Method for preparing urotropin by ammoxidation of methanol in presence of vanadium compound catalyst
A technology of urotropine and vanadium compounds, which is applied in the field of ammonia oxidation of methanol to prepare urotropine, can solve the problems of long storage time, high cost, unstable formaldehyde, etc., shorten the synthesis steps, improve production efficiency, improve The effect on total yield
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[0022] Add 70% methanol solution, 25% ammonia solution, and 20% hydrogen peroxide solution into the reaction kettle at a ratio of 2:1:4, add a vanadium compound catalyst, and control the pH value of the reaction solution between 4 and 4.5. Keep the temperature between 50°C and 55°C and stir for 180 minutes.
[0023] After the reaction is completed, the reaction solution is taken out, and alkali is added to adjust the pH value between 8 and 10, the catalyst is allowed to settle, separated by filtration and recovered for reuse.
[0024] The filtrate is post-treated, unreacted methanol is recovered for the second ammoxidation reaction, and the final product urotropine is obtained through steps such as evaporation, concentration, recrystallization, and dehydration.
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