Separating the oils from the alcoholic beverages?

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Edenhazard
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Separating the oils from the alcoholic beverages?

Post by Edenhazard »

Hello,

I have been really struggling about an experiment for a significant time and so I have doing some research for a long while, about separating the volatile compounds (essential oils etc) from fermented alcoholic beverages (wine, beer) or from distilled beverages (absinthe,Pastis, raki etc) or from distilled spirits before their purification (vodka,whisky etc) . For some reasons, the oils stick to the hydro alcoholic solution. The alcohol and the oils form an azeotrope and they distill together.

I tried diluting to form a solution, changing temperature, changing densities, adding non polar solvents like hexane but the oils would never separate. I would get a stable turbidity/emulsion at most.

It is possible to get more info from people who have knowledge/experience about terpeneless oils, centrifuging, purifying distilled alcohol from other volatile compounds (in case of distilled spirits like vodka and whiskey), molecular sieves or chromatography..

The alcohol I distill always contains volatile compounds even if the temperature is very precise). Whenever I add water, the distilled alcohol forms a solution (whether it is the first, middle or last distilled portion)

Any idea?

Thanks for your time
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Re: Separating the oils from the alcoholic beverages?

Post by jonnys_spirit »

I feel like it’s best rendered in a complex biological process.
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jonnys_spirit
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Re: Separating the oils from the alcoholic beverages?

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79726689-5F25-4235-8D1C-96536C9D7D53.jpeg
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Re: Separating the oils from the alcoholic beverages?

Post by still_stirrin »

Whatcha’ makin’ Edenhazard? I really wonder if it belongs on our website. Your questions lead me to be doubtful.
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Re: Separating the oils from the alcoholic beverages?

Post by LWTCS »

Are you trying to do this on the fly?
Or after dilution to bottle strength?

Large scale production uses a decanter.
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Edenhazard
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Re: Separating the oils from the alcoholic beverages?

Post by Edenhazard »

OK. I read some threads here so I will reformulate the questions.

Anyone used fining agents (like charcoal or bentonite) or some specific types of filters to separate oils from distilled spirits? (like gin or vodka). By doing this, a liquor that previously louched will not louche again. All flavors will be lost as well and the alcoholic spirit will become completely neutral.

@lwtcs It doesn't matter to me If it is diluted or not. My main purpose is to separate oils from a hydroalcoholic distillate (and without adding toxic substances). I can make essential oils without using alcohol btw.
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Re: Separating the oils from the alcoholic beverages?

Post by Demy »

I'm not sure about the question, but if it helps, I extracted the hop aroma (similar to commercial oil) by soaking the hops in very cold alcohol (to dissolve the resins) then evaporated in a large container, the product remains oily, rich in aroma .... if that's not what you are looking for ... patience, I tried ...
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Re: Separating the oils from the alcoholic beverages?

Post by LWTCS »

This is a type of 3 column system used to scrub ethanol clean.
At the hobby level, this type of cleanliness seems a bit much?
A proper hobby column is capable rendering some pretty azeotropic distillate when correctly operated.
I dont recall anyone ever complaining about the quality of distillate rendered from a measured strip and spirit run with adequate theoretical plate count.

Seems you require laboratory grade purity levels?

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Re: Separating the oils from the alcoholic beverages?

Post by Saltbush Bill »

Edenhazard wrote: Tue Nov 23, 2021 2:22 pm to separate oils from distilled spirits? (like gin or vodka). By doing this, a liquor that previously louched will not louche again.
Any Vodka that will Louche has got to be very poorly made to begin with.....someone stuffed up the cuts and used the wrong still to make it.
My gut feeling is that your doing a whole lot of thinking and have done very little distilling.
What stills have you run ?
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Re: Separating the oils from the alcoholic beverages?

Post by Edenhazard »

Demy wrote: Tue Nov 23, 2021 2:40 pm I'm not sure about the question, but if it helps, I extracted the hop aroma (similar to commercial oil) by soaking the hops in very cold alcohol (to dissolve the resins) then evaporated in a large container, the product remains oily, rich in aroma .... if that's not what you are looking for ... patience, I tried ...
Nah. What I am looking for is the product you evaporated :D
This is a type of 3 column system used to scrub ethanol clean.
At the hobby level, this type of cleanliness seems a bit much?
A proper hobby column is capable rendering some pretty azeotropic distillate when correctly operated.
I dont recall anyone ever complaining about the quality of distillate rendered from a measured strip and spirit run with adequate theoretical plate count.

Seems you require laboratory grade purity levels?


My purpose is to extract essential oils from distilled alcohol. Let's say you have Pastis or absinthe. If you dilute it, it will louche. It louches because of the volatile compounds (especially oils) that are dissolved in the alcohol. I want exactly those oils in a pure form but I am really struggling. I tried changing the temperatures (cooling or heating), distilling, changing densities but nothing works. The turbidity is very stable. I haven't tried activated charcoal and other types of adsorbents yet, but I am sure many here have previously used them. So I was wondering if adsorbents will do the trick if added? If not what works?

(concerning vodka or the distillation of spirits. I was citing some potential experiments that might do it. Because in spirits like vodka, everything except alcohol is discarded so fining agents are used sometimes. Whereas for spirits like Pastis or absinthe, the oils are kept with the spirits). I don't think such a still will isolate the oils from the alcohol.
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Re: Separating the oils from the alcoholic beverages?

Post by Edenhazard »

Saltbush Bill wrote: Wed Nov 24, 2021 2:00 am
Edenhazard wrote: Tue Nov 23, 2021 2:22 pm to separate oils from distilled spirits? (like gin or vodka). By doing this, a liquor that previously louched will not louche again.
Any Vodka that will Louche has got to be very poorly made to begin with.....someone stuffed up the cuts and used the wrong still to make it.
My gut feeling is that your doing a whole lot of thinking and have done very little distilling.
What stills have you run ?
I did a lot of distilling but I never distilled vodka or alcoholic beverages. I sometimes distill to get a 95% alcohol and that's it. (sometimes it is mixed with volatile compounds and it louches)

My purpose is to separate the volatile oils from the distilled alcohol.

My aim is to get the oils in a pure form for therapeutical reasons. For example, Pastis and absinthe contain essential oils and they louche. I want to find a way to separate the oils. Heating, cooling or changing the densities won't make them separable. Distilling doesn't work because both distill together and form an azeotrope. I made my own distillation setup. 1 retort and 1 receiver inside a large gallon of water. I use a common hot plate. I calibrate the temperature to around 80 deg C. I never find problems with fractionation
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Re: Separating the oils from the alcoholic beverages?

Post by NormandieStill »

Would you not be better starting with the herbs and performing a steam distillation rather than starting with an alcoholic end product?
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Re: Separating the oils from the alcoholic beverages?

Post by Edenhazard »

NormandieStill wrote: Thu Nov 25, 2021 4:24 am Would you not be better starting with the herbs and performing a steam distillation rather than starting with an alcoholic end product?
Normally, yes. But let's say I Want the essential oils of wine or beer, or the essential oils of mead?
The oils in wine and grapes are different for example.
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Re: Separating the oils from the alcoholic beverages?

Post by NormandieStill »

Then I think you want to distill all the way down to late tails to collect them, but I don't think you'll get a very high yield. If you want to separate them out completely you're probably going to need an absolutely enormous plated column with individual take-offs and a fairly large amount of wash.

Or you need to speak to an organic chemist. You're going to need to transform your solvant (ethanol) into something in which the oils are no miscible without attacking the oils. I don't know if simply applying heat and height will get you what you want.
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Re: Separating the oils from the alcoholic beverages?

Post by jonnys_spirit »

Heat and pressure applied to the seeds/material plus just enough of a solvent that you can evaporate out. Probably under vacuum to minimize cooking.

Cheers!
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Re: Separating the oils from the alcoholic beverages?

Post by Saltbush Bill »

Edenhazard wrote: Thu Nov 25, 2021 4:00 am . I use a common hot plate. I calibrate the temperature to around 80 deg C. I never find problems with fractionation
If I understand this correctly, you are controling the temprature of the boiler...or the wash in the boiler? Attempting to keep it at 80C?
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Re: Separating the oils from the alcoholic beverages?

Post by Kareltje »

Maybe you can start to concentrate them like in https://homedistiller.org/forum/viewtop ... =14&t=5994 ?
Of course after adaption of the cutting points.

And when there are floating oils on top of the fluid you could pick them up with a small piece of clean cloth, which you later can extract with water. Absorbing them in coal or the like will be difficult, as this will not let go of the oils.
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Re: Separating the oils from the alcoholic beverages?

Post by Edenhazard »

NormandieStill wrote: Thu Nov 25, 2021 8:55 am Then I think you want to distill all the way down to late tails to collect them, but I don't think you'll get a very high yield. If you want to separate them out completely you're probably going to need an absolutely enormous plated column with individual take-offs and a fairly large amount of wash.

Or you need to speak to an organic chemist. You're going to need to transform your solvant (ethanol) into something in which the oils are no miscible without attacking the oils. I don't know if simply applying heat and height will get you what you want.
Transforming ethanol into something else is a good idea. I think I looked into that before but nobody came with an answer.

Heat and height?

The method in the link given by kareltje works by distilling until the tails, but there are always lots of oils lost in the heads and the middle (the oils that will remain soluble in the alcohol and won't float. They float when the alcohol is supersaturated.

And you're sure I would need lots of quantity of fining agents? I don't mind using like a 1:3 ratio. But I am not sure if someone tried it here. I think the most convenient thread would be one where someone used a fining agent and lost all flavor in his distillate or fermented product. Not sure if it happened to anyone here before
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Re: Separating the oils from the alcoholic beverages?

Post by Edenhazard »

jonnys_spirit wrote: Thu Nov 25, 2021 10:18 am Heat and pressure applied to the seeds/material plus just enough of a solvent that you can evaporate out. Probably under vacuum to minimize cooking.

Cheers!
-j
I am not looking to make oils from fresh material but from fermented solutions like wine or beer or distillates like Pastis or absinthe. I want to extract the volatile oils that are contained therein. In the distillates like Pastis, they are responsible for the louching.
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Re: Separating the oils from the alcoholic beverages?

Post by Edenhazard »

Saltbush Bill wrote: Thu Nov 25, 2021 11:49 am
Edenhazard wrote: Thu Nov 25, 2021 4:00 am . I use a common hot plate. I calibrate the temperature to around 80 deg C. I never find problems with fractionation
If I understand this correctly, you are controling the temprature of the boiler...or the wash in the boiler? Attempting to keep it at 80C?
I am controlling the temperature of the boiler. Nothing is wrong with the temperature as I could always make pure alcohol except when I distill with herbs that contains volatile oils..
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Re: Separating the oils from the alcoholic beverages?

Post by Edenhazard »

Kareltje wrote: Fri Nov 26, 2021 7:20 am Maybe you can start to concentrate them like in https://homedistiller.org/forum/viewtop ... =14&t=5994 ?
Of course after adaption of the cutting points.

And when there are floating oils on top of the fluid you could pick them up with a small piece of clean cloth, which you later can extract with water. Absorbing them in coal or the like will be difficult, as this will not let go of the oils.
I did this before. Thanks for the link as I completely forgot about this. It is not a 100% solution because I had the following disadvantages.

There is always a decent amount of oils that won't separate and will remain in the alcohol. I also think the oils that will stick to the alcohol are better. (they have a better smell). And I am not sure how much oil the alcohol contains. It might contain like 4x more than all the floating oils... I don't have the tools as well to measure the mass difference as I work on a small batch.

If I bring a wine from the supermarket and try this experiment, it doesn't work as the oils aren't so abundant in the wines sold in stores. I need to do the whole fermentations myself. I think I'd need to leave the fermentation for a long time as well in this case... How long I don't know....

If I absorb them with the oil, I am not sure if I can let them go or not, but it might be possible with distillation or extraction..
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Re: Separating the oils from the alcoholic beverages?

Post by jonnys_spirit »

Maybe try salt and cold crashing?

https://homedistiller.org/forum/viewtopic.php?t=64496

Cheers!
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Re: Separating the oils from the alcoholic beverages?

Post by NZChris »

Look up the Cousin's process for high ester rums. You might be able to put the esters you want into non-volatile forms that you can extract by evaporating all of the water and ethanol or using membrane technology. Good luck trying to reconstitute them back to VOCs without adding alcohol back. What are you trying to make? Non-alcoholic beverages?
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Re: Separating the oils from the alcoholic beverages?

Post by atarijedi »

Have you tried using a reverse osmosis filter? The ones made for purifying water, and I'm just talking about the filter membrane itself, will also let ethanol through, it will also let methanol through, but most of the other stuff present will be blocked.
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