Process for preparing 5,5-dimethyl-2,4-imidazolinedione by intermittent presurizing method
A technology of imidazoline dione and dimethyl, applied in five fields of pressurized batch method preparation, can solve the problems of difficult to realize industrialization, complicated reaction equipment, high toxicity of sodium cyanide, etc., and achieves easy-controllable conditions and simple preparation process. Effect
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Embodiment 1
[0009] Example 1: Add 34 grams (36.48 mL) of acetone cyanohydrin, 40 milliliters of water, and 35 grams of ammonium bicarbonate in a 140 milliliter autoclave, heat to 65-75 ° C, and the pressure rises to 0.8-1.4 MPa. Insulate and react at 70° C. for 1.5 hours until the pressure drops by 0.26 MPa. Pressure relief, cooling, filtering and drying. Yield: 35 g, 70% yield.
Embodiment 2
[0010] Example 2: Add 34 grams (36.48 mL) of acetone cyanohydrin, 45 milliliters of mother liquor, and 35 grams of ammonium bicarbonate into a 140 milliliter autoclave, heat to 65-75 ° C, and the pressure rises to 0.8-1.4 MPa. Insulate and react at 70°C for 1.5 hours until the pressure drops to 0.25MPa. Release the pressure, cool down to 20°C, filter and dry. Yield: 46.5 g, yield 92-94%.
Embodiment 3
[0011] Embodiment 3: add 340 kilograms (364.8L) acetone cyanohydrin in 1500 liters of autoclaves, 450 liters of mother liquors, 350 kilograms of ammonium bicarbonate, under stirring, pass steam in jacket and heat to 40 ℃, stop heating, naturally warming up to 70~ At 75°C, the pressure rises to 1.4-1.8MPa. Insulate and react at 70-75°C for 2 hours until the pressure drops below 0.3MPa. Cool down to 40°C with cooling water, release the pressure, continue cooling to 20°C, discharge, filter, and dry. Yield: 468 kg, yield 92-94%.
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