Sciencemadness Discussion Board - Distillig ethanol from corn mash. Help?

Distillig ethanol from corn mash. Help?

Saganism - 6-10-2012 at 19:55

So I have a glass kit, no metal/copper bull. I've had a mash going for the past 2 weeks that is very potent with alcohols. Well, I setup for fractional distillation and used a water bath. Well my cimarec hot plate/stirrer combo was literally at its max capacity of what is apparently 540 Celsius, which I know is false, cause I took a thermometer to it and it only read up to 300 Celsius. On top of the disappointment of an apparently really bad plate which cost me 340$(never buy one of these), the water bath wouldn't even boil after 2 hours? Didnt even get past 90 Celsius. So then finally it boiled a bit(not to mention I had boiling stones in both solutions(water bath, still flask) from the beginning. Still, through the water bath boiling nothing for 30 more minutes. Well I was rushed away from this to go to a wedding so I couldn't finish. Before I left though I checked the flask, and some sort of white solution had halfway hardened into some sort of emulsion?? Wtf? Turns out the boiling stones in the still flask had been literally caked to the bottom. Could I get some tips? Is a bunson burner better for this? I'm extremely agitated

CaliusOptimus - 6-10-2012 at 20:37

Lab hotplates don't put out much heat compared to cooking hotplates. They are more geared toward even heating characteristics. You don't need stirring for this kind of thing anyway, but insulating your bath with fiberglass should get you up to 150c range no problem.

Use an oil bath on a $15 kitchen hotplate, you won't be disappointed.

[Edited on 7-10-2012 by CaliusOptimus]

violet sin - 7-10-2012 at 00:35

so what all did you do to the mash before you tried to still it off? from what I read, and tips from the brew store owner, say that it has to be clarified unless you want crud to gum up your boiling flask. like boiling down a thinned out corn soup

eventually it boils down to a gum. and if you are doing glass distillation set, maybe a sand bath would be best. you can stick a thermometer in the sand next to the flask to easily monitor temp, and you don't have to worry about heat losses from you water bath boiling off. you only have to get it to ~80'C. -starts coming over at like 65'C, fine tune it to about 78'C- paraphrased from book

I bought a book and a few things to get started, and being that I am a beginner, I wonder how much experience you have with this? not to be a jerk, but 2 weeks for the mash is a bit longer than recommended no? the turbo yeast I got said 48 hrs for 14% and after 5 days a full 20%. all you have to add is water, sugar, and optionally yeast nutrients( comes in packet with mine). I didn't wanna use corn b/c of the mess but there is nothing wrong with going that route. clarify it and still, or use something stainless for vessel that can just be cleansed thoroughly with food grade chems. also sold in a brew shop. I bought a stainless beer keg for my boiler.

side note, I found a "acid cleaner no. 5" there at the store, and looked up the msds, its 5% phosphoric acid and 30-35% nitric. blue liquid in 1 gal botttle. just fyi.

I have only read up a lot so deff not trying to act all know it all. there is stuff every where online to read, and the book I got is called "moonshine made simple and the still makers manual" -byron ford- ISBN 0-473-07404-4. was only like 12$ and 125pg cover to cover. it has a LOT of info though, including still basic designs and operations, essential oil production and more. I highly recommend it. if not then consult a local brew shop owner. they (in my experience) are really nice and you can ask all kinds of questions w/o having to worry too much about what you say. they are use to it.

good luck

vmelkon - 7-10-2012 at 14:39

Quote: Originally posted by Saganism

Is a bunson burner better for this?

I would not do that. If your glassware has ground joints, there will be some ethanol vapor at the joints. Always use electric heaters when working with flammable organic liquids.

Purification of ethanol from an alcoholic wash

Fossil - 7-10-2012 at 14:59

I would give you a full write up of my experiences, but I honestly don't have the time right now, so i'll refer you to the place where I learnt a lot of what I know. The rest coming from experimentation.

http://homedistiller.org/
http://homedistiller.org/forum/

A few tips I'll give are:

-Have copper somewhere in your fractioning column or in your still (where it will interact with the alcohol vapors. The copper reacts with the congeners (fusel oils) and helps to remove some of the foul smell/taste you will encounter.
-Use a fractioning column.
-Heat slowly, especially once the vapors reach the 70c range. I try to keep my thermometer in the high 60's-low 70's for as long as possible.
-If your aim is to get a neutral alcohol, do not go over 80c-81c
-Never distill a wash that has yeast left in it. Always rack away the yeast. The heat will break the yeast down realeasing all kinds of foul smells/tastes.

I am by no way an expert and these tips are purely from experience. Make sure to do a lot of reading on the subject, you won't regret it.

Saganism - 7-10-2012 at 15:19

Should I use a sep funnel and separate my layers draining the bottom? Will the alcohol layers be on top? And What i did to the mash before I stilled it, was filtered out all of the corn meal and such only leaving behind liquids but when i shake it up a bit and it eventually settles out, there are two layers? One on the bottom is obviously gum like. How do I 'rack' out the yeast? And again yes, I'm going for neutral ethanol. Obviously I'm a beginner, didn't think that needed to be stated considering here I am asking for help?
Fossil, you say you like to keep your thermometer in the high sixties low seventies, I assume this is for the purpose of stilling off all of the Methanol? I have no copper and I've read in places where it can be done without the copper, I'm going for neutral ethanol so the copper isn't exactly necessary is it? If I must, could copper sulphate be used for this in the way a drying agent would be used? Just a simple swirl or two and let it sit sort of thing? or what? Lots of questions.. sorry. I have a festival I'm going to in a few days and I really need at least a liter to go out there with. ALSO. if someone could give me a recipe to use in a 5 gal bucket that would be awesome, as well as a recipe that actually works with only sugar, water, and yeast?? That would be great. But how long does that take? This mash I made last was a 4 gal pot and I put 8lbs of corn meal and equal parts sugar and about 21 grams of yeast. Red star to be exact. I'm looking for the most efficient formula, as is everyone I guess.

Bot0nist - 7-10-2012 at 15:22

"Rack" simply means to siphon all the liquids off the settled, dormant yeast.

Dr.Bob - 7-10-2012 at 16:40

I did this once in a biofuels class, it took almost 2 hours just to get it up to temperature with a large hotplate. Water (which the mash is ~ 90%) has an enormous heat capacity so it takes forever to boil a large amount.

Plus you will need to clarify first, just pour off the top fluids leaving most of the yeast behind. You can then pour the yeast goo in a small glass and then pour off more fluid back.

This process took over 5 hours for a 10 L batch, to get about 1L of EtOH, which was about 90%, but using a stainless steel fractionating column. This is not a trivial process, just like many other things.

cyanureeves - 7-10-2012 at 17:10

i did it with a crock pot warmer .the two part ones not the single self heating pot but first you have to separate the liquid from the solid. i also didnt use copper tubing but instead used a couple of heat resistant silicone tubes i got from the inside bottom of old regular coffee makers.i attached aluminum tubes in segments along with the silicone tubes and hung it on a string. i put the mash in a tin gallon xylene can and wrapped it in aluminum foil. water boils at 212 deg. so just under was enough to send ethanol over. sometimes i wanted to speed up the process and turned up the heat but it would steam and water would condensed into my alcohol so i would turn it down to a steady drip instead. out of 5 gallons of mash i got 2 pints of very strong ethanol and i'm sure its poisonous but its still ethanol and not methanol and burns clean until dry. my mash was made from corn meal,sugar,yeast and distilled water and the ethanol smells like bacardi and boy i wish i had used all copper instead.

Saganism - 8-10-2012 at 00:24

I've got it running well now. Thanks for all the help

Ethanol

cal - 8-10-2012 at 17:38

Quote: Originally posted by Saganism

I've got it running well now. Thanks for all the help

I made a 220 volt hot plate for my ethanol distiller from a 8 inch electric stove burner and a 220 volt 4000 watt motor dimmer from ebay for 10.00. Total cost of hotplate $40.00

I make all my ethanol from just sugar and yeast
( Fleischmann's ) for baking. I tried the special yeast for brewing and it produced less alcohol. I made a Boka http://wiki.homedistiller.org/Boka_Reflux_Still__How_To_Buid
and it works really well as I use about 2 to 3 liters at a time with my experiments.

IrC - 10-10-2012 at 15:03

From your link : http://wiki.homedistiller.org/Boka_Reflux_Still__How_To_Buid

"Boka Reflux Still How To Buid

There is currently no text in this page. You can search for this page title in other pages, or search the related logs."

Did I miss something? Other than Buid should be build.

A quick site search yields : (works)

http://wiki.homedistiller.org/Boka_Reflux_Still_-_How_To_Bui...

And :

http://wiki.homedistiller.org/Boiler

http://wiki.homedistiller.org/Column_Connection_Options

[Edited on 10-10-2012 by IrC]

zed - 11-10-2012 at 15:06

Well, I did onetime produce a water cooled distilling condenser entirely from Copper plumbing pipe. Used lead-free solder. Screwed it onto a modified pressure cooker. Wasn't very expensive, and all of the parts were available at home depot.

Unlike a glass condenser, you can make it as big as you like, and yer Copper condenser will not shatter if torqued or dropped. Also, pressure cookers come in friendly sizes, and sometimes can be purchased cheaply at garage sales. Even come in stainless steel. Very handy.

Once again, a caution; distilling ethanol from mash...may cause you legal problems in the U.S..

Uncle SAM wants his ethanol beverage tax.

hyfalcon - 12-10-2012 at 03:31

Varies from state to state. Some states, Missouri for example, allow you to produce a certain quantity for your own consumption.

Arthur Dent - 13-10-2012 at 05:09

Interesting thing about the copper reacting with the Ethanol vapors... I also have an all-glass distilling apparatus. Would a spiral of copper wire in the claisen adapter be useful to obtain the same effect?

Robert

watson.fawkes - 13-10-2012 at 06:13

Quote: Originally posted by Arthur Dent

I also have an all-glass distilling apparatus. Would a spiral of copper wire in the claisen adapter be useful to obtain the same effect?

Better yet, use a knit copper mesh (as can be found for scrubbing pots) as packing in a simple column.

Arthur Dent - 13-10-2012 at 07:12

Quote: Originally posted by watson.fawkes

Better yet, use a knit copper mesh (as can be found for scrubbing pots) as packing in a simple column.

Thank you for your suggestion, but I must warn you that I have discovered much to my dismay that the "copper" scrubbing sponges that I find in my neighborhood stores are actually coarse steel wool with a thin copper coating. That fubared one of my chemical reactions a while ago.

I don't know if it's just a local thing, but I thought I should mention it to make people aware that those shiny copper sponges may not be what they seem.

But I'll try to make a makeshift copper wool ball out of multiconductor electrical wire and stuff it in the neck of the claisen adapter.

Robert

watson.fawkes - 14-10-2012 at 06:36

Quote: Originally posted by Arthur Dent

I must warn you that I have discovered much to my dismay that the "copper" scrubbing sponges that I find in my neighborhood stores are actually coarse steel wool with a thin copper coating. That fubared one of my chemical reactions a while ago.

I have head (but only heard) that they work adequately, though with not so long lifetimes, as column packing. But there is a pure copper product available that's very much like it: structured copper mesh.