Alcohol Fractionating Still

The Enabler Alcohol Fractionating Still

While messing around with passive butane essential oils extraction and recovery, it occurred to me that with very few extra pieces, the new Skunk Pharm Research passive butane extraction and recovery system could also be used to turn 80 proof drinking alcohol into 190 proof, for those of ya’ll who are unable to get 190 proof for essential oil extractions.

If we use the butane storage and recovery tank for the boiler, and the lid from the BHO recovery tank, we can install a 36″ tall stainless sanitary spool for a refluxing column, packed with stainless steel pot scrubbers.

A sanitary cross at the top will provide ports for a thermometer, a refluxing condenser, and a product bleed.  A product condenser on the product bleed port will condense the vapors bled off from the upper chamber, and the temperature of those vapors will tell you what they are.

Check with your personal attorney for their read on local laws, but by using the butane recovery tank, the volume of the boiler is under one gallon (.86), the taxes on the alcohol that you are condensing have been paid for, and it is used for extracting essential oils, not drinking.

In theory, the still could just as easily make 190 proof out of a ferment sugar wash, but that is illegal at least here locally, so we are not recommending it for that use where prohibited.

Here is a conceptual of how such a system might work, and here is a picture of what a 36″ column with cross looks like.  More when the parts come back from the welder and machine shop.

As with the passive extraction system, most parts are off the shelf.

Hee, hee, hee, ahwooooooooooooooooooooooooooooooooo

Enabler Configurations

Progress has been made.  I picked up a dozen of the stainless pot scrubbers at Hongs Restaurant Supply for $5.99, and after I first pulled them apart, I rammed them firmly into the column, using a hard wood dowel.

They are held between the two combination Viton gasket/10 mesh screens at each end of the column, which I scored from brewerygaskets.com.  I chose Viton because of its compatibility with hot ethanol.

I recommend this Cole Palmer site, for choosing alternate materials from what I have used here, should it be more readily available:

http://www.coleparmer.co.uk/Chemical-Resistance?referred_id=1033&mkwid=smji51NEu&pcrid=15195968645&gclid=CNfn8YSciLECFWYbQgodGUVoPw

The science behind the 1 meter column packed with stainless ribbon, is that the large surface area of the ribbon continually cools the rising vapors until the point that they cool to a liquid and rain back down the column.

Eventually the vapors will heat up the insulated column, and they will rise higher and higher in the column, until the column and its contents reach thermal equilibrium.

Because of this continuous refluxing action, when it reaches equilibrium, the lowest boiling point vapors will be at the top of the column, and the heavier vapors below them in the column.

Because I would like to do this in a 1 meter column, I have elected to install an Alhin refluxing condenser above the column.  This refluxing condenser condenses everything that rises above the packing, so that a shorter column can be used.

There is a digital thermometer in the cross below the refluxing condenser, with the probe far enough back, so as to not be affected by the temperature of raining condensate.  It tells which constituent is at the top of the column, by the temperature of the vapors.

Bleeding off the fractions:  

There are a couple of standard ways to bleed off the fractions, with one called liquid control, and one called vapor control.

With liquid control, you capture some of the liquid raining down from the reflux condenser at the top of the column and bleed it off.

Instead of liquid control, I will be using two different vapor control techniques with this fractionating still.  I will detail them below, but the principle with both liquid and vapor control, is that if you provide a means to extract the liquid or vapor at the top of the column at a slow enough rate, the column will continually reestablish equilibrium, and you can bleed off that constituent.

The rising temperature tells you that the next constituent, or an azeotrope of that constituent has reached the still head.

Providing a bleed path using vapor control: 

You will notice that besides the Alhin reflux condenser at the top of the column, there are two Liebig product condensers that come into play, depending on where the vapor stream is coming from.

Path A is created by cracking the valve  on one leg of the cross, which allows some of the vapors at the top of the reflux column to exit through the Liebig condenser, where it is cooled to a liquid.

This technique relies on the fact that water steam is lighter than air, at 0.6 its density, while ethanol vapors are 1.6 times as dense.  That means that given an opportunity, that the steam will rise and the ethanol vapors will sink, until their concentration falls below about 41% by volume in the top of the column.

This is a handy feature if you are making ethanol from scratch, as you can strip the wash with the valve wide open, and the product will drop off as the critical temperature for tails is reached, making the separation easy.

Usually the first constituent to reach the head of the still will be the Ethyl Acetate, and Methanol, which are bled off and discarded, followed by their azeotropes with ethanol, called the heads.

After the heads, comes the purified ethanol, until it reaches about 41%, at which time the tails arrive, with fusil oils and other cogens.

The advantage of this type of vapor control, is that the temperature and flow of the incoming water to the condensers isn’t as critical, and it is self regulating on shut off.  The temperature will not only rise, but product through the Liebig condenser will dwindle.

Path B, provides even finer separation of the constituents, but does rely on regulating both the flow and temperature of the water to the Alhin refluxing condenser, because we will be using it as the control point.

The way we operate it, is to run it in full reflux mode until it reaches equilibrium, and then start cutting back the flow to the Alhin condenser.  That will permit the very lowest boiling point constituents to flow up and out the top of the Alhin, where it is directed through a Liebig product condenser and cooled into a liquid.

The advantage is very fine control, but it has to be monitored more closely and cooling water pressure, temperature, and flow are more critical.

You can also achieve the same effect by leaving the flow through the Alhin reflux condenser constant, and cranking up the boiler heat.  Less system losses, the amount of heat added by the boiler, has to be removed by the reflux condenser to stay in balance.  Increasing the heat will drive the vapors out the top of a finely balanced heat exchanger, just like reducing the cooling capacity.

Pot still:

For those applications where a simple pot still is just the ticket, with the Enabler’s modular design, the head cross can easily be attached directly to the boiler itself, eliminating the column altogether.  Hee, hee, hee, what could be sweeter?

GW

17 responses to this post.

  1. Posted by Matt on December 29, 2013 at 9:39 AM

    Can this be used to fraction BHO? Could you load it with bho in a carrier oil with higher boiling point and then isolate different Cannabinoids by their vaporization points

    Reply

  2. All the more reason for me to built the little terp. 10/10. brilliant post. Anyone interested in recipes for fine liquors and more still plans should check out http://homedistiller.org. I’ll enjoy making absinthe with this…kinda want to use cannabis as an infusion herb in the coloration procedure

    Reply

  3. Posted by Bobby G on October 21, 2013 at 1:14 PM

    how cold is to cold for winterizing? would it beneficial to get colder I’m having problems of it warming up too fast. Thinking about using dry ice under the mason jar in the freezer. the coldest I can get to is -8 it flexes for -1 to -8.

    Reply

  4. Greeting, Im new to the discussion and passionate to assist others, I recently purchased a Coldfinger extractor from edenlabs and feel that there are steps missing with this piece of equipment in regards to creating a pure smokable essential oil, are there any ways to modify this unit to better utilize it, or use it in conjunction with another apparatus to reach the desired outcome

    Reply

  5. Posted by Robert From San Diego on October 6, 2013 at 7:33 PM

    Has this been built and tested yet?

    Reply

  6. Posted by Sebastian on June 14, 2013 at 9:16 AM

    Dam look at that old grey wolf hand hahaha ;)

    Reply

    • Hee, hee, hee, snicker, snark, snort…….My hands have always looked ancient. When I was a kid, my mom used to tell me that my hands looked like they had worn out a dozen bodies, so I guess it must now look like at least thirteen worn out bodies.

      Reply

  7. Posted by Pete on March 4, 2013 at 3:48 PM

    I appreciate the design, what adapters or fittings are you using to reduce from the 2″ sanitary cross to the glassware? My glassware has a diameter of just under an inch. Also have you thought of doing a distillation under vacuum?

    Reply

    • Solly to fall behind bro!

      Excellent question, and yes I’ve considered vacuum as a way to tilt the azetrope toward the alcohol again.

      The issue I am trying to resolve at this point, is my abysmal recovery percentage under vacuum compared to a simple compound fractionating or even a pot still. I am still losing too much through the pump, so I need to go to a colder trap, lower flow, or to more surface area.

      Dry ice and acetone would resolve the colder cold trap issue, but would be an added hazard to deal with.

      We picked up a small liquid nitrogen Dewar and plan to run some experiments using a liquid nitrogen cold finger, but the whole purpose of our Enabler design, is something that most ma and pa patients can whomp together, with few modified parts, to make or condense ethanol for extracting their meds, where it is legal to do so.

      The added complication of vacuum distillation would be a push for many, so perhaps there needs to be a Mk I ma and pa version, and a Mk II professional version. Hee, hee, hee………

      Reply

  8. I am not Sure if this would apply here, and the stainless scrubbers are easy enough to find most Anywhere. I have a buddy who built a still that he used for various applications including essences for candy, baking, being a chef in general. It was also used for alcohol. Instead of the scrubbers, he had glass marbles in what I guess would have been the column of the still. Worked a treat for him. Thanks for all you do!

    Reply

    • Yes, glass marbles will work as well and are easy to clean, but don’t have as much surface area as the stainless ribbon, so it takes more of them to accomplish the same effects. You can also use commercial Raching rings, which ostensibly would work even better than ribbon.

      GW

      Reply

  9. Hello, I’m in the cannabizness in CO, and also made a living doing industrial design for a few decades, now working on making better canna-extractions. My current goals are in building or buying an affordable CO2 extractor, and also a much bigger bho recovery-type extractor than the current Tamisium unit I have (and have a lot of issues with, notably recovery time too long). I like your open format, and may have something to contribute too, with an idea to build on what you’ve done. I would be interested in fabricating your latest iteration if that’s ok with you? I don’t do my own machining but apart from that I do have a good fabrication shop, and good machinists including cryo. Also curious if you have a favorite supplier for the stainless klein fittings? I would really appreciate a chat if you have the time.

    Reply

    • Hi Tom, please feel free to build anything I have published, and improve upon it for your own purposes as you see fit. I am delighted at how many folks world wide have been doing so, and how the idea has caught on.

      I will update the Mk III page, to add part numbers, and so that the landscaped parts list that I posted is reduced small enough for you to see the complete page showing resources. Currently the whole right side of the spread sheet is not visible.

      All of my sanitary fittings came from Glacier Tank here in Portland, and I have provided Rochelle at that location, with a complete parts list, which they will assign a part number to. They have also agreed to start stocking the specialty sanitary seals that we use, so that it narrows the number of vendors required down to Glacier Tank and Paramount Supply.

      I am in the process of making similar arrangements with Bob at our local Portland Paramount supply, so that all that will be necessary for builders to pick up a complete kit, is to ask for it by part number.

      Good job on having good machining resources. Good technical support makes things easy and building a Mk III could hardly be simpler with a good machinist and TIG welder, as there is only the lid assembly and injection tee to build.

      The rest just screws or clamps together.

      I deleted your phone number from this post, but will try it about mid morning today and if I miss you, I will leave you a contact number.

      Peace, GW

      Reply

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