Im currently looking into winterization and trying to make distillate. I understand the simple process but am looking for tips or really a better way to make distillate in larger quantities at a time while keeping it potent.
How are you getting your crude?
on what scale are you operating?
The tip I can offer from a micro scale refinement point of view is to reduce the size of your boiling flask to the bare minimum needed for production. These huge boiling pots being seen now along with the nature of the crude as it is being a mix of high and low boiling points mean by my standards an enormous amount of time the compound is being held at high temp really just being held in storage at boiling temps waiting for a chance to stop refluxing and get collected - often starting before sunrise and being held that way until sunset.
By itself this appears to be manageable except that into that mix is tossed Volitile Organic Compounds known as terpenes. At least one of those compounds, pinene, is known for instance as an oxidative compound and can be used to induce oxidative stress, especially as temperatures rise. This is useful on its own for some problems but certainly becomes a counter productive reaction during a boil. This might not impact a boil that takes place and is done in say two hours VS a boil that takes sixteen hours. Winterization will not remove these products that create reactive oxygen species from the mix at all prior to boil. There is a simple method to remove this stuff prior to boil but I speak on a micro scale. I also, being a clandestine and largly untrainable sort of criminal type do not have my hands tied in my home nefarious research by laws forbidding certain solvents which gives me enormous flexibility over nearly any commercial bigger operation. By this I mean that I am free to use Hexane or any other solvent legal to use and am not bound by protocols directed by paperwork legality rather than what works best.
The tip is confirmed by my own small scale clandestine lab efforts - the longer the crude remains in the boiling pot and boiling away amidst terpenes while being stored for future collection and such the more likely the crude will degrade and change while still in the pot essentially being used just as a storage vessel. If we dealt only with distilling water then it would not matter but we deal with something that breaks down easily. The question would be why use a 10 liter pot if a five liter pot ran twice will do IF what I say is accurate.
“Watts” is a measure of work energy but is one that generally takes time into account. Watt hours then would be how much energy (in watts) per hour is used. Run the math on your boil. Multiply the temperarute by the time the crude is held at temp and that can give you an idea of the total energy input the crude had to withstand during process while being held in storage and of course would apply only to that which remained longest but the byproducts of breakdown will also transfer because as you know distillation is never a completely efficient way to seperate and there will always be at least some of the boiling pot stuff that transfers along with the good stuff. For this discussion I am not even factoring in the heat transfer losses involved with every single gram of glass in the system that also conducts heat at less than 100% efficiency and by itself represents a huge hurdle so to speak for the crude to cross.
A 5 liter pot held at 190C for five hours would compute to a just made up term of 950 thermal units to process. A 15 liter pot held at 190C for fourteen hours would be is 2850 thermal units input into the crude to produce the same hoped for outcome. The question then often framed as discussions about “mystery peaks” and so forth becomes what does that few extra thousand thermal units do to this compound that is legendary for being prone to thermal breakdown? Toss in a bunch of reactive oxygen species and a mix of other unknowns and suddenly all that extra energy starts to impact quality and recovery in a negative way.
Finally, if you truly want success in business, NEVER EVER put your trust in anybody whose high school nickname was “Beaker” and who claims to know what the hell is going on! I hate to show disrespect for a high school graduate who graduated with a D- average and still believes that Pluto is a planet (it is damnit!!!) but I have not yet vaped today and am still Dr. Heckler. Once vaped, I becomes The Beaker just like Hulk but small, puny, old, and pasty. Watch that guy. He operates a clandestine lab somewhere deep in the shadows of darkest Oregon plotting and scheming… at least until I gotta go potty. Then I mostly just focus on the task at hand and bone up on my technical knowledge with Readers Digest and The Enquirer. Some of the words are big but I manage… 
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Im sort of on the same path for micro refinement. I just started piecing together a small .5L short path because i dont think i can fill any size larger at the moment. I think making a 1/2lb of crude to feed just this is gonna be a task for me monthly, but at the same time i dont think i will need to do this monthly if my calculations are correct. I really only need about a OZ a month of distillate as i make shatter, live resin and other concentrates as well. Im just looking to replace the oz or so of distillate i buy a month by the gram for what i think is a bit too expensive. Especially for someone thats been making concentrates for a while.
Now im stuck on how to recover all the ethanol im gonna need to winterize. Lets just say i use the standard 10:1…so im gonna need about 2.25 liters of ethanol to fully winterize 1 run. Since 190 proof is very hard to get my hands on, how would you guys go about recovering the ethanol i use WITHOUT a Rotary Evaporator.
Right now im thinking of getting a megahomme distiller to recover the alcohol before distilling. I really dont have the money right now for a rotary evaporator right this second. It is on the purchase sheet for 2018 but i just dont have the money to pluck down $1500 more on a rotovap.
Thanks for the advice in advance…hopefully this will help with the OP question too as im pretty much sure this question will come up if they are micro refining too.
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125.00
Tabletop alcohol distiller on ebay
I use that when not enough to toss in the rotovap
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When I recover solvent I use simple distillation as a rule but use a two,or three neck 250 ml boiling flask. Into the side neck I put my separation funnel used this way as an addition funnel. I just keep feeding from the sep funnel as the level gets lower in the boiling flask. It is all 24/40 joints. Once the mantle is hot this can process a lot of solvent pretty fast.
Of course then your options at purifying further via fractional distillation are well known so any sort of fractioning distillation rig will do. A rotary evaporator is not necessary at all for solvent recovery and in fact unless you process daily I could not envision that one of those would be much more than a very nice luxury piece of gear.
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$55 water distiller, PID or on/off or limit selectable controller with mechanical relay, Variac for power regulation, Kill A Watt P3 volt/amp/watt/kW-h meter.
The cheap Chinese water distillers are 750 watts. MegaHome’s 580 watts, MegaHome’s alcohol distiller is 330 watts. First pass at distilling vodka down works fine at 330 watts, my next passes are at 125 watts or less on the meter (the meter and Variac use 16.3 watts, 9.6 watts for the Kill A Watt, the Variac 6.7 watts.) I’m doing probably the final distillation on a batch I’ve already taken to 90.5% BV using only 100 watts on the meter.
I’m posting up about my experiences here,
and here (where I take a cheap Chinese water distiller apart and mod it - though that’s not necessary, also info on advanced controllers with both power regulation and temperature control,)
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@Demontrich your referring to one of these. Similar to what @SkyHighLer posted right?
https://rover.ebay.com/rover/0/0/0?mpre=https%3A%2F%2Fwww.ebay.com%2Fulk%2Fitm%2F153129758442
I’m not so much on the path of making 95% ethanol like @SkyHighLer as much as recovering 80% percent of what I have. I feel like a traditional still and thumper would be more economical in making high proof ethanol which I might try to while down the road. In searching for the electric still I found several 5-8gal still with thumpers for under $150 and for that price and my ability to do this once a month. Making my own high proof ethanol might worth it, but then again I’m lazy and my friends already send me down cases of 190proof ethanol already. Why not keep doing it and recover 80% now. Lol.
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That’s the one. Works great for a small run.
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What type of controller does that unit use Demontrich? Does it vary the wattage to the heater, or does it hold a set temperature like a PID controller?
Astute observations from a seller of modified water distillers:
"This countertop still can store out in the open and is easy to operate, just plug it in. If you haven’t operated a still/distiller before, the main concept is this. Water boils around 212 degrees and alcohol boils at 172 degrees. If you have water with alcohol in it, the alcohol will boil out first. The key is to cook it slow and collect the alcohol before the water boils. This distiller has been modified to run on reduced wattage that allows the boiling process to maximize the production of alcohol. Regular water distillers cook at a much higher temperature and will not work for alcohol distillation. You will end up with low % of alcohol or a boiled over mess. Once the unit slowly heats to produce the alcohol vapors, the cooling coil on top of the unit condenses the vapor back to liquid alcohol and drips down into your collection jar.
This unit does not limit the boiler temperature. I have modified distillers with this modification in the past and the reduced temperatures do not allow the boiler to build enough head pressure to fully collect your alcohol. This unit has a modified heating element to control how fast the boiler heats, allowing the alcohol to fully separate itself from the water and be collected fully without the water diluting the final product."
From here,
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It/mine has a temperature dial to vary the heat. You can, I have, remove the stop screw and run it at a higher temperature than normal, or higher than your supposed to. I dont any longer.
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Really appreciate it guys. You just saved me a nice chunk of cash. I thought the rotovap was a little much for someone that only wants to really distill about an OZ a month.
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You guys are really great, i will be comming back to this site for more tips forsure!
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Here’s the same unit for only $101.88,
And a unit with digital readout for $99.99,
Both units are thermostat controlled, they limit temperature only, not wattage, they turn the full 750 watts of the heater on and off and on and off… The MegaHome Alcohol distiller is dialed down to 330 watts, and I dial my distiller down to 100 watts for the final distillation.
I tried substituting a cheap power controller for the Variac I use to lower the wattage of my water distiller. It works ok, dialing exact wattages isn’t nearly as easy, but can be done.
To use a cheap ($55) countertop water distiller to distill alcohol I suggest you at least lower the wattage, this can be done simply by plugging the condenser fan in with it’s own plug, and then feeding the base unit through either a Variac or solid state power controller like I mentioned above, the wattage is monitored with a power meter before the Variac or power controller.
What you need:
- Water distiller
[url]water distiller for sale | eBay
- An extra appliance cord (one comes with your distiller, you need a second one) to plug the condenser directly into the wall
- Power meter
- Variac or solid state power controller
[url]20a variac for sale | eBay
or
[url]https://www.amazon.com/gp/product/B00OZ5MBM6/ref=oh_aui_search_detailpage?ie=UTF8&psc=1[/url]
That solid state power controller is simple to wire with just an extension cord (see the picture below.)
No taking the distiller apart or anything. You just adjust the power to a 1-2 drip per second rate, note the wattage for the next time, and taste the output until it’s water or near so.
To go further you need to open the base of the distiller, and add a thermocouple for temperature readings and/or temperature controller input.
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