C
cronicoldguy
- 102
- 28
Sorry I can not help here and Moe is on vacation , but I can bump it up to the topSo I have a dilemma. I have 2.5 gallons of solution to distill. Have been using a fractional still in the past. But it takes quite a while and needs to be monitored closely. Hoping @Moe.Red and others in the know will reply.
I already have a 5L glass jacketed reactor. Would it be as efficient and do as good as a job as a rotovap if I purchased a circulating heated water bath, and distilled with the reactor instead? I realize it wont be as fast, but will it do as good of a job?
I also already have a circulating chiller. But it only goes down to -5C. If I purchased a heater/chiller combo, I could extract, winterize, and distill in the reactor. I am already using it to extract. Works very well. Constantly stirring during extraction, and temp controlled if I had a heater/chiller. I made a cheesecloth bag and stainless steel cage that fits inside the reactor kettle. It retains the biomass for easy removal.
Reason I ask is because both are relatively the same price and I could really use the heater/chiller for the reactor. But at the same time, I want to be efficient and cost effective. The reactor is so versatile, I am leaning towards the heater.
I am wanting to purchase ASAP.
EDIT: Does anyone know if it is possible to configure 4X Soxhlet Extractors with my reactor? Would the 5L volume of the kettle have the capacity to supply 4 extractors at same time? Or is that too greedy? Maybe only 2 Extractors?
Ordered! Hope this dont bite me in the ass! After two failed attempts ordering one from China, I said fuck it and ordered one from here in Canada.
Went with this rotovap: 2L Electric AquaVap Turnkey System
I already have the same circulating pump. Guess I have a spare now.
I really hope this works well for me. I wanted to go with a 5L unit that can utilize 1L and 3L boiling flasks as well. But cost was much higher, and a delivery date of over 1 month. I am already months behind. Not sure if getting the circulating water bath instead would have been a better move.
Thanks for the interest.I'm pretty happy with my chicom rotovap but I got it off eBay from guys with American stock. Think I ended up paying a hundred more for it that the same ones on aliexpress but I think it is worth it not to deal with the issues you have had. I'd invest in a large receiving flask and an adjustable support for it. These guys make decent quality:
Proper chillers are crazy expensive for what they are. They don't seem to come up used and working for that much of a discount either. I thought about building a Peltier cooling array on a bunch of heat exchangers but found an easier solution.
For coolant I use a big aluminum pot full of antifreeze that I keep in a chest freezer. When running, 2 12v fuel pumps pull it through tubes in a foam lid I fitted to the freezer, through the condenser and back. Had one of these and was great while it worked:
Really high capture rates for delicate flavors at high vacuum and low bath temp. That mostly matters for making fresh brandy and stuff like that. Broke after 3 months but I paid for the 3 year coverage and they just refunded me cause they didn't have replacements in country at the time. If I hadn't just bought a -86C freezer, I'd get another and just swap them around as they go tis up. Regular chest freezers from Home Depot can do -25C though and that works just fine for simple ethanol recovery as long as your vacuum isn't pulling too deep of a vacuum.
Not sure I get the point in the CPF. Wouldn't you be better off with a chamber and a pump to circulate through the material under pressure? Would be a lot simpler and you would be able to run it with the solvent at whatever temp you want. A chamber like this but longer:
With DE filtration at the bottom and seals at both ends, you could force liquid though to extract then blow out the remaining solvent with air once you were happy with your extraction. Pressures would be higher since vacuum can't exceed 1 bar so flow should be faster. Clean out would be easy with both ends open, you could just push out the puck. Still seems like overkill given that everything we are trying to extract is on the surface of the material. Insulated bucket and a spatula to stir with is probably functionally fair close.
-Eskander
If you are pulling a light vacuum and using a fairly high bath temp then -5C is just fine. Remember the 20 degree rule for rotovaps. The bath temp should be 20C higher than the BP at that pressure and the condenser should be 20 degrees or better colder than the vapor temp. Vapor temp will be way lower than the bath temp so the only way to know is with a thermometer in the vapor tube. A colder condenser will capture more and saturate slower so your solvent recovery rate will improve. At -40C I had to run insulation over the lines and put the pumps in a styrofoam box to keep them from condensing a half inch of frost but the capture rate was great and I could us a bath temp of 30C. That matters more for distilling things to drink then for solvent recovery though.It holds -5C with a 300mm Graham Condenser on a 1L and 2L fractional still no problem. So I am hoping it is sufficient for the 2L rotovap. Or am I going to need a heftier chiller?
"given that everything we are trying to extract is on the surface of the material." The reason I was using the CPF was to ensure I was leaving nothing behind. The soxhlet process continually circulates a given volume of distilled ethanol until no available ethanol or user stopped. I only used it to pull the last bit after 2 soaks/washes. I can remediate most all undesirables, so I thought I would pull everything. Or is this pointless? Bad idea? Waste of solvent?
Now filtering. That is my next project. I am only filtering down to maybe 2.5 micron with a Buchner funnel and filtrate papers. If I am even achieving that. Also, is it best to do all filtering while in the extracted ethanol solution isnt it? I am hoping to find or somebody can point me towards an affordable simple filtering system. I want '0' particulate if all possible. Small batches, 0.25lb-1.0lb.
Can you explain DE filtration further? The biomass is sealed and pressurized for the 'soak', then released, passing thru filter(s)? If that is the case, I can already do that on small scale with a HTHP Filter Press I have. But only about a 1.0oz batch. I have used it to do BHO extractions as experiments. Can actually soak the biomass in butane with it.
I used 242f I did it on the hot plate in a pot half filled with canola oil, and a candy thermometer, after the temperature stabilized I then put the oil into decarb. I didn't do it in the oven because I thought the oven temperatures would go too far out of whack.Traditional distillation is fine. It will be slower and require more energy that distilling under vacuum but that is the only meaningful difference. The boiling point for iso is low enough that you aren’t really getting conversion to CBN in meaningful quantities. It is also an oxidative process and the solubility of gas (oxygen) in a boiling liquid is essentially zero so it is unlikely to happen at that step anyway.
When you decarb the oil, what temps are you getting it too, for how long and what kind of thermometer are you using?
-Eskander
If there is a functional difference between feco and fso, I’m unaware of it. I think to call it rso, it needs to be the lowest quality of unrefined extract possible though…
If you are stripping color adequately in a slurry then by all means, keep at it. If you are going through celite and are getting particulate still, something is off. Are you using the funnel type with the holes poked in the base or the fritted glass type that I showed? My guess is that you have some liquid bypassing the cake somehow.
You can recover the ethanol to anhydrous With this:
Amazon.com: Magnesium Sulfate Anhydrous - 19.8% Mg, 26% Sulfur - 5 Pounds : Health & Household
Amazon.com: Magnesium Sulfate Anhydrous - 19.8% Mg, 26% Sulfur - 5 Pounds : Health & Householdwww.amazon.com
Just keep adding it and mixing until it swirls around like a snow globe and then filter it and you are at 100% EtOH. That actually sucks for winterizing though and you need to add water to get it back to 95% there or the solubility of wax is too high.
For decarbing oil I either use a hot plate/stirrer or I put it in a retort pouch and run it through the pressure cooker for 20 min. Decarbing flower I do on cookie sheets in the oven. The retort pouch works there too but it ends up smelling like hay and tasting like ass.
-Eskander
I would say it still falls under the FECO/FSO umbrella. It certainly wouldn't qualify as QWET or distillate. I kinda assumed that the order of things went from RSO being extract full of garbage to FECO/FSO being as much garbage removed as possible while still being a long room temp soak.But is an extract still considered FSO or FECO if it has been winterized? I ask because a few compounds are participated/filtered out in the process, leaving the extract 'not whole'. So technically, would it no longer be considered FSO/FECO?
I think it is possible that this relates back to still being cloudy after filtering. The charcoal exposure should be functional either way. Filtering through it might create an even finer filtration cake if it is finely ground though."If you are stripping color adequately in a slurry then by all means, keep at it."
I believe I am stripping colour adequately. Always amber to clear. But my question comes from your comment about the oil tasting like ass.
The batch I mentioned I filtered with a cake of charcoal in tandem with DE, the oil tasted spectacular. Very flavorful. Tasted like the aroma of the bud. All batches without didnt. Could that be why? I noticed any jars I winterized with charcoal present inside, the residual smelled worse than ass. So your comment had me thinking.
Epsom salt is magnesium sulfate hydrate and has essentially zero water binding capacity. you can bake that extensively and it will release the bound water to become anhydrous MgSO4 but I wouldn't really bother. The anhydrous stuff I linked isn't that different in price than epsom salt. 1g of MgSO4 will bind roughly 1g of water. If you have 1 liter of 85% you need to add roughly 150g."You can recover the ethanol to anhydrous With this:"
1) So, Magnesium Sulphate (Epsom Salt) will do the trick. If I were to source it locally, could I just use any Epson Salt as long as it is pure? And is room temp OK to mix?
2) I am going to order the exact product you suggested. Can you give me a ballpark figure as to how much required mg/L for lets say 80%-85% ethanol? This will give me an idea as to how much to order so I have a sufficient stock.
3) So once the ethanol is anhydrous, it will extract better. But for winterization, a water emulsion is desired? So it is fine to extract with 100% ethanol, but emulsify 5%/vol water prior to winterization? As with an emulsified oilwell drilling fluid, I would love to keep water content minimal. Is it possible to remove that 5% from the extract? I can do it with hot lime in an oil based drilling fluid. Mind you these are light oils. Distillates or diesel fuel. Is there a friendly way to do it?
For oil I like 121C for 20 min in a hotplate and for flower 250F for an hour in an oven. You are getting to the point where the better answer is, you need to do some TLC testing and refine your method though."For decarbing"
No offense, but this is the typical reply given. Yes, I know heat and time are required for decabarboxyltion. Regardless of flower or extract. And aware can be done with an oven or heated stirrer. But can you be specific as to times and temps for both? What works for you? This is the problem I am facing. Enough info given to make a person "dangerous", but not enough to get the job done competently. There is still so much secretcy in the cannabis world.
"Water and ethanol are a solution not an emulsion."I would say it still falls under the FECO/FSO umbrella. It certainly wouldn't qualify as QWET or distillate. I kinda assumed that the order of things went from RSO being extract full of garbage to FECO/FSO being as much garbage removed as possible while still being a long room temp soak.
I think it is possible that this relates back to still being cloudy after filtering. The charcoal exposure should be functional either way. Filtering through it might create an even finer filtration cake if it is finely ground though.
Epsom salt is magnesium sulfate hydrate and has essentially zero water binding capacity. you can bake that extensively and it will release the bound water to become anhydrous MgSO4 but I wouldn't really bother. The anhydrous stuff I linked isn't that different in price than epsom salt. 1g of MgSO4 will bind roughly 1g of water. If you have 1 liter of 85% you need to add roughly 150g.
Water and ethanol are a solution not an emulsion. Emulsions are usually cloudy like when you add water to Raki or Ouzo and they go from clear to cloudy called "breaking". That is the oil dissolved in the ethanol being pushed out of solution by the increased water ratio. Drilling muds as I understand them are suspensions that are under high shearing loads which keep the solids suspended while in use. True emissions are stable aqueous/organic mixtures like milk or mayonnaise.
Going from 100% to 95% helps break the solution during winterization and drops the less soluble wax into an unstable suspension. Once you are done reducing the winterized solution in a rotovap, you need to boil off the residual ethanol somehow and boiling off the water at the same time just involves slightly higher temps.
For oil I like 121C for 20 min in a hotplate and for flower 250F for an hour in an oven. You are getting to the point where the better answer is, you need to do some TLC testing and refine your method though.
Back to drying... Nothing precludes adding drying agent to the extract. I'm washing several bags of trim here that are all at 20% RH and I'm periodically drying it back out and filtering it as I process the trim. It is all going to be filtered anyway and some soluble crap from the plants will get salted out if it is anydrous upon filtering. Before the last filtration, I'll chill it to reduce the solubility of remaining salts, sugars and protein.
-Eskander
"Once you are done reducing the winterized solution in a rotovap, you need to boil off the residual ethanol somehow and boiling off the water at the same time just involves slightly higher temps."
This I have been doing on a heated magnetic stirrer at about 100C. End point being when no more bubbles. Is that acceptable? Or should I have the higher temp for decarb and water evap?
"Back to drying... Nothing precludes adding drying agent to the extract. I'm washing several bags of trim here that are all at 20% RH and I'm periodically drying it back out and filtering it as I process the trim. It is all going to be filtered anyway and some soluble crap from the plants will get salted out if it is anydrous upon filtering. Before the last filtration, I'll chill it to reduce the solubility of remaining salts, sugars and protein."
Again, please excuse my ignorance. Could you please explain further? Adding drying agent to extract solution? So there is no chance there could be residual salt in finished oil?
Well, the issue was the grease I was using. I tried DuPont Molykote 55. It was the closest to vac grease I could get locally at that time. I read that it worked as a vacuum grease. DuPont being a big brand, I felt confident buying it. Later that day, I ordered the Haynes grease off Amazon. I was thinking the Molykote was a higher quality grease, so that is what I used first. It is too thin and 'greasy' to work as a vac grease. High potential for contamination. Very messy as well.So, having major issues with vacuum. Cant seem to get vacuum deep enough. Lowest pressure I can get is 411 Torr. Using a 1L fractional still. Has 7-8 glass joints. I greased the living shit out all joints, rotating male/female connections for clear and see-thur glass. I even used teflon tape to no avail.
Tried running 2 pumps in tandem. No go. Has got me fucked trying to figure out issue. I think either pump alone should be able to pull a deep enough vacuum.
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