Sciencemadness Discussion Board

Ethanol Still

BCPneumatics - 9-3-2007 at 15:22

I am in the process of building an ethanol sill, but a 'too good to pass up' auction on e-bay has put me over my monthly chemistry budget. My question is, would it be okay to use a (galvanized) steel pipe for the column of a reflux still? I have no intention of drinking any of this ethanol, I just want to be sure that I wont be producing ethanol that contains too many contaminates to be useful as a reagent after drying.

12AX7 - 9-3-2007 at 15:25

I don't see why not. Add some EDTA to the pot if you want to keep the zinc from doing anything. :P

Tim

roamingnome - 9-3-2007 at 15:39

why not copper.... in that case... worked for the moonshiners

Conversion of ethanol to acetone over zinc oxide-calcium oxide catalyst. Optimization of catalyst preparation and reaction conditions and deduction of reaction mechanism

The conversion of ethanol to acetone in the presence of water vapour was studied in order to find the catalyst composition, catalyst calcination temperature and reaction conditions and to deduce the reaction mechanism
http://cat.inist.fr/?aModele=afficheN&cpsidt=6762883

google shmoogle i know...

12AX7 - 9-3-2007 at 15:45

What the....hell does that have to do with anything!? Are you drugged, gnome!?

BromicAcid - 9-3-2007 at 15:56

I think that the point roamingnome was trying to make was that copper is the time tested material to build these types of things with. When you work with galvanized pipes certain side reactions might be catalyzed such as the conversion of your ethanol to acetone, specifically as roamingnome hinted at with the reaction between water vapor with zinc oxide catalysis.

roamingnome - 9-3-2007 at 15:59

just when im going to log off ..i see such a presumptuous post....

Are you drugged, gnome?

no im not.... your really something else... pugnacious for sure....

Zinc coatings prevent corrosion of the protected metal by forming a barrier, and by acting as a sacrificial anode if this barrier is damaged. When exposed to the atmosphere, zinc reacts with oxygen to form zinc oxide
Fingwikipedia


so your telling me that water vapour in a hot ethanol distillation coloum with zinc oxide affecting the gentlmens ethanol doesnt make sence...?????

[Edited on 10-3-2007 by roamingnome]

BCPneumatics - 9-3-2007 at 16:11

Ah, I should have been more specific. The reason I am searching for an alternative to copper is that I cannot afford the $50-75 that it would cost at this time. I already have a list of things that I am in need of, and a still isn't terribly high on the list at that cost, but it would be very handy to be producing ethanol.
Thanks for the help thus far... at least I now know how to produce acetone.

[Edited on 3/9/2007 by BCPneumatics]

not_important - 9-3-2007 at 18:28

Galvanized is a bad idea for distilling fermentation ethanol, the volatile acids present will make fairly short work of the zinc coating.

One way to dry ethanol or other low boiling alcohols - vapour phase using corn grits
http://journeytoforever.org/biofuel_library/ethanol_grits.ht...

Making your own ethanol is a bit of work, and you will need to lay out some money to do it on anything but the smallest scale.

Magpie - 9-3-2007 at 20:40

@BCPneumatics: How much absolute ethanol do you anticipate needing?

My consumption rate is very low, maybe a liter or two/yr. At that level rectification of cheap vodka (40% ethanol) using a laboratory scale glass fractionation column packed with broken glass has been working out just fine. If I need it absolute I just add some 3A molecular sieves. But like most here I just use it for my hobby chemistry and don't require anything ultrapure.

not_important - 9-3-2007 at 21:35

Something possibly cheaper than vodka, depending on taxes on potable alcohol where you live, is the Chinese cooking wine. This is basically a distilled rice wine with salt added to it, I usually can find products in the 20 to 40 percent (call it 40 to 80 proof) range for ... about US$ 2 per liter. A simple distillation with a little added soda ash to get it up to 60% and salt and acid free, then a proper fractionation to 95%. And if you check and pick the right brands, you can even consume the product without wondering what else is in there.

not_important - 9-3-2007 at 23:17

Taxes raise the cost of vodka in many areas, generally the tax is more than the cost of the untaxed cooking wine; try buying vodka in Sweden, Finland, or Hong Kong. For me the cheapest vodka ran about 5x the cooking wine for a given amount of ethanol, the cooking wine is 35% ethanol.

Tossing some soda ash in before the first distillation takes care of much of the acids and esters, leaving just the higher alcohols. And for me, a 15 plate Oldershaw does well in cleaning things up. I haven't used it recently, don't have the room to set it up, easier to get someone at the hospital to get me a couple of liters of 95%.

If I remeber correctly, Thai alcohol taxes have their lowest rate on lao khao as opposed to wine and beer, this is the reverse of much of the rest of the world.

garage chemist - 9-3-2007 at 23:21

Vodka is a really bad starting material, both in views of cost and of concentration.
I make ethanol starting from 94 Vol-% denatured ethanol which is cheap here and contains no methanol.
Refluxing over NaOH for a day takes care of most of the MEK which is the prime denaturant. Distillation then affords quite good 96% ethanol.
The rest of the MEK and any aldehydes and ketones are completely removed by distillation over sodium borodohydride, this gives carbonyl-free ethanol.

BCPneumatics - 10-3-2007 at 07:55

Thanks for the out pouring of information. I had assumed that steel would be no good, but I of course wanted some conformation.
Yes, the plan for drying was via corn meal. (A good page: http://journeytoforever.org/biofuel_library/ethanol_grits.ht...). I do live in N.A., but borosilicate is not as scarce as you seem to think, at least not in California. A tube of the size you described wouldn't be difficult to locate, or even terribly expensive. I had planned on weighing my product to determine purity, using a friend's triple beam balance, but I could use a balance in the school's lab, I'm sure. (The most accurate one being .0001gx100g as I recall) I had planned on fermenting sugar, and my 'lab' is a section of my shop- so there are three fire extinguishers near by, although one is far too small to do anything in this situation. As expensive as you seem to think it is, I am convinced (read: I have seen it done multiple times) using a copper column and stainless boiler.


"In short my hat is off to moonshiners because what they do is hard skilled messy work and I think their motto ought to be "Crime doesn't pay...enough!)"

My family on my father's side ran shine in Kentucky during prohibition... maybe it is still in the blood.

roamingnome - 10-3-2007 at 09:23

Yes Sauron always has a way of inspiring me and discouraging me at the same time, what a kick…

a person in my local thinktank wants to build the molds for making a ceramic perforated column as you have pictured. It might be doable stacking them up…

For he who has the molds controls the product…. To increase value some break the molds…. Others print the money from the molds. And secret kung fu fighters with Uzis fight for them…

Im really a beginner with distillation that’s for sure… but ive spent the last 4 days chomping on 316 SS and still haven’t cut threw, so I can potentially do it right….

With genetically modified yeast and fungus I hope ethanol gets easier…
VOX is distilled 5 times… but grey goose is still more popular…

BCPneumatics - 10-3-2007 at 09:42

I suppose it would have been more appropriate to write "reasonably priced borosilicate work is not as scarce as you seem to think," my apologies. I know of a few places that sell 'turbo yeast', so no worries, I know I am not making bread...
Still, I don't think this is a matter where a terrible amount of luck is needed, just proper procedure.

roamingnome - 10-3-2007 at 11:23

Quote:

drilling smal holes in glass is a specialist task


i certainly wouldnt want to drill the 1000 plus holes needed for a glass column, but ive had pleasurable luck with a dremel tool, diamond bit, and water spray.
even pyrex cuts nicely....
i think haha wouldnt the anceint people fight a war for this bit....

thanks for the scotch wiskey copper required tip.....i do want some medicinal wiskey ageing for good measure....



a DIY condensor that i saw in a store for $75 but made a 3X as long one for $40 was

a coil of copper tube inserted through a large (1-2 inches) clear plastic tube....( lube it up....for sure) the right brass compression fittings and plastic T pieces on the ends.... i havnt used it yet but it sure looks pretty....

i dont like turnips no sir....

BCPneumatics - 10-3-2007 at 11:31

I know you aren't trying to scare anyone off or anything of that nature. I have been sifting through the topics on these forums for some time now, and I have seen that it is a pretty good little community. (Very refreshing compared to some other boards I have seen.)

I am planning on a design of this nature: http://homedistiller.org/image/mini_explained.jpg However, I may use a different packing material if it produces much better results. (I also think that adding some sort of a seal to the lid is a good idea.)

I can't imagine myself using more than a couple hundred mL's in a week, so I am not concerned with 'low output', but I also have a friend who wants some. (The same person I mentioned earlier, with the balance.)

It is indeed true that New Zealand has a wealth of information on the subject. Most of what I have read seems to originate from there, including the link above.

evil_lurker - 10-3-2007 at 15:05

Ya'll are making shit way too complicated...

Get some sugar, 48 hour turbo yeast, and a fermenter.... thats all you need for brewing and as cheap as it gets... even though you'll spend more on yeast, its cheaper timewise as you can get more alcohol made over a shorter period of time.

I built a small pot still head outta a turkey fryer, a bulkhead fitting, some copper pipe, a condensor outta some PVC, and sealed everything up with GE Type II silcone from wally world... figure I got about $125 tops in everything.

This thing can process about 4 gallons of wash at a time in about an hour... usually I concentrate into one gallon and be done with it... final proof is around 35-40%.

Then by using a 300mm Hempel column packed with ceramic rings and doing a nice slow distillation I'm able to kick out 85-88% second time around... 500mm column would probably give better results.

If one is worried about those nasty stinky impurities, throw in a coupla heaping teaspoons of sodium carbonate the second time around... it will neutralize the esters while your doing the distillation and improve quality dramatically.

potstill.jpg - 118kB

BCPneumatics - 10-3-2007 at 17:13

Thanks evil_lurker. There is always something to be said for doin' things the back woods way.

Sauron - 10-3-2007 at 18:37

I have removed my posts from this thread. This new member did not come on here looking for advice, though he pretended to. He already had his mind made up. Therefore it is a waste of forum resources to proffer advice to him, and I won't.

Aurum - 11-3-2007 at 06:50

Here's a nice document on building a still.

Attachment: still.pdf (680kB)
This file has been downloaded 855 times


BCPneumatics - 11-3-2007 at 07:03

Sauron, how did you reach the conclusion that I was not looking for (practical) advice?
The fact of the matter is that I am looking for advice on building a still within my means. I am aware that there are one hundred and one ways to skin a cat- just because I am not following your method to the 'T' does not mean that I did not appreciate your input, I simply cannot afford the method you offered, even if it is superior.
The reason I checked this thread this morning was to re-read the wealth of information I was provided, and add some things that I realized I had left out of my previous posts. Your posts were certainly some of the better ones in this thread, and I am sad (and honestly just a slight bit ticked) that they are gone, but if you deem me unworthy of your insight, then I suppose that is your own choice.

For anyone that still thinks I am worth the resources of a response, I forgot to mention that I was planning on using CuSO4 for a quick and easy test for dryness. (Though I still plan on testing samples by weight to check the concentration after each phase.)

Sauron - 11-3-2007 at 07:40

Tony Ackland the proprietor of www.homedistillers.com is an old correspondent of mine and in fact the vapor dividing still I described to you came from him about 5 years ago, though I did not notice it on his site now (he sent it to me privately.)

If you make creative use of the interactive calculator on his site for designing a reflux still, you will do well. Tony likes SS pot scrubbers; I like Raschig rings the smaller the better. His calculator has both pot scrubbers and 6mm Rashig rings built in and selectable; you can compar those to each other and to "marbles" (they suck) and you can define your own packing material if you wish.

The calculator will tell you % ethanol out, and how fast (for a given amount of watts heat in and % ethanol in wash) and you can play with column height and diameter and the equations (algorithms really) will tell you minimum ID for avoiding flooding and HETP and # of TPs etc all of which are things you really want to know whether you know it or not.

Tony knows what he is doing and he is a chemical engineer.

Don't worry about me, I'm a grouchy old fart. Good luck and best wishes.

BCPneumatics - 11-3-2007 at 08:24

I am still going over his site, there is a lot of information there. I am defiantly going to take the advice of using something better than scrubbers though- it seems to be a very good, cost efficient improvement.

No worries here, I am used to far worse ;)

evil_lurker - 11-3-2007 at 09:01

If your drinking the alcohol, copper scrubbers will result in a finer tasting product as I am told.

BCPneumatics - 11-3-2007 at 09:09

Judging from what was mentioned earlier, some copper id needed in there for the taste.

Sauron - 11-3-2007 at 10:59

To destroy some sulfur-containing organics that otherwise bugger up the flavor. These are yeast waste products. Copper is of no significance if one is starting with potable ethanol such as vodka, and just concentrating it. I used to strip grape spirits out of (cheap) brandy to make absinthe. Did it in glass only using Rotavaps, fast and easy. I only needed 70-80% so simple distillation (a la Buchi) was fine. I also distilled the absinthe the same way. It's made rather like gin, from herbs and alcohol and water, nothing else.

But, I can't drink any more so I quit making the stuff. Damned diabetes!

YT2095 - 15-3-2007 at 01:40

I`ve been doing it the Other way around, I started with some Gin, and am currently extracting the alc from it here: http://myweb.tiscali.co.uk/yt2095/experiments/still.jpg
it`s not amazingly fast, and was set up in a matter of minutes, but no-one here drinks gin, and I can use the raw alc, saves wasting it :)

Sauron - 15-3-2007 at 01:53

Those essential oils in gin will mostly steam-distill over with the water portion of your distillate and so will be quite hard to remove by distillation. AC would do better as a pretreatment, either batchwise with powdered AC like Norit or fixed-bed (column) with GAC like Darco. Don't concentrate the stuff first, you want to treat it at 40-50%, then fractionate it afterwards.

YT2095 - 15-3-2007 at 02:18

to be honest with you I`m not all that fussed if a little bit of the oils come over as long as it potable, I only want it for my capsaicin extract.
oddly enough there isn`t even a smell trace that would say it ever came from gin anyway, so I`m quite pleased thus far.

I have to ask though, what is powdered AC?

I was going to add a little bicarb and dehydrated MgSO4 and re-distill it anyway, but if this "ac" is any better and I have some, I`ll give that a shot instead :)

not_important - 15-3-2007 at 02:39

AC = Activated Charcoal

YT2095 - 15-3-2007 at 02:40

Fantastic Thanks! and I have plenty of that :)

Sauron - 15-3-2007 at 02:46

That's the way that home distillers and professional vodka distillers get congeners out and end up with neutral spirits (vodka). Slow passage through a tall column of the right sort of granulated activated carbon. Always at not more than 50% abv (alcohol by volume) i.e., 100 proof. THEN you can rev it back up to 95% and dry it if need be.

YT2095 - 15-3-2007 at 02:54

I have Israeli NBC gas mask filters, and when they`re used up, I pop them open and dump the contents on a baking tray and heat them up in the oven for a few hours to reactive them, then store in a jar.
these will be ideal I expect.
I don`t need a massive amount of EtOH, just as long as it`s potable, unlike the pure EtOH I have that has some MEK in it :(

this ultimately will be a Food product, so a little care NOW, will pay dividends in the long run :)

Sauron - 15-3-2007 at 03:18

The GAC used in gas mask filters is optimized for that purpose and is quite different from GAC used for polishing ethanol.

Check out Norit's web site and get the tech data sheet for the appropriate grade. I used to buy this stuff by multiple 25 Kg sacks and Norit were happy to give me 1 Kg samples of lots of grades to test for free. GAC is not expensive as a rule. Not from the OEM. If you buy it from a repack operation like Aldrich then you pay a lot. (Aldrich makes a lot of chemicals but I am sure they don't make activated carbon.)

YT2095 - 15-3-2007 at 03:28

too late now, it`s done and for some reason looks even more clear than before, and it looked Crystal then!?

I`m committed now, so I`ll go with this. I can see what you about the oils though, in the distillation flask that I washed with plain water, now has a region where it looks almost oily, the rest of the glass is wetted except for this region where it`s Patchy at best, I think a hot soapy water soak with a little NaOH is in order.

I was wondering if there was a Chemical way to denature these oils and/or lock them up?
NaOH and the likes is a little harsh and may affect the alc also. how about a group 2 hydroxide like Calcium or Magnesium? perhaps lock the oils up as a stearate?