Bkhan3 Posted December 7, 2023 Share Posted December 7, 2023 The usual way seems to be heating a mix of Niacin and catalyst (I used basic copper carbonate) and limiting temp at the heating mantle to 250 deg C. I put a K-type thermocouple between the mantle and distillation flask. After 2 hours the head temp was only 60 deg C and nothing was happening (actually something was happening the Niacin was melting with drops forming in the head). So I raised the mantle temp and started getting distillate. Problem is the Niacin sublimes as a white vapor passing over to the receive flask, the Niacin in the rxn flask is burning and recrystallizing in the rxn flask. A loss of yield. Do I have to just let it sit at 250 deg C mantle temp? Link to comment Share on other sites More sharing options...
exchemist Posted December 7, 2023 Share Posted December 7, 2023 8 hours ago, Bkhan3 said: The usual way seems to be heating a mix of Niacin and catalyst (I used basic copper carbonate) and limiting temp at the heating mantle to 250 deg C. I put a K-type thermocouple between the mantle and distillation flask. After 2 hours the head temp was only 60 deg C and nothing was happening (actually something was happening the Niacin was melting with drops forming in the head). So I raised the mantle temp and started getting distillate. Problem is the Niacin sublimes as a white vapor passing over to the receive flask, the Niacin in the rxn flask is burning and recrystallizing in the rxn flask. A loss of yield. Do I have to just let it sit at 250 deg C mantle temp? I thought it was copper chromite that was commonly used as a decarboxylation catalyst. Link to comment Share on other sites More sharing options...
Bkhan3 Posted December 8, 2023 Author Share Posted December 8, 2023 Yes, that is the catalyst of choice here - can also use basic copper carbonate and I had some. I have to make some of the other which I will do and try this again. Thanks. Link to comment Share on other sites More sharing options...
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