Allantoin synthesizing process
A technology of allantoin and new process, applied in the field of new process for synthesizing allantoin, can solve the problems of large amount of catalyst, long reaction time, equipment corrosion, etc., and achieves improvement of atom economy, reduction of production cost, and reduction of usage amount Effect
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Embodiment 1
[0017] (1) Pretreatment of catalyst
[0018] Add 0.03 moles (8.4 g) of FeSO to a 250 ml four-necked flask equipped with a stirrer, condenser, thermometer, and constant pressure funnel 4 ·7H 2 O, add 66ml of 30% H dropwise under stirring 2 o 2 , Control the reaction temperature at 20°C. Catalyst A containing metal salt was prepared.
[0019] Soak the resin treated with ethanol and water in the saturated solution of rare earth metal salt, the proportioning ratio is 1g of resin to 8ml of ceric sulfate metal salt saturated solution, after soaking at room temperature for 22 hours, filter, then wash with distilled water until neutral, After drying, put it in a drying oven and activate it at 110°C for 5 hours before use as catalyst B.
[0020] (2) Synthesis of Allantoin
[0021] Add 100ml of 30% glyoxal aqueous solution to a four-necked flask equipped with a stirrer, condenser, thermometer, and constant pressure funnel, and slowly add the above-mentioned catalyst A under stirri...
Embodiment 2
[0023] According to the method of embodiment 1, in the mixture containing 5.62g urea, resin cerium ion catalyst B0.156g and 100ml30% glyoxal aqueous solution, at a temperature of 25 ℃, under stirring conditions, slowly add the above-mentioned catalyst A to carry out oxidation reaction, and then gradually generate temperature to 80°C for condensation reaction, and all the other processes are the same as in Example 1. The yield was between 52-54%.
Embodiment 3
[0025] (1) Pretreatment of catalyst
[0026] Add 0.03 moles of CeSO to a 250ml four-necked flask equipped with a stirrer, condenser, thermometer, and constant pressure funnel 4 , add dropwise 75ml of 30% H under stirring 2 o 2 , Control the reaction temperature at 10°C. A mixed solution containing rare earth metal salts, that is, catalyst A, is prepared for use.
[0027] Soak the resin treated with ethanol and water in a saturated aqueous solution of transition metal ferrous sulfate, the proportioning ratio is 1g of resin to 8ml of saturated ferrous sulfate solution, soak at room temperature for 26 hours, filter, and then wash with distilled water until neutral , after drying, put it into a drying oven and activate it at 100°C for 4 hours before use, it is Catalyst B.
[0028] (2) Synthesis of Allantoin
[0029] The method is the same as in Example 1, and the yield of allantoin is 54%-56%. Catalyst B can be recovered and reused 11 times, and the yield is basically stable...
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