For anyone curious, a vacuum chamber paired with a magnetic stirrer and set in a warm water bath followed by a cold trap is an effective recovery apparatus.
I definitely need to dial in my temperatures a bit more. I used 20 lbs of dry ice to recover 1.75L and that seems a little excessive. I’m maintaining temps by adding dry ice directly to my isopropyl cooling baths and by swapping cooled warm water baths with freshly heated water. Temps were between -20 - 0°C on average in the cooling baths, and ranged between 30 - 60°C for the warm water bath. Internal temperature of the vacuum chamber ranged from 20 - 46°C. Vacuum started at -27inHg and settled at -25inHg. Interior cooling bath was 1L, exterior cooling bath was 3L, warm water bath was 2L. I couldn’t maintain a stronger vacuum because it was making my pump sound unhealthy. Any thoughts or advice?
P. S. I noted an unusual phenomenon. Where the solution wouldn’t bubble when the stir bar decoupled from the stirrer magnet it would boil once the bar was recoupled to the magnet, even when the magnet was not being turned. Just something of note.
Like an empty condensing coil inside of a container you fill with your cooling bath mixture? Or the standard coil of cooling liquid inside of an empty chamber for condensing?
I had originally been playing with the idea of using a coil submerged in a cooling bath that would have an ethanol vapor stream going in and a liquid stream of ethanol coming out the other end, but it’d been suggested by a fellow member that might be overkill.
Purge pot in hot water bath mag stir under beaker inside pot line going to coil inside cooler w modified ac unit for bath coil to another purge pot 2nd purge pot to vac pump I didn’t think of a small coil inside a purge chamber I think more cool fluid around the vapors vs the vapors around the cooling coils will do a more stand up job
Modified ac unit for cooling? I tried to find some information online, but couldn’t get anything. Care to elaborate?
It occurred to me before starting today using small chunks to keep things cold is only increasing the rate of evaporation of the dry ice by increasing surface area. I’ll be trying large chunks today to see if that helps reduce usage. I’ve also added towels for insulation, better than nothing. I still wonder if I’m running either too warm or with too much agitation for how cold my cooking liquid is. I need to find some good formulas on heat transfer from phase change and a few other things to better dial this in.
Also, if it is possible to reduce the amount of solvent to filter by recovering a portion of it without damaging the quality of the oil I highly recommend it. Filtration through a thick cake of t-5 with vacuum is extremely slow. 6hrs or something to filter about 4L.
Nice, thank you guys. Not overly excited with my results after second filtration. There’s got to be a lot of leftover pigments in this stuff. Gonna try a filtration at super cold temps, around -40°C to see if that helps. I’m not getting anywhere near yellow this time before going into full recovery. I’m sure it wasn’t the reduction, the liquid in the chamber never got above 30-31°C.
Leaning back towards purging this completely onto silica and dumping it into a mini closed loop on top of a bed of silica and t-5 then running with butane for its nonpolar nature. We’ll see what happens after the cold filtration.
I was hella tired so I just let it winterize at around -45°C over night. I’m going to let it keep winterizing until probably tomorrow morning then I’ll filter the fats, rechill to -40°C and run over t-5. So we’ll be hoping removing the fats and filtering at subzero will result in the pale yellow extract we desire.
My first filtration was through carbon and t-5. So essentially t-41, but using all neutral pH medias. I stopped using carbon once I could tell it had effectively removed all the green hues I was seeing, unless the are still some minor amounts present that are contributing to the brown coloration I currently have.
I really need to quit dragging my feet and get some silica and maybe even some activated alumina.
I tried making my own t41 using hwc and ac mixed at different ratios with t5 but couldnt get the same results as using prebought t41
Sometimes to do with the um difference
That and the pH differences between the medias you used to recreate it and its own pH of 3. pH of the media and solvent play a large role in these processes.
The similar particle sizes is important for keeping a good mix if I’m not mistaken. Think about how shake ends up at the bottom of the bag, but large bits end up on top as things move around. No matter how hard you tried to get them mixed evenly, the carbon would want to end up at thre bottom.
Filtration through AC and T5 should be all you need. I use it regularly and am super happy with the results. I make a slurry of the bentonite with ethanol to make the puck (on 6" filter plates). I then do the same thing with the AC (we use hardwood). 1/2" to 3/4" for the bentonite layer and 1/8" for the AC. Seems to do a bit better when we filter cold but have achieved the same results with warm filtration as well. This is what 3 passes should get you:
Those results seem awfully remarkable. Can you run us through your extraction process? Cleaner input equals cleaner output so I’m assuming you have a fairly clean starting extract.
cold for cheap!
