On Tue, 10 Sep 2013 08:21:49 -0400, Joe Gwinn
wrote:

In article , Ed Huntress
wrote:

On Mon, 09 Sep 2013 21:33:58 -0400, Joe Gwinn
wrote:

In article , Ed Huntress
wrote:

On Mon, 09 Sep 2013 08:53:53 -0400, Joe Gwinn
wrote:

In article ,
Scromlette wrote:

It's got some minor metal work involved, but unfortunately no guns or
politics.....

I use quite a bit of methylated spirits to clean electronic PCBs as
part
of a cottage business I run. The solvent becomes laden with dissolved
rosin flux & has to be discarded so I've been thinking about distilling
it for reuse. It's costing me 3 or 4 dollars per litre.


I was toying with the idea of electrically heating an old pressure
cooker vented through either a copper coil or an old refrigerator heat
exchanger. I'm not sure if draping wet cloth on the heat exchanger
would
be sufficient cooling.

This can work, but be aware the some of the vapor will escape, and is
*very* flammable. I would do this outside, well away from away
buildings.

A long enough bit of copper tubing will work as a condenser, so long as
there is adequate airflow.

The alcohol may destroy the seal rubber. Some pressure cookers will
accept large viton O-rings. Maybe some makers use viton.


I think the BP of the methylated spirits is ~ 82 Celsius (180F).

That sounds about right.

It's not a good idea to get the pot too hot. I'd set it up in a double
boiler arrangement, unless you implement an automatic controller.
Regulating temperature by hand without a double boiler is likely to
cause trouble.


Has anyone any experience doing this sort of thing (moonshine perhaps?)

Lots of folk, but they are in the woods, and tend to shoot revenuers
and other nosey people.


Will it be worth the effort?

Depends on volume of alcohol to be processed.


Joe Gwinn

If you cool the condenser, vapor doesn't have to escape. In fact, you
can seal the outlet with a cork or rubber stopper and put a simple
gooseneck (a manometer) in the same stopper, and you can maintain
*negative* pressure.

Yes, I've done it, with a fancy laboratory reflux still made of 100%
glass, distilling ethyl alcohol (you blow off the fusel oil and light
aromatics, waiting for the temperature to indicate ethanol, before
turning on the cooling water). It works as well with copper, and it
doesn't have to be reflux.

True enough. But I'm assuming a homebrew still, far from lab grade.
I'd start outside for sure.


If this is methanol, check for a potential reaction between the
alcohol and copper. Ethyl alcohol is no problem, obviously, but I
don't know about methyl.

Hmm. Never heard of this, but maybe. Perhaps one of our resident
chemists will chime in.


I've seen copper-coil condensers run through a bucket of water that
will cool and condense the outlet to negative pressure. You just have
to pour in cold water from time to time, and let the excess flow over
the side of the bucket. That's what the gooseneck is for -- to tell
you when you're getting positive pressure and you need to pour cold
water around the condenser.

Why do you want negative pressure, given that ethanol won't decompose
from the heat at atmospheric pressure?

Joe Gwinn

Just to avoid explosive vapors.

OK. Making the still airtight will require care and workmanship, but
is certainly doable.


The reason I think you should check the corrosive effects on copper is
that methanol has been a problem with copper and brass parts in race
cars, where it's used as a fuel.

I know that ethanol stills have been made of copper forever. The big
issue was that the joints needed to be silver brazed, not soft
soldered, so the hooch wouldn't contain too much lead.

Well, I think you'll find that most of the pot stills made during
Prohibition actually were soft-soldered with lead-tin solder.

As I mentioned, my uncle made those things for sale to the moonshiners
in the Jersey Pine Barrens during Prohibition. When I was a teenager
he taught me how to sweat-solder pre-tinned parts (that's how I
soldered almost the entire hot-water heating system in my house), and
he described the process of making a still. I've since seen it
described the same way elsewhere.

I could tell you the details but it's lengthy. The short version is
that the seams were double-folded and they only sweated the contact
point between the *outside* of the outer fold and the body of the
still. It required a lot of skill and a lot of heat because of the
conductivity of the copper. The area was heated with a plumber's
gasoline torch and the sweating was done with massive soldering
coppers.

The solder never contacted liquid and no significant amount of vapor.
If a moonshiner fell asleep and let his pot run dry, the still was
ruined because the solder would melt.

It's interesting stuff. If Prohibition comes back, I've got a
sideline. d8-)



There is some methanol in the fermented mash, and this too must be
discarded to yield potable hooch. The old rule was to discard the
first (fusel oils) and last (methanol) fractions, and keep only the
middle fraction.

Hmmm. I thought that methonol had a lower boiling point than ethanol,
and that it was part of the initial discard.

My memory could be failing on this point.

Someone mentioned azeotropes earlier in the thread. That's for people
with more knowledge than I have, but be aware that some of the
volatile liquids involved, and there are a bunch of them in the
fermentation/distiallation process, form azeotropes and can't be
separated by this kind of distillation. It makes the whole thing
fairly complicated but a home distiller only needs to know a few
basics.


I don't offhand know how much methanol there is in the third fraction,
but it isn't going to be a lot.

When methanol is used as a fuel, what is the problem seen with copper
and brass parts? Whatever the problem, it will be worse in a still,
because of the higher temperature (82 C, not 300 C).

All I've ever heard is that it corrodes several different metals in an
engine, and that copper and brass were among them.

It's not a big problem in racing because you should drain the fuel
system after races are over. But it is a problem if you let it sit
there.


I did a little googling. The effect on aluminum, magnesium, and zinc
is pretty rapid, on brass far slower, and pure copper slower still.
This assumes that the methanol contains some water, which is easily
absorbed from the atmosphere. The methanol vapor in a still will not
contain much water, so the corrosion effects may be greatly reduced.

Joe Gwinn

It's just something to be aware of. What you said there sounds
reasonable. The biggest corrosion problem was with carburetors, and
they're usually aluminum/zinc diecast alloys.

--
Ed Huntress