Bkhan3 Posted December 7, 2023 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?
exchemist Posted December 7, 2023 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.
Bkhan3 Posted December 8, 2023 Author 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.
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