Alcohol distillation

[jtryptamine]

Hey maybe one of you guys can anwser me this. swims got a nice distillation setup, all glassware, not some ghetto still. He knows it'll work fine for his purposes (see thread title) but here's the problem- the RBF will only hold 1L at a time. So when he's distilling the wash he knows normally you discard the first 50mL that comes over but since he can only do 1L at a time and he'll gonna be working with 20L wash would he throw out the first 5mL (want to be extra safe so he's doubling it) of each pass or would the volitiles all be at the top or bottom or middle what? Understand what I mean? Any help would be greatly apperciated. swim likes his vision  

[embezzler]

what are you distilling to seperate the alcohol from and what type of alcohol is it?if it is an ethanol/h2o seperation then you will need to distill it a number of times and then use a drying agent to reach purity(which you probably wont)

what do you mean by wash?

 it depends on what you are seperting from what and which fraction you want to decide where the impurities (volatiles??) are. the first few mls run off should be discarded are you asking how many mls should be discarded?

try be clearer.

[jtryptamine]

sorry not a good explainer  

the wash is the sugar, yeast, nutrient, ect.
So he want ethanol yeah. He's starting to get a better idea of what he's doing though. just let me check it with you guys. here's the boiling points for what will be in the wash

Methanol --------------- 64.7 C
Ethanol ---------------- 78.4
2-Propanol ------------- 82.4
3-Methyl-1-Butanol ----- 99.5
Water ----------------- 100
Butan-1-ol ------------ 117
Pentan-1-ol ----------- 138
Hexan-1-ol ------------ 157

so he's gonna distill off the methanol at 64.7 and discard, he'll go higher than this for safety since what he wants won't come over until 78.4 anyways correct? then collection after that he can learn since there is no danger other than nasty tasting brew, he believes. And your correct he will not be using a drying agent for purity. He does need to buy a coloum though, but for now his current setup will have to do.

[embezzler]

so let a lot of run off come away first even a shot of that stuff will fuck you up.
repeat the distillations though and discard a fair ammount of run off.
swim is not sure how safe the rest of the expected componants are though? look up msds since they will be left in the mix.

 are you going to distill again to collect ethanol and leave all other componants in the rbf??

if you are not using a column what are you using you using, you said its not ghetto ware?

[jtryptamine]

well hes got the distillation column but could use another one for reflux. he was planning to stop collecting at around 82 or 83C and leaving the rest in the flask yeah, do multiple distillations since a good amount of ethanol should still be in the tails.

[Chromic]

Ok, jtryptamine, pretty much all the posts here are from people who don't know much of what they're talking about and have never distilled alcohol before. I take it you mean this for consumption. If you mean it as a solvent, well, I guess most of this advice is valid too. (but there's no need to treat with activated charcoal if it's for use as a solvent)

Use a Turbo Yeast, 8kg sugar, 25L water. It will go to about 18% in 5 days. Filter if you can--but it's not necessary.

Use simple distillation for the batch. Do not discard the first part... don't worry about methanol. It won't be produced by the yeast. Fusel alcohols, okay, yeah, you need to worry about them. They taste horrific. But keep anything up to about 40% that comes over. (T(vap)=96C).

Okay, next you need to fractionally distill the alcohol that you get. This time you throw out the first few mls (just in case you get methanol) and try to distill only up to about 85-90C (BP of the vapor next to the liquid--not at the top of the still head).

You will need a LONG column. Think about something at least 600mm. It's easy to make such a column from 3/4" copper pipe to fit into a 24/40 flask. Pack it with stainless steel scrubbers. It's ideal to have a Nixon-Stone type still head, but not necessary.

Then dilute this down to about 40% alcohol, boil with 5v/v% activated charcoal (from a fish store, there's many sources for this stuff)... then filter, distill again. Keeping just the stuff that comes over at 90%+. You may have to retreat with activated charcoal a couple more times just to have it really palatable. Good luck!

[Chromic]

I've found these four pieces of data useful. Hope they are to you too.

[ApprenticeCook]

Ahhh.... why? what are you trying to do? simple dist ethanol? (drinking alco) from the yeast crap left over...?

embezzler is right, dont go near methanol, its nasty stuff to drink (stupid me tried it out of curiosity ~15mL), and i was sick straight after.

Best to use fractioning column to get pure enough fractions but still going to have some impurities, as long as you distill about 3-4 times with the fractioning coloumn and discard the first and last 10% of the distillate collecting the ethanol bp fraction you should be ok... then use a drying agent to remove the water in solution, filter out the agent and fractionally distill again and remove first and last 10% of distillate range for ethanol. Thats the only safe way to do it in my eyes...

Suggestions?

[elfspice]

have patience grasshopper... raise the temperature slowly. turn it up, then wait for carry-across. wait a decent amount of time, there can be up to a few minutes lag depending on your heat source. Then if nothing comes acros, turn it up a little more. and then wait.

alcohol and water are the two in the mixture that are the most difficult to separate, as they form azeotropes. methanol distills off relatively easily in comparison. slowly slowly raising the temperature allows you to put minimum heat in to get just enough vapour pressure to cross into your condenser.

I haven't done much in the way of alcohol distilling (which is legal here), nor is my heat source that great (damn stupid fixed setting, 0 1 2 3 4) but that's how it worked fractionating naptha, and i didn't have enough heat control to really be confidient i succeeded. However, in some instructions on fractionating i read, might have even been stuff linked from rhodiums site somewhere, said, if you want to fractionate you control the proper fractionation by aiming to only boil the lowest fraction, and only just, to the point of maybe 1.5ml of distillate per minute.

it's damn tedious but if it's ethanol, you'd probably find you distill off the teensy amount of methanol and so forth bla bla... just turn up heat slightly, monitor drip rate, and don't let it get too low. If the temperature is maintained at a certain point everything that can boil off will and no more condensing will occur. the ethanol would come all across at one of those adjustment points and from there on it would be more water and more other junk.

all theory on my part, when i get some good temperature control i will learn how to do it properly and i might be a better person to ask... but this is the theory i've gathered so far, theory plus limited experience. I really like distilling but it's boring, i recommend having something that doesn't generate any risk of sparks nearby to entertain yourself while you absently monitor the drip rate and turn it up as it slows down too much. and check the column temp etc.

oh my condenser is one of those copper liebig jobbies... 500mm long. seems to work quite well, without fractionating, and heating the boiler as high as safe without causing choking, and it dribbles out an almost stream, about 1ml ever 10 seconds or so (makes the process more easy but it can't be as pure done that way) I don't know the advantage of shorter or longer or coiled or whatever at this point. the condenser has been employed vertically and at an angle and is good for more simple distillations vertical (seems to permit slightly faster condensation, or maybe it just reduces holdup).