mol / L, drop it into the trickle bed reactor from the top at a flow rate of 200mL / h, carbon dioxide and ammonia gas flow from the bottom of the bed at 0.045m 3 / h and 0.025m 3 The speed of / h is passed from the bottom, the bed is heated by the jacket, and the temperature is controlled at 70°C. After the reaction solution is exhausted, the solution obtained after the reaction is collected and concentrated to 1 / 3-1 / 4 of the original volume. , cooled and crystallized to obtain hydantoin, recrystallized and vacuum dried to obtain hydantoin 130g, the purity was 99.2%, and the yield was 64.48%.
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