How do you devolatilize before your WFE?
We are WFE crew and currently Devolatilize (degas) in our 5L SPD’s before loading into our WFE. I know there are other ways but i havent had time to test them. I hear roto over night and using ovens. We are looking for something scalable as we are expending. We dont want to use our WFE to strip because that just adds another cut and takes processing time from our machine. The goal is to devolatilize and remove all water, ethanol, and light terps before loading in the WFE. Otherwise you have to sit and wait for it to settle in feed flask before you can run. Right now we do it in our SPD’s and it works ok but is not scalable unless i want to have a bunch of SPD’s in the lab. I prefer to move away from glass if possible and find a more streamlined way to accomplish this task. So i would like to hear what you guys do out there. Thanks in Advance!
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I prefer vac oven, prob the most scalable solution that you’ll find that can also be used for multiple processes in the future
We crank the Rotovap up for a couple hours and then two passes on the wfe. Sometimes I can do it in one, but two is the norm.
I would think devol would be more effective in the wfe, then switch to spd for your final pass. Been wanting to try this.
Or get a wfe with no internal condenser, just external, for first pass, then into your final pass wfe.
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How long does it take to do certain amount of volume? Do you run it all night? I currently degas 10L of crude a day but i will need to do 10x this at my new facility. Any and all help is greatly appreciated.
We just bought a KDT-6 -2 stage. We dont want to waste its time with devolatilizing. I was thinking we decarb and devolatilize before the WFE and it limits our passes. Then this machine is just full production. What temps do you run your roto and for how long? I have heard some groups run roto all night. My biggest concern with roto is cranking up the heat on silicone and then dealing with a slippery ball. I love the idea of it…set and forget. The other question i have is…does it stick to the sides after you take it down that far?
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im experimenting with inert gas stripping the ethanol after a winterization partially because i think it will devolatilize it at the same time
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Interesting. Let me know how that goes. I need to be able to scale this. We will be extracting 500lbs a day and degasing 200+ L a day of crude. So what ever we do it needs to be scalable.
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Yeah, I hear you on the slippery ball. Lately I’ve been using water instead of oil for that reason, so I’m limited to about 90c for as long as I want to babysit it. Usually run the roto at about 50mbar or so for 3-4 hours. I just watch the ∆T across the condenser to tell if I’m still evaporating anything. I know I’m not doing as good a job as I was with oil at 100c+, so I’ve taken to doing two passes on the wfe. I have the luxury of time right now, too. I’m in the same boat you are, about to find all the bottlenecks in my work flow.
I’m betting one could probably stick with a water bath and just pull harder on the Rotovap and get back to a single pass on the wfe. My little diaphragm pump doesn’t go very deep.
Anyone know what the lower vac limit is on your average rotovap?
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