Fractional Freezing / Freeze Distillation

Fiji_Spirits

This process is basically the inverse of steam distillation, where you freeze a liquid and it separates into crystals and liquid components. the crystals are separated from the liquid and the two streams can then be used or re-distilled until desired purity is obtained. It is a way to separate acetic acid from Vinegar and more commonly to purify apple cider into Apple Jack.

Has anyone had any experience with this or can anyone point me to some resources for a fractional freezing apparatus either on a small commercial or a large lab scale??

Curators_Reserve

1000L IBC tote or 200L food grade barrel in a commercial cold store freezer.

Daily stirring removing ice - collect in seperate tub/ tote.

Conical with drain would be of great help to drain residual Alcohol.

punkin

It's practiced in environments where the weather does the work at zero cost as far as i have ever seen.

Fiji_Spirits

I have a chemical process that requires freeze distillation to extract the desired product. It should be fairly lucrative even with high per liter costs.

I've kind of considered an alternating freezing/ heating column that purifies as the product goes down. Liquid separating from crystals at each stage.

Other types use wall condensation/ freezing/ melting cycles to obtain results.

I'm betting there is a way to use modular parts tho.

grim

Other than in the far back colonial history of applejack, it's never been commercially produced by freeze jacking, it's expensive, labor intensive, inefficient, etc. By the early 1700s, freeze jacking was all but abandoned and replaced by pot distillation. The main issue is, you can't make cuts, only concentrate the volatiles. I can't imagine pre-distillation colonial applejack was a very refined product. It was probably awful. In fact, I don't need to imagine, it was probably chock full of methanol too. It also requires mind numbingly cold temperatures to achieve even a moderate ABV, and the early history of applejack is dotted with examples where the bright side of brutal winters was producing the strongest product - so at least you could be drunk when you froze and starved to death.

grim

I hail from the home of commercial applejack - New Jersey - where scot William Laird setup a distillery in the late 1600s, and changed the process by producing it through distillation, and aging it like whiskey. So popular was the style, in fact, that hundreds of local producers popped up emulating it. Laird won out, owning the category for more than 400 years. The Laird family went on to found the first licensed distillery in the US (1780, DSP No. 1), and has a history that includes George Washington and Abraham Lincoln. Today, no longer made in NJ, and it's now a blend of apple brandy and neutral spirits.

It's a bit of a misconception that applejack is made by freeze distillation, it's not, and hasn't been for 400 years. The closest commercial products on the market are eisbock I believe. I don't think there are any commercial spirits produced through freeze distillation in the US today. Maybe some enterprising craft startup is doing something, but I hadn't heard.

CothermanDistilling

They do that freeze crap with beer, and sell it in a bottle stuffed in a taxidermied squirrel or other animal... I tasted it, it tastes like they stored it in the dead squirrel, not the bottle..

This Dead Squirrel Filled with 55% Alcohol Beer Only Costs $20K

Fiji_Spirits

Cool history of apple jack and squirrel beer.

I agree that freeze distillation for booze is not a good solution. It was about the only reference I could easily find in common literature.

It is used to concentrate juices, desalinate salt water, and clean waste water as well as rectify acetic acid and other chemicals.

zymurgybob

I've had a couple of experiences with freeze jacking, and the most important distinction between it and distillation is that simple water removal is way different from purification. You concentrate everything that isn't water - good, bad, or awful.

Unsensibel

That dead squirrel bottle looks already disgusting!

Fiji_Spirits

I was looking at a rotovap. I wonder if one might use that and a chiller to freeze the liquid onto the walls at room temp as it rotated in a super chilled liquid. Then when enough has be frozen, start pulling a vacuum to remove the more volatile liquids and dump the liquid out leaving the acetic acid.

Kind of a reverse use for the Rotovap.

I got a quote from China for a complete system including vacuum pump chiller and 20l Rotovap system for $7600 usd. For another $3000 I can make the chiller a 200c to -30c heater/chiller.

grim

Like an Ice Cream Maker?

Fiji_Spirits

Roflmao

Yeah. Exactly like an ice cream maker.

This is why I come here. Lol

Craigarino

Hi, I've done it a few times. Many years ago with cider to make apple jack- it's amazingly delicious, and a lot of work for only a little product and like one of the blokes says above, it concentrates the fusil oils and the head ache in morning is worse than death- proper apple palsy! Then recently I got given a pallet of grolsch that had expired! I only had a seven litre still in those days, so would pour the beer into a bucket, freeze over night in deep freeze and smash open next day to run. Saved me some stripping time but was a lot of dicking around! Definitely worth making apple jack but