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arkoma
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Arkoma attempts 95% azeotropic EtOH
13 APRIL 2016 Attempt at 95% Azeotropic Ethnanol
I have attached actual photos of my lab notebook.
Summary:
Well, I started with 56% EtOH and H2O solution. Figured this would be as straight forward as the initial distillation of my low percentage
EtOH wash. First off, I way overloaded my 1 litre RBF. 819ml. STOOPID. My heat source is a fry daddy with no thermostat. This caused several
SERIOUS bumping incidents, including one that blew my thermometer adapter out of my distillation head and sprayed boiling EtOH everywhere. Thank
goodness there was no source of ignition, and I did have a fire extinguisher within arms reach. By trying to "hurry" at the end of an 2 hours I ended
up with 100ml of 87% EtOH per my hydrometer. I could have burnt my house down.
Conclusions:
I need a water bath instead of a temperature unregulated oil bath for a distillation of EtOH at high percentages. Or perhaps a triac control or maybe
a damned real thermostatically controlled hotplate. THIS STUFF BUMPS LIKE YOU WOULD NOT BELIEVE, noobs and youngsters take note.
What I listened to "While Doing The Dirty" LOL;
Belinda Carlisle-Heaven is a place on Earth
Marilyn Manson-Tainted Love
Katy Perry-Wide Awake
Pet Shop Boys-East End Boys
Cranberries-Linger
Disturbed-Down With the Sickness
Duran Duran-Rio
Easton Corbin-A Little More Country Than That
Patti Smyth-I Am the Warrior
Lady Gaga-Poker Face
Madonna-Music
Pistol Annies-Hell On Heels
Metallica-The Memory Remains
Brooks & Dunn w/Reba-Cowgirls Don't Cry
Carrie Underwood-Blown Away
Blondie-Heart Of Glass
Sugarland-All I Want To Do
Jamey Johnson-In Color
Slayer-Seasons In the Abyss
Travis Tritt-Modern Day Bonnie and Clyde
Megadeth-A Tout Le Monde
Jethro Tull-Locomotive Breath
Now, on to "Bad Habits in the Lab"--DRINKING--Just noticed I "lost" an hour in my notes *sigh*
    
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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crystal grower
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Yay Arkoma, Im glad nothing happened to you  , by the way, you're real mad
scientist! 
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arkoma
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This is gonna be harder than I thought. Think I might need to distill over oven dried gypsum. Getting to 60, 70% is no sweat, 95% is a challenge
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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j_sum1
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That is quite a playlist you got going there.
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arkoma
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I have "Eclectic" taste. Put vlc on random and let it go. Have HUNDREDS oif music videos.
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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Magpie
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If you are distilling just pure water and alcohol (no mash particles), AND you have added boiling stones (I use porous pottery shards) you should not
have bumping problems. Bumping problems are often caused by solids settling on the bottom of the pot and causing localized overheating.
The single most important condition for a successful synthesis is good mixing - Nicodem
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JJay
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I have done this dozens of times with no boiling stones or anything of the sort. A boiling water bath is definitely the way to go. I'm not sure why
you would insulate your Vigreux.
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violet sin
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First off, just have say... Was a little dissapointed to see you were making 95% not drinking(trying) 95%. Lol.
Secondly, nice work keeping that noggin fed and trying new things. If you get some of the kinks worked out, you may find aga pulling down your
driveway one day boiling chips are nice, just for peets sake be smarter than i
was... Put it in first, not after its warmed up.. steam clean your flesh over the flask neck and end up wearing god knows what some time(think it was
copper chloride for me). Keep up the good work man!
Here is something dirt cheap that could help:
http://www.ebay.com/itm/50-110-C-Heat-Cool-Temp-Thermostat-T...
$3.19 free s/h, can switch 10A appliance so may be a winner!
Another note,.. put a glass globe over you light bulb. Looks like it takes one, with 3 or so set screws on the rim. Be a shame to have temp shock
give you an ignition source if it were to spray from your glassware just right. I live by Murphy's law daily(technically it's my law, but i take no
responsibility for the pizza franchise). Think ahead of the curve
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woelen
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Indeed, that was a good lesson learned and happily nothing worse happened than the loss of some ethanol. This could indeed have resulted in a huge
fire!
You need a long column and need to apply minimal heat so that the ethanol just boils over. In that way, you should be capable of getting 85 to 90%.
You will need patience though. If you hurry and have a lot of liquid distill over in short time, then a lot of water distills over as well.
Getting to 95% azeotrope will indeed be hard. I think that a chemical drying agent like CaSO4 or CaCl2, combined with distilling, is the best for
getting water out. Having all these solid materials, however, introduces other problems like caking. Especially CaSO4 will lead to a very hard to
remove cake of solid.
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Corrosive Joeseph
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Quote: Originally posted by woelen  | Indeed, that was a good lesson learned and happily nothing worse happened than the loss of some ethanol. This could indeed have resulted in a huge
fire!
You need a long column and need to apply minimal heat so that the ethanol just boils over. In that way, you should be capable of getting 85 to 90%.
You will need patience though. If you hurry and have a lot of liquid distill over in short time, then a lot of water distills over as well.
Getting to 95% azeotrope will indeed be hard. I think that a chemical drying agent like CaSO4 or CaCl2, combined with distilling, is the best for
getting water out. Having all these solid materials, however, introduces other problems like caking. Especially CaSO4 will lead to a very hard to
remove cake of solid. |
How long is a long column............?
This is VERY similar to my latest project. I am using a water bath (an old deep fryer with no thermostat running water), a 1l RBF and a 300mm length
homemade column of 30mm stainless tube filled with stainless steel scrubbers. I also have a 400mm length of the same tube which is about to be tried
next. I have just taken delivery of an 'alcoholmeter' and will report back with my findings.
My starting material is distillate from the mash in the 'beer stripper' and measured 58% EtOH
95% is also my target figure..............
I will be watching this thread with great interest.............
CJ
Being well adjusted to a sick society is no measure of one's mental health
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aga
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It just so happens that i'm also distilling booze, although i want 100% EtOH.
woelen's suggestion of gentle heating does seem to help.
Insulating the vigreux might be counter-productive, although i'm not sure exactly why (something to do with the reflux equilibrium).
After two initial runs from a 1L bottle of 37.5% vodka, the distillate was distilled again to get around 350ml of constant-boiling 78C ethanol.
Next up is dehydration using tripotassium phosphate if i can sucessfully make it properly. CaO doesn't seem to work very well for me.
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woelen
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A column of 30 to 40 cm should be OK. I myself have a vigreux and this works quite well, but you need to heat, so that the top of the column is just
reached and the column must be wrapped in isolating foil or linen or something like that, especially if there is variable air-flow in the room where
you perform the distillation. Otherwise the behavior is erratic, at one moment the distillation goes too fast, at other moment nothing distills over.
I can see in my colum that the top of the vapor column moves up and down with wind around the column varying in speed and direction.
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JJay
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I usually do three runs using an uninsulated 30 cm Vigreux with a boiling water bath and then finish dehydrating with 3A molecular sieves. This
doesn't completely eliminate ketone denaturants (for that I could probably reflux with sodium hydroxide but I'm not drinking the stuff), but the
resulting anhydrous ethanol works ok for most purposes.
[Edited on 14-4-2016 by JJay]
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CuReUS
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I may be paranoid,but a naked incandescent bulb so near a distillation setup for ethanol sounds like a recipe for disaster,does it not ?
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aga
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Paranoid.
I use an open flame spirit burner for ethanol, acetone etc.
That said, the shed is pretty much expendable.
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Chemist_Cup_Noodles
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Also if you don't have any boiling chips, just add some glycerin to your alcohol and water. I did it the other day just sort of chucking science at
the wall, and I must say I'm very happy with the result. It has almost triple the BP of water, and quadruple that of EtOH. This stuff will make the
liquid a lot more viscous and thick and hopefully it won't bump as much. It will also allow the temperature of the solution to be a little higher
while boiling. By this means I've gotten some very vigourous but very tame boiling that nicely hovers ~85oC so the alcohol boils out truly
quite fast. And because it bumps very gently if at all with the addition of the glycerin, I don't even need a vigreux column. It actually sort of
bubbles like the swamps of Dagobah.
I too use a hot oil bath, and I do this outside with absolutely no possible sources of ignition. But I like to keep my oil bath around
~120-130oC. At this temperature I still get a fantastic drip rate coming out of my condenser. And after all is said and distilled I just
swirl around my glycerin and most of the remaining EtOH escapes, and then I burn off any last little traces. 10/10 would recommend.
I'll be honest-- We're throwing science at the wall here to see what sticks. No idea what it'll do.
-Cave Johnson, Portal 2
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arkoma
Redneck Overlord
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@violet sin 95% can be rather toxic
@JJay no denaturants as this was a simple sugar "wash" made with turbo yeasts
I had a bunch of bent pennies in the bottom of the flask. I'll try actual porcelain chips as the name of the game is nucleation sites, right?
@aga, I can't explain the science behind it, but Mr. Vogel in his wonderful Org Chem book says to keep a fractioning column insulated or even in some
cases heated. I can use Trisodium Phosphate to dry EtOH? I have a box of it as it is still OTC here.
And yeah, I need to do two things:
1) Do this earlier in the day so I ain't as "buzzed" on Tasty Malt Beverages
2) cover and move that damn light.
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
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JJay
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I am of the opinion that insulation isn't really necessary with liquids boiling under 100 C. What really matters is the reflux ratio; insulation tends
to lower it, and higher reflux ratio leads to purer product. Of course, you may need to insulate if your product can't make it through the column.
Here are Vogel's words on the subject:
In practice, it is usual to employ a fractionating column to reduce the
number of distillations necessary for reasonably complete separation of
the two liquids. A fractionating column is designed to provide a continuous
series of partial condensations of the vapour and partial vaporisations
of the condensate and its effect is, indeed, similar to a number of
separate distillations. The effect of partial condensation will be evident
from Fig. /, 4, 2. If the temperature of the vapour is lowered, it will partly
condense giving a hquid richer in B and leaving the vapour richer in A.
The vapour passing up the column will accordingly contain more of A than
did the vapour which left the boiling liquid. Similarly the hquid returning
to the flask will contain relatively more of the less volatile component B.
A fractionating column consists essentially of a long vertical tube
through which the vapour passes upward and is partially condensed;
the condensate flows down the column and is returned eventually to the
flask. Inside the column the returning hquid is brought into intimate
contact with the ascending vapour and a heat interchange occurs whereby
the vapour is enriched with the more volatile component A at the expense
of the hquid in an attempt to reach equihbrium. The conditions necessary
for a good separation are :—(i) there should be a comparatively large
amount of hquid continually returning through the column ; (ii) thorough
mixing of hquid and vapour ; and (iii) a large active surface of contact
between liquid and vapour. Excessive cooling should be avoided ; this
difficulty is particularly apparent with liquids of high boiling point and
may be overcome by suitably insulating or lagging the outer surface of
the column or, if possible, by surrounding it with a vacuum jacket or an
electrically heated jacket. Various types of laboratory fractionating
columns are described in Sections II, 15-11,18
[Edited on 14-4-2016 by JJay]
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arkoma
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As soon as I get my "Safety Protocol" a bit more in hand, I'm going to re-attack this. I might try it with and without the foil. I've got Vogel's
Third in eBook. My older brother had a damned HARD BACK of it once. Got stolen, dangit.
I think the biggest thing I need to realize is that I need to slow way down on my input of heat. The last piece
of my "Bunn-O-Matic" that I haven't utilized yet is this thermostatic control. I'm seeing it repurposed to rein in the FryDaddy
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
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JJay
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A boiling water bath is the perfect temperature for this application - hot enough to boil ethanol but just not quite hot enough to boil a flask of
water. You can use a higher-tech solution, but it's going to be awfully hard to find one that works better than boiling water.
I've been thinking about using thermostatic controls too, but I'd want one that is good to 300 C.
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aga
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Column insulation must certainly depend on ambient temerature.
I have no idea where Vogel lived, cold or hot.
Here the ambient temps are relatively high (24+) at least during the day.
In my current ambient temperatures i think that a water bath would be an excellent choice for EtOH distillation, the column needing no insulation.
Reading your post AFTER doing 5 EtOH disty runs today makes me feel like an idiot.
Nothing new there then !
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aga
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Gentle boil dude, just like, yeah, simmer.
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arkoma
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OK. I dug out the "Bunn-O-Matic" thermostatic control and wired it to an outlet. Anyone that notices the duct tape, know that I AM a Red Green devotee. The temp control isn't very "fine", BUT I can keep the temp within' MUCH more acceptable limits. Hovering around 93 C is way
better than the wide open temp of around 202 C.
This evenings notes and "playlist" I'm thinkin' the playlist is kinda like solving a blockchain hash--"Proof of Work" LOL--plus y'all get a peek into
the mind of an eccentric middle-aged Neck*
*Y'all do get the pun, dontcha'?
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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Sparklehorse
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Arkoma, love your posts and sense of humor. Also great taste in music. Posting playlists should be a forum requirement
I just did about the same thing, starting from vodka, distilled in 1L RBF with a vigeraux, but I was using a mantle/stirrer. Looking at the column, I
could see the difference between the water condensation and the ethanol condensation and sort of a break about half way up the column where the water
condensation stopped and ethanol was more pronounced. As the distillation approached completion, the water condensation slowly worked its way up until
it was all the way in the still head. I was thinking that as long as I didn't have any water condensation in or near the head, that the ethanol coming
over should be pretty close to azeotropic. The water would for many droplets while the Ethanol hardly formed any. After the first run I redistilled
the distillate, dried over 3A sieves, and then filtered through diatomaceous earth to get rid of the particulate from the sieves. I was shooting for
100% anhydrous but I don't really have a good way to check the moisture content besides checking the density.
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JJay
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I'm not really sure where to post playlists. I am in a KMFDM mood today:
KMFDM - Krank (Official Music Video)
KMFDM - Megalomaniac [HD]
KMFDM - A Drug Against War - Bohemia Afterdark
KMFDM - Amnesia (Official Music Video)
Juke Joint Jezebel - KMFDM
KMFDM - Bitches
KMFDM - Stray Bullet
KMFDM - Looking For Strange(Super Strange mix).
KMFDM - D.I.Y
KMFDM - Free Your Hate
KMFDM - Virus - (Ghost In The Shell)
Eisenfunk - Pong
KMFDM - Power
KMFDM - Anarchy
KMFDM - I Am What I Am
KMFDM - Godlike
KMFDM - Money
KMFDM "I Heart Not" (Official Video)
KMFDM - Professional Killer
KMFDM - Bait And Switch.
PSYCLON NINE "parasitic" -official-
KMFDM - Risen
KMFDM - Light.
KMFDM - Today
KMFDM - Blackball
KMFDM - Waste
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