Novel allantoin synthesis process
A technology of allantoin and new technology, which is applied in the field of new synthesis technology of allantoin products, which can solve the problems of production equipment corrosion, energy waste, environment damage, etc., achieve light production equipment corrosion, improve product quality, and reduce production costs Effect
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Embodiment 1
[0017] While stirring, add 4.0 mol (160 g) of sodium hydroxide to 15 mol (480 g) of methanol, and after stirring for 1 hour, add 1 mol (143 g) of methyl dichloroacetate dropwise at 70 ° C. After the dropwise addition, keep warm and reflux And continue to stir for 6 hours, add 1mol (118g) of 31% hydrochloric acid, then filter out the solid, wash twice with 1mol (32g) methanol, and combine the washing filtrates to obtain a sodium dihydroxyacetate solution; Distill and recover methanol, stop the distillation when the gas phase temperature rises to 100°C, add 4mol (240g) of urea, 4mol (471g) of 31% hydrochloric acid, stir and keep warm at 90°C under reflux for 6 hours, cool to room temperature, and wash with water until Neutral, dry in an oven at 110°C to obtain 0.626mol (99g) of allantoin finished product, the product yield is 62.6%, and the infrared spectrum is consistent with the standard spectrum.
Embodiment 2
[0019] While stirring, add 8.0 mol (448 g) of potassium hydroxide to 30 mol (960 g) of methanol, stir evenly, add 2 mol (286 g) of methyl dichloroacetate dropwise at 75°C, keep warm and reflux after the dropwise addition and continue Stir for 6 hours, add 2mol (236g) of 31% hydrochloric acid to neutralize, then filter out the solid, wash twice with 2mol (64g) methanol, and combine the washing filtrates to obtain a potassium dihydroxyacetate solution; Distill and recover methanol, stop the distillation when the gas phase temperature rises to 95°C, add 8mol (480g) of urea, 9mol (1060g) of 31% hydrochloric acid, stir and keep warm at 75°C for 4 hours, cool to room temperature, wash with water until Neutral, dry in an oven at 120°C to obtain 1.24mol (196g) of allantoin finished product, the product yield is 62.1%, and the infrared spectrum is consistent with the standard spectrum.
Embodiment 3
[0021] While stirring, add 10 mol (560 g) of potassium hydroxide to 40 mol (3680 g) of ethanol. After stirring for 1.2 hours, add 3 mol (387 g) of dichloroacetic acid dropwise at 70°C. After the dropwise addition, keep warm and reflux and continue stirring 6 hours, add 3mol (155g) 95% sulfuric acid (1 / 2H 2 SO 4 ), then filter out the solid, wash twice with 4mol (184g) ethanol, and combine the washing filtrates to obtain a potassium diglycolate solution; the obtained potassium diglycolate solution is distilled to recover ethanol, and the gas phase temperature rises to 98°C Stop distillation, add 12mol (720g) urea, 10mol (516g) 95% sulfuric acid (1 / 2H 2 SO 4 ), stirred and kept at 85°C for 8 hours, cooled to room temperature, filtered and washed with water until neutral, dried in an oven at 120°C to obtain 1.88mol (297g) of allantoin finished product, product yield 61.6%, infrared spectrum and standard The spectra are consistent.
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