Drug info - Extracting ethanol without distillation?

[Mammon]

Is it possible to extract the ethanol from booze without distilling it?

Is there a method based on alcohol's low freezing point? It's been suggested on my previous thread that SWIY can freeze beer and the alcohol will remain liquid and can then be filtered off. Is this right?

Reflux and pot stills are expensive so I was wondering if there's another way.

[Pondlife]

Freeze distillation, more correctly known as "fractional freezing" is probably the most common technique after distillation.

As you say, this is based on alcohol's low freezing point of -114 degrees C compared with 0 degrees for water. However, it's not a simple case of all the water freezing at 0 leaving pure alcohol. What happens is that the material that freezes contains relatively less alcohol, and the liquid that remains contains relatively more.

It's not possible to obtain the same high alcohol concentration with fractional freezing in a domestic freezer as you could with distillation. However, it is a simple way to increase the concentration somewhat.

Applejack is traditionally produced by fractional freezing.

I've heard that fractional freezing can produce a more hazerdous end product than distallation, as the "nasties" like methanol and higher alcohols are not removed as they would be in distillation (by discarding the heads and feints).

[Mammon]

Yeah, I saw some stuff on the net about that. Has anyone out there done it with a commercial beer / cider? Was the result nice or rank?

[Paracelsus]

Isn't applejack made by freezing cider?

[gunnaknow]

SWI-Jamal, freeze distilling can only concentrate the alcohol, not purify it. With a standard home freezer, the temperature is only sufficient to achieve a maximum of 30% ABV and even then, that would require freezing several times, leaving a proportion of the alcohol behind in the ice. Swim will post some info on freeze distillation below but SWIM senses that SWIY is really after nearly pure ethanol, which can only be achieved with a reflux still. SWIY can build his own reflux still very cheaply if he follows some simple designs.

Freezing

Another technique is to freeze the wash, and separate the ice (water) from the alcohol. Freezing appears to fall somewhere in-between the legal issues for many areas (eg can you really stop your Applejack from freezing if its left outside ?). Sort it out with your own authorities (or just keep your freezer contents personal).

One thing to be aware of is the the more alcohol that is in the wash, the cooler it will need to be before it freezes ... Disolving (or mixing) something into a liquid will make the freezing point go lower than when it is pure.

dT = Kf m where Kf(water) = 1.86

Adding ethanol to water will therefore depress the freezing point by 1.86 C per molar conc present. Doing the translation between molar and regular % by volume gives ...

5% abv 1.6 mol% 3°C lower
10% abv 3.3 mol% 6°C lower
20% abv 7.2 mol% 13°C lower
30% abv 11.7 mol% 22°C lower
40% abv 17.1 mol% 32°C lower
50% abv 23.6 mol% 44°C lower

This explains why beer (at 5% abv) will freeze for ya in the freezer, wine will need it to be a bit colder, but frozen schnapps or vodka won't normally be possible.

Another method, known as fractional crystalization, is done by inverting the process and freezing the beverage instead of boiling it. This works for very similar reasons to that of normal heat distillation, namely, the differential in freezing points of the two liquids involved. Water freezes at a temperature of 0 C, while ethyl alcohol does not freeze until reaching -114 C.

This allows the water to be frozen out of the liquid, leaving behind the ethyl alcohol, as well as the other alcohols and esters. This produces a drink of a rather different character from heat distillation, as it contains everything except water, while heat distilled beverages leave everything behind except alcohol. Note also that simply lowering the temperature to 0 C will not produce an increase in alcoholic strength. The temperature required for this process is in the range of -15 C and below, but must vary, much as the diurnal cycle naturally does.

This allows crystals of ice to form as the temperature drops. As the temperature rises slightly the alcohol will drain out of the crystals so that when the temperature again goes down and more crystals of ice re-form they are purer crystals of water, containing less alcohol. As this process repeats itself the solution will gradually work its way toward the alcohol concentrations listed in the following table which is adapted from a chart on page 102 of the book, Wines & Beers of Old New England:

Temperature (C) % Alc.
-12.2 8
-15.0 11
-17.8 14
-12.2 8
-20.6 17
-23.3 20
-26.1 24
-28.9 27
-31.7 30
-34.4 33

I've just tried making some myself, with no success. Poured 1.5L of beer into a plastic container, and put it in the freezer. When frozen, I broke it open. The trouble was though that it appears that it all froze too fast - any alcohol there is trapped within the ice matrix - there was no clean "core" of alcohol. I think that if this is to work, you will have to freeze it VERY slowly, so that the alcohol has time to diffuse its way ahead of the freezing ice front.

Raj tells me though that to get a good clean separation ...
The trick with freezing is to partially thaw and refreeze a few times to promote larger pieces of ice--the frozen cylinder with a heart of alcohol is the consequence of diurnal cycling in a barrel over weeks.

Jack tells me though ..
Don't bother trying to get a frozen heart of alcohol- it's not really needed. Just fill a gallon (4liter) milk jug half full of your beer/wine, let it freeze solid in the freezer, then get a one quart (1liter) wide mouth jar, and stand the milk jug upside down in it. It will take about four hours or so, but eventually as the ice slowly melts (don't apply any heat), the jar will fill up, and you will have just about doubled the alcohol (by cutting the volume in half). using a 10% wine this method will turn a half gallon into a 17% quarter gallon. I have not tried sticking this 17% wine back in the freezer to see if I can get any more ice out of it, but it's worth a try. It also seems to be the easy way to get "distiller's yeast" performance without fooling about with yeast starters and the like.

However, Ups474 writes :
More correctly known as "fractional crystillization", the practice of freezing an alcoholic mash then removing the (concentrated)alcohol was used in ancient times before distilling was known. The problems with trying to purify alcohol this way was that not only did the ethanol come out of the block of ice, but so did all the nasty higher and lower alcohols that cause painfull hangovers, and there is no way to separate them from the ethanol by freezing.

The other reason you may have already seen: if you have ever put a bottle of vodka in the freezer (a traditional method of serving), you will notice that no matter how long it is in there, it never does anything but turn slightly thick, like syrup- no water freezes out once the alcohol gets up to 40%. Unless you have easy access to a source of liquid nitrogen, etc. so you can "super cool" the mash, then bring it's temp back up in a controlled enviroment so as to melt off various alcohols at various times, it's not worth bothering. Even then, it ain't worth it-the energy needed to keep the mash that cold would exceed the energy requirements needed to distill it.

Home winemakers use this technique to make fortified wines without using distilled spirits- Put the mash in a plastic jug, leaving enough room for expansion, then put this in the freezer until it's a solid block of ice, then invert the container over a collection jar and gather everything that melts out until you have collected half of what is in the jug. With a 10% mash, this will come out to about 17% ABV.

AppleJack

Here's what I've found on making Applejack. Its from a 1957 book "Home-made wines" by Mary Aylett, you may find similar in other wine-making books at your local library.

Apple-jack.
Make a good strong cider and then put it in a sealed cask. Place the cask in some place where it can freeze through very slowly. In Canada this is done by digging a large hole in the ground and covering the cask about three inches deep. When the thaw comes, the cask is at once dug up, and the contents will be found to have separated into apple water and to pure spirit. The spirit will be in the centre of the cask. The ice must be broken with great care, and the liquid spirit in the centre carefully run off. This is the apple-jack. It should never be drunk undiluted.

Reputation Comments on this post:

Good informative post

[Mammon]

Thanks for the advice, guys. SWIM will give the freeze/thaw method a go with some cider when he gets the time. He saw the amazing still, though, and thinks that's probably the way forward for drinkable stuff. That's a great site as well - loads of good info.

[gunnaknow]

No problem bud.