Lolz I just vaped it. Keep in mind this was the ONLY way for me to distill extract at ANY kind reasonable temps. As you likely know this is the old school way of disitlling thermally sensitive compounds. In this rig the temp at the head rarely exeeds about 115C and runs easily albeit slowly at 100C. 115C is where is really starts to work fast and obviously requires higher boiling flask temps and then starts to superheat the steam just a bit.
Other than that the method runs the same as vacuum distillation. Terps fracion off first and boy howdy does my home smell like a pine cone when that happens! Remember this is not a closed system so you can smell what is happening.
The difference between steam distillation and vacuum distillaiton as I ran it was almost zero really. In other words multiple runs through the rig are needed for higher purity. If you look carefully at the rinse off portion you can spot around one of the water pocket bubbles a mistake I made. I saw dark tails start but kept running it a short time and you can spot some dark material around one of those pockets. The two other differences are steam distillation is slow comparatively and of course water purge issues need to be addressed.
This is not my first steam rig either. The first ones I guess the vids did not get archived and GOOD! They were VERY efficient and FAST producing distillation butā¦ embarassing to sayā¦ I felt the only way to do this at the time was a single vessel and not to inject the steam but rather add water via addition funnel onto very hot oil. This meant continuous multiple explosive releases of water vapor. This means the steam would get trapped under the puddle, then superheat as steam, superheated steam becomes explosive (think Mt. St. Hellens) and the superheated contained explosions produced RAPID disitillate in the condenser. Superheated steam was used when I was a kid on the farm in Central Oregon to extract mint oil from the mint crops. That is how I knew how it worked although they donāt just dump water onto the top of hot oil. The machinery is well thought out. My try was foolhardy to do this but it worked GREAT at pulling across the fractions. This is not a new idea to me at all because I learned it as a kid in the mint fields but my implementation was unsafe.
Those mint rigs were built of heavy steel and such. Here I was running the process using superheated steam (in a way unsafe and different fashion) as if to extract sensitive mint oil but only in a glass rig! Face palm moment and after each run then the boiling flask would develop the start of tiny cracks in the bottom. The steam injector is much safer and I do not allow the superheated popping now. Even then I was seeing cracks in the boiiling vessel after several runs and now believe my error was in not having the boiling flask temp set high enough to avoid the sharp thermal spike created by the steam at point of injection.
That whole explanation and processs though is really a post on its own. In fact I might rig up again for a complete run and vid showing this because it is hands down the cheapest and most effective way to start a career distilling this stuff. No vac pump is needed and I stopped refining my process further when I could get set up with a vacuum pump that could pull well enough to distill.
On a commercial basis or if I could never afford a vacuum set up I would have modified the rig to be all metal and there are a few refinements otherwise too but once set up like a mint still (which are enormous machines pulled into the field) as a metal superheated steam injection system the throughput can be very high .
All that being saidā¦ as I mentioned I grew up on farms doing this sort of thing. Never EVER underestimate the horrific danger of superheated steam. One foot away and the day is happy. Get hit by a blast and life becomes very unhappy for a long time if you survive past a week. Like anything explosive and hot it MUST be engineered to handle it if you go the superheated route. This rig shown is NOT a superheated style.
I have hardwood floors and use a steam mop. Here is the picture. If I were to engineer a unit for production I would just modify the output of this to provide steam injection instead of the lab rigged way shown. This unit is the PERFECT steam generator and comes complete with a handy flexible hose so routing is easy. Plusā¦it is cheap!
ā¦and you used to be so adamant about that slow stirringā¦ silly man! Itās really awe inspiring to see the breadth and scope of your understanding of this distillation procedure, and it is why I have sent several people to you to consult. I am so very pleased with your open-minded approach, and always excited to teach you new things! I am more impressed with your application of your knowledge every day, and I sincerely appreciate being able to help you on this path! You are the man, as they say!
Was i adamant about slow stir? Watch some videos from 3-4 months ago. Youll see 5-10L of crude spinning so fast you can see the stir bar. But i will say that stir greatly affects the vacuum depthā¦ as it should. I find that stirring slow until 60C is just because trying to go fast is impossible with the puck of solid crude that the stir bar runs into and losses course because of. After that all bets are offā¦ id use an overhead stir if i could find a good high vacuum one.
Was it failry easy to rebuild, I usually send them out to be repaired but I would like to know how to do it my self. Was there any special tools you needed to have.
@anon42519203 Iāve read this Tek and all of the comments about a dozen times and Iām still learning things. Your process is amazing and Iām very keen to modify my 5L to work on your shotgun approach. I believe I already have most of the parts I would need to put the set up together except for the ability to bring the head condenser temp to 155Ā°c. What are you using to achieve that temp? Is it a full spectrum chiller or do you have another (potentially less expensive) way of maintaining that temp in the condenser? The warmest I can get my chiller is 40Ā°.
Much like yourself I started in this industry with no real world distillation experience (just my undergrad in Microbiology with some limited exposure to distillation in O-chem and biochem). I am also just getting started. Iāve done 2 runs so far on our stock Lab Society 5L. While I am getting clean, transparent, and relatively smell-free distillate after a second pass I have been struggling with purity. While the product looked and smelled great the testing has been in the mid 80s and even as low the high 70s (which is embarrassing to admitā¦ Though there is a good chance our lab is giving wonky resultsāWe donāt have in house testing yet and weāve seen results all over the map from them).
I believe the time it takes to get through our runs as well as the high vacuum levels is causing isomerization. Each run has taken significantly longer than expected as I was constantly fighting the vacuum during the ramp. The first pass on my last run of about 2200 grams of EtOH crude (winterized 3 times in dry ice and decarbed at 140Ā°c prior) took just over 17 hours. Second pass took just over 13 hours. On the first pass the lowest I was able to maintain the vac was about 850 microns, but it was frequently above that. Second pass was closer to 300 microns. After reading this I am convinced that a good chunk of my vacuum issues are due to leakage from the numerous gl connections in the system as well as the stock thermocouple adapters. I also think the turbulence caused by going from a 24/40 condenser to a 5/8 gl connection at the cow is holding me up. I can see very clearly that your set up will give a deeper vacuum by way of fewer leaks and less turbulence as well as higher a throughput. However, given that we just purchased the system a few months ago I doubt that I would be able to convince the powers that be to invest in any expensive equipment to modify it, assuming that is what is required to get the head condenser to temperature.
If I am not able to achieve the 155Ā° at the head then my only option seems to be modifying my current set up. The thermocouple adapters could easily be switched out to thermowells (which I was going to do anyway). I canāt do anything about the turbulence but would connecting my vac lines directly to the glass using hose clamps be a good way to eliminate the gl connections? I am currently using reinforced vac hoses but I do have a good amount of black rubber vac hose I could use instead. Do you have any preference between those two? Are there additional purification steps for the crude that would help such as enzymatic dewaxing and/or carbon scrubbing?
Sorry for the barrage of questions. Your post and the great comments that followed have a lot of thoughts spinning in my head.
Let me offer an alternative explanation regarding the vacuum levels you mention. If that sentence was isolated away from the rest of the post I would look at it and think that what you are describing is not a leak in the system but rather an indication of the percentage of volitile organic compounds (VOCs) left in the boiling puddle. A confirmation of this would be to run a third pass and see if you pull down even further. If it does and everything else is equal then that is what you are noticing likely. VOCs evolve rapidly during these operations and it is not an error condition. The vacuum determines the boiling temperature but the āboilingā determines the vacuum level achievable. Lots of gas boiling raises the pressure and vacuum depth suffers during this. However when the vacuum progresses deeper as refinement progresses it would normally indicate expected operation in my rigs because the VOCs begin to deplete. I run very low temps comparatively to a standard distillation SPD.
I see this behavior and almost identical pressures on starting extract when run in my micro scale distillations. I can run low temps and as the pressure drops slowly from hundreds of microns the terpenes keep collecting. As the pressure apporaches about 40 microns terpene collection slows. At about 10 microns terpenes and all VOCs are depleted from the boil. I run a boiling puddle temp at 135C nominal. I normally run the pressure down to one micron then remove the terpene fraction collected and proceed with the run collecting D9 THC.
@Beaker This was also a theory I was floating around after seeing the vast difference in pressures between the first and second passes. I had considered prepurging the crude in a vac oven overnight after decarb. Alternatively I was thinking that I could just load the crude into the boiling flask, set the temp to around 75Ā° to 100Ā° and let it sit for a day or so to purge in the system before begining.
When you say you remove the terpene fraction collected before proceeding to the D9 fraction do you break vacuum? We had a consultant come in for our initial run to get us started and he used an approach that involved ramping to 140Ā° at the top of the column with a single distribution adapter then breaking vacuum and switching out the condenser and changing to a 3-way cow before resuming the vacuum proceeding into the main fraction. Your process sounds similar except with a lot more patience. Just to make sure I have this right you are ramping to 135Ā° in the boiling flask quickly, vac be damned, then sitting at that temperature letting the vac drop until the VOCs are in range to come off? How long does it usually take for you to get to 135Ā° and how long after you get there do you see the vac come into range?
While I do agree that a large part of the problem is the volitiles I also definitely have a problem with leakage. The lowest I have gotten an empty system is about 135 microns. While at this point I would sell my mother into slavery to maintain that durring a run it is clearly not good enough to get the purity I want out of this product. Do you think eliminating the gl connections by going straight to the glass with hoses and clamps will help or is that just folly?
I am currently running an AI SuperVac for my pump. After a few oil changes I can get it down to about 6 microns blanked off with a thermocouple meter. We have a Welch 1402B currently being rebuilt that is intended to replace the SuperVac. The Welch should be able to pull down to 4 or 5 microns blanked off. Having seen @anon42519203 set up I am now thinking about getting a manifold to run the two pumps in parallel. I would pull down the volitiles with the SuperVac and when it comes time for the main fraction I would kick on the Welch. Thatās the plan, anyway.
Yes I do break vacuum often to deal with volitiles. I remove terpenes in bulk as a seperate process. Usually I have used a horizontal rig to pull just the terpenes out then pour the boiling flask into the sublimator. Then the trace terps are removed from the cold finger once the vacuum drops below about 10 microns or so. They just get wiped off and the finger is acetone clean.
I can and do now remove terps with a liquid to liquid extraction and plan to no longer boil them out. Either way I remove the terpenes prior to attempting to fraction the THC.
As far as temperature I set it at the target and there it stays. I do adjust but not at first when the VOCs are evolving. I can easily see a 1000 micron reading at first but it pulls down fast to say 300 microns. Then slow but sure it keeps ticking down as fewer VOCs evolve into gas. If the pressure is slowly dropping then it is contraindicated to raise the temperature in this case because what you will end up doing is unbalancing the equation the other way.
By this I mean I assume you want to fraction as cleanly as possible. If the pressure is dropping and not as a result of a leak then the equation is balanced in your favor because one fraction alone is depleting. If you turn the temp up and the result is a pressure rise then you are no longer only evolving the VOCs as a gas and fractions then overlap.
Let me suggest to you a vacuum valve like the one I purchased.
Place this valve just an inch or so away from the inlet barb on the distillation rig so you can blank off the pressure right at the rig. Now fire it all up and begin distilling. Once you are up to temp and the distillation is proceeding blank off the rig but keep the pump running. The vacuum should immediately pull down to some lower value.
If it does then you can get an idea of how much is evolving in the flask by subtracting pressures. Then blank off the pump at the pump too. If the pressure in the system with both ends blanked off falls steeply and does not flatten out it is a leak. If it flattens out at say 1000 microns and only bleeds off slowly then that would seem normal to me and the problems if any then would be isolate to either or both ends.
Then here is another test as you quickly return the system to full vacuum. As it runs note the pressure. Now crack open the three way valve to allow fresh air to be gulped into the system while running. The vacuum should bleed off considerable. Do this for 15-30 seconds then seal back up and watch the pressure. Did it plunge a bit below where it was before the air purge? Sometimes it will and stay there but if it goes below and creeps back up then pump oil contamination is indicated. Sometimes a purge like this three or four times in succession will clear my system and allow it to pull deeper vacuum.
Here is the instagram slide show that talks fast about it. Today I am getting some more crude as well. I believe this same LLE technique but flip flopped from one sep funnel to the next so to speak can also dewax and remove chlorophyl with a very carefull mod. Do you see what I see in the slides and the green? then reference back to my post about waxes being disolved. Methanol doesnāt touch them but hexane soaks en up instantly. I have already run a twelve tube counter current sep lab twice to see how this could be exploited but missed the forest for the trees metinks.
Perfect! Thank you, Sir! Yes, I am very aware of how this type of ālouching alcohol partitionā works to pull color, some terpenes, and how waxes always fly to the purely np phase (just like cannabinoids) which is why I always Winterize in the ethanol that Iāve used, first.
@Beaker very interesting! Iāve read some of your other posts on louching and Iāve been keen to give it a try. I do not have access to methanol or hexane. Iām working in a medicinal facility with tight state and local regulations on solvents we are allowed to keep and use. Iām currently trying to get acetone just to clean my glass!
I currently have access to oodles of EtOH (190 and 200 proof) and we have tentative approval to begin using limited amounts heptane. We were planning on using the heptane in order to perform a saline wash but would it also work for louching? I would say so but I figured it wouldnāt hurt to ask. While we are all here.
I am unfamiliar with the term louching but the idea with methanol and hexane is that they are both immiscible in each other but they both also disolve the compound of interest. They happen to be at opposite ends of the polarity chart. I would predict any combo with a similar relationship would be about the same.
Other than methanol, hexane is miscible in just about everything else so using it this way with another alcohol would be something very different and would be a completely different mechanism really.
I have seen unique layers form under circumstances using acetone, hexane, and isopropyl alcohol though and all those are miscible in each other so it is just hard to know until you try. However the core of what I presented is the idea of two immiscible phases that both disolve the compound as a starting point and that would not include ethanol - only methanol.
Yes, I see what you mean. I just consulted a helpful chart on solvent miscibility and while it looks like heptane will work well in place of hexane I would still need methanol as a second solvent. Ethanol seems miscible in just about everything so thatās out.
Looks like I need to call the fire cheif and ask for more solvents!
Louching is a term I use for adding water to an alcohol to precipitate dissolved compounds in the form of a milky microemulsion, @Beaker . It works with ethanol as well as methanol, it would appear. The water also keeps the ethanol or gets the methanol out of the np phase. @TheLostBiologist
