So when running the CBN disty to isolate I am getting the distillate to crash out but when pulling vacuum to dry out the crashed out material I am only getting is down to an almost ice cream consistancy. Any one ever had this situation? When I run from sulfur the crash out is very fast and pulls dry isolate and it seems the pd/c way has an almost different consistancy. Anyone experience this at all?
Use a fritted disk and that shouldn’t happen. Dilute in cold solvent so the solvent goes through the filter faster and doesn’t get the jello consistency
I’ve had it happen from a poorly placed filter paper or felt pad. Are you building vacuum as the cake sits now or is it just losing vac through a channel?
It’s possible to achieve >85% CBN in your reaction with iodine at temperatures half of what folks here are saying about Pd/C, or from what I’ve heard about sulfur. This conversion can be done well below 150C…with no H2S or palladium.
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I need to be able to get large amounts of isolate made at once and most frits are small amounts. I am using a 20L buchner filter with 2 micron filter paper
Try a faster flow paper. I think the frit is 30 -60.
2 micron is going to slow it down even if you dilute in cold solvent
Across makes a 2000 ml frit. You can easily filter a kg at a time pretty quick
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If I go to big will I loose isolate through the filter?
That’s why I like the frit better. You don’t get any loss
I do feel you loose some around the edges of the paper filtering with the filter papers
I think the papers I use are 30um
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I’m having issues purchasing this article, I keep getting an error code. Does anyone know where else I can get access to this article?
Thank you in advance for any help!
What do any of you know about remediating the mother liquor when doing a sulfur reaction. The ML will be contaminated with sulfides and I have heard I can clean the sulfides out through washing with hydrogen peroxide, and validity in this?
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I remember @RockSteady was working with a lot peroxide doing washes maybe he’ll chime in.
it’ll also oxidise the phenolic hydroxyl group
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yeah using h2o2 is a common technique for desulfurization in the petroleum industry, works here aswell, just keep it dilute and do more washes then you think youll need.
as for remediating the ML, elemental copper works well aswell, you just need a ton. make friends with a machinist near by and have him make tons of small copper chips, and use em super quick before the copper froms an oxide layer on it. copper powders are also available and you can preemptively remove the oxide layers with various acids, its just a pain in the ass. easier to by a ingot of copper and make chips the same day you remediate imo.
filtering through copper and washing with dilute h2o2 works pretty well, really depends on the concentration in the ML.
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The king mentioned carbon (‘course he sells it), any thoughts there?
column filtration through carbon would deffently help deodorize, might take a few passes through a big ass column tho to get them below the odor detection threshold.
I always run column filtration anyways, its good practice too. always yields a cleaner, superior product, its just slow going.
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Ohhh just read the thread, you were talking about pd/c! Yeah pd/c is vastly superior too S imo. So much easier to clean up, and its reusable, pdc is good stuff my go too method for CBN.
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You were right the first time, I was ignoring the premise of the thread to focus on sulfur remediation 
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My only issue with pd/c is when I crash it out the crystal’s are so small they clog my filters. S route crashes at room temp whereas pd/c needs to be frozen
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Dissolve in a diffrent solvent to have better crashing yields
THF or DMA
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