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Author: Subject: New synthesis of Ethanol
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Absinthe is a nice enough drink but a poor place to start if you want pure alcohol. It's got all sorts of stuff in it.

However, back at the topic, another potential pitfall of producing ethanol from ethyl acetate is the condensation of ethyl acetate with itself in strongly alkaline conditions.
http://en.wikipedia.org/wiki/Claisen_condensation
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Pulver:
Well, I thought the first procedure in Vogel's didn't look to rough to get it up to 99.5% which was all I was looking for.
I was going to use it with suphuric acid for the production of ether to clean my glassware, but opted for the starting fluid route. (Thank you Len1)
So now that I'm not doing that, I need dry it up so that I would be afraid to put it in my orange juice which reduces yields.
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Mood: Torn between two monikers ─ "hissingnoise" and the present incarnation!

My interest in et0H is quite narrow, shadow---blasting-caps and night-caps, in that order.

ScienceGeek's excellent online fulminate synth revived my childhood interest in MF.

Take a bow, SG!

Not having a fume-cupboard I'll end up intoxicated whichever way I use it!

Sho Scheerzz! (hic!)

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Sauron
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Woelen, surely you mean 80 proof (40%) vodka?

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MagicJigPipe
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That was shadow, not Woelen, BTW.

But I second Sauron's question. Would it truly be vodka if it was only 40 proof? That would almost be like a one of those girly drinks like Pucker or peppermint shnapps.

"There must be no barriers to freedom of inquiry ... There is no place for dogma in science. The scientist is free, and must be free to ask any question, to doubt any assertion, to seek for any evidence, to correct any errors. ... We know that the only way to avoid error is to detect it and that the only way to detect it is to be free to inquire. And we know that as long as men are free to ask what they must, free to say what they think, free to think what they will, freedom can never be lost, and science can never regress." -J. Robert Oppenheimer
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If you meant me, Dr. Sauron, I'm sure it was 40 proof. They sell it 1750 mls at a time for about $10 in every market and pharmacy in town. I'll go check to make sure, but watching it go over sure was a waste of time. Sauron International Hazard Posts: 5351 Registered: 22-12-2006 Location: Barad-Dur, Mordor Member Is Offline Mood: metastable I was addressing woelen, but, if both of you say 40 proof/20% then maybe it is so. It's just that I have never seen vodka bottles at anything but 80 (formerly, 86) proof, and 100 proof. The trend seems to be 700 ml bottling at 80 proof replacing 750 ml, and 80 proof replacing 86 proof some time ago. Whether this is being driven by the regulators to make their taxation arithmetic easier, or by chiseling distilleries, deponent knowetrh not. In my country it is now a criminal offense to import anything over 80 proof potable spirits. So no absinthe, no Chartreuse, no 151 rum, etc. The very last bottle of liquor anyone gave me prior to my going tea-total, four years ago, was a nice cask strength (93 degree) Armagnac - which I never opened. Anyone wanting to obtain high proof neutral spirits for solvent use in jurisdictions where it is not readily available can either ferment mash himself, strip that to 40% or so, and fractionate from there. Or buy potable spirits, and fractionate those. Vodka is best as it is already neutral. Rum, cheap brandy, gin, whiskey etc can all be used. 151 rum is great if you can get it, as it is already 75% ethanol. In the case of gin you can remove a lot of the botanicals by treatment with activated carbon, either batchwise with powdered AC or in a fixed bed (long tube) with granular AC (GAC). This is also the method used by home distillers to polish their "vodka". Best done at about 50% ethanol/water. Getting the neutral 95% ethanol to anhydrous is another matter and has been discussed extensively in other threads. It is only necessary if you need anhydrous ethanol. In my locale I can buy Merck anhydrous ethanol, and I can buy denatured 95% ethanol, but the latter is loaded with MEK and god knows what else. It is OK for most recrystallizations. [Edited on 7-5-2008 by Sauron] Sic gorgeamus a los subjectatus nunc. MagicJigPipe International Hazard Posts: 1554 Registered: 19-9-2007 Location: USA Member Is Offline Mood: Suspicious Wow, and I thought my state's liquor laws were bad. Anyway, I wonder, is the normal 80 proof (I know Smirnoff and Absolut both make 100 proof vodkas) more expensive (per amount of EtOH) than this reduced strength 40 proof vodka? If not, why not just get the stronger stuff? Is hard liquor illegal or not allowed in your area? I've often wondered how cost effective it would be to set up an EtOH "distillery". You know, to make it out of corn or something similar. Of course, there would be something illegal about it as it would be the clear eqivalent of "moonshine". Honestly, I don't really care. It just seems like it would be kind of a hassle to concentrate and purify the resulting EtOH. I've read a little bit about EtOH production but it was a long time ago. Perhaps that will be one of my projects I'll do in the future when I have more money and time. It certainly can't hurt if it's done "legally" or in absolute secrecy. Does anyone have ANY experience with production of EtOH at home? Surely this has come up before. Time to UTCSE (UTcrappySE)! [Edited on 5-6-2008 by MagicJigPipe] "There must be no barriers to freedom of inquiry ... There is no place for dogma in science. The scientist is free, and must be free to ask any question, to doubt any assertion, to seek for any evidence, to correct any errors. ... We know that the only way to avoid error is to detect it and that the only way to detect it is to be free to inquire. And we know that as long as men are free to ask what they must, free to say what they think, free to think what they will, freedom can never be lost, and science can never regress." -J. Robert Oppenheimer Sauron International Hazard Posts: 5351 Registered: 22-12-2006 Location: Barad-Dur, Mordor Member Is Offline Mood: metastable In Thailand it is all driven by the de facto monopoly of Suramaharaj Co., (King's Liquors) which used to be the concessionair of the royal monopoly (now discontinued). By a revolving door system this company keeps a tight grip on the Escise Department and that's what sets the regulations. I tried to get into this racket to make absinthe for export, with heavy political backing, including the brother of the deputy director general of Excise, but it turned out that she was looking forward to a big consulting retainer from Suramaharaj when she retired - in other words, they bought her before we even put in a bid. Meanwhile the Public Health Ministry has an anti-alcohol program going (the same hypocrisy goes on with regard to tobacco, which is grown here as well as imported). Whether the 80 proof limit is at the behest of the liquor monopoly or the PH people, I am not sure. I am not the only one frozen out of the booze racket. Suntory of Japan in partnership with the Boonrawd Brewery folks wanted to set up a distillery to make Suntory here for export back to Japan. They got fucked too. Suntory imports Thai glutinous rice and ferments that to ethanol to make Suntory in Japan but they run afoul of the powerful rice farmer lobby and so they figured why not do the fermenting and distilling here? But, Suramaharaj blocked them. Welcome to Asia! Bottom line, my former partner now makes Jade Absinthe (I named it) in France, and distributes it through a British company. I dropped out. We also investigated doing this in Laos (communists) or Cambodia (thugs) but then I determined that the real market for absinthe was about 10% of what I'd been led to expect, and thus not worth my while. So, adios. I'm sure my former partner has a nice hobby, and makes a fine product. But he is not getting rich, even at$100 a bottle. Just not enough bottles moved for that.

MJP, there's a great deal of information about home fermentation and distilling of ethanol on the net, the best to my mind being my old pal Tony Ackland's website, Tony is an enthusiastic Kiwi chemical engineer and home distiller. New Zealand is one of the few places where this is legal.

Another old pal, Gert, in Malmo, Sweden, sells turbo yeasts for fermenting sugar-water and a variety of other substrates to concentrations as high as 20% (but getting much beyond 15% requires very efficient temperature control.) He also sells Rashig rings for column packing, and for the large semi-underground Scandiavian bootleg market, essences for flavoring vodka (including a horrible one for absinthe.) www.partyman.se. I am sure Gert has distributors for his yeasts in USA.

Fermenting is best done in a cool dark place. Fermenting in a tropical climate like mine requires cooling systems, and under he best of circumstances is a messy laborious, somewhat finicky process demanding attention to detail, cleanliness , and careful technique. In practice you need to keep microbial contamination to a minimum, that means cleaning up with biocides, but then you have to rigorously remove all traces of the biocide from the fermentation vessel or else they cheerfully kill the yeast! Biocides also are necessary to keep the yeast from overgrowing the entire area (floors, walls, ceilings, furniture) and again, protecting the fermentation vessels from contamination with biocides. Bacteria are an enemy as they multiply much faster than yeast and love sugar water. So do insects. Sound like fun? Welcome to Biotechnology 101. A microbiology lab is de rigeur for keeping track of what is going on in your ferments and environment. You will have airborne yeast and airborne bacteria in absundance.

[Edited on 7-5-2008 by Sauron]

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Sauron
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The Tony Ackland website is

http://homedistiller.org/intro.htm

Very valuable information there.

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Twospoons
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I'll second Sauron's link - some excellent info there that I've used to great effect. Building an alcohol still is fairly easy. I used a stainless stock pot and put a jug element in the bottom. For a reflux column I used a 250ml measuring cylinder, with a hole bored in the bottom (diamond holesaw), packed with knitted copper mesh and siliconed to the potlid. An adjustable reflux head was built from odd bits of broken glassware (I save the ground joints) and creatively applied MAPP gas and silicone .
28L of wash, fermented from 7kg of sugar, yielded roughly 5l of spirit at an estimated 90%. Didn't bother to measure the conc - I dilute by taste!
Copper mesh works very well as column packing. Copper is also supposed to destroy any sulphur compounds coming off the wash.

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Sauron
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A couple of tips:

1. There's an awful lot of dormant yeast that settles out of the mash, and even after you filter or decant the mash will continue to throw more. Removing the dormant yeast is important because it is a source of diacetyl off slavors if it is overheated in distillation.

2. As any confectioner will tell you, sugar-water loves to boil over, and mash stiull contains enough unfermented sugar to do the same. This can be very sticky and messy, be prepared.

Twospoons' estimated yield of 5 liters 90% from 28 L mash is about right, it means he got the mach to about 16% abv or a little better which is normal. With special yeasts and expensive equipment it is possible to get to 20% but honestly, it is not worth the trouble and expense to get 6 L instead of 5 L. At those levels the heat of fermentation is such that it has to be removed by external cooling (or internal cooling coils) with good engineering to hold temperature constant +/- 1 C or so. This costs money.

I also recommend the website of a company called Louisville Brass & Copper if you want to see how real distillers, even microdistillers, do it with commercial copper stills from 5 liters to 200 liters, and on up to proper massive industrial setups.

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Contrabasso
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Is the commercial formation of anhydrous alcohol not done in the gas phase? by catalysis?

Distillation of fermentation mash can get stuck at the azeotrope point. Be very careful that absolute alcohol in the UK is produced by the addition of benzene - leaving a benzene trace in the alcohol.
Sauron
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As a practical matter one never distills straight from mash (16% or so) to high proof spirits, you first strip the mash, then polish the ethanol/water mixture with GAC to remove gross congeners, then distill the 50% or so to high proof, which is at best the azeotrope.

The use of the ternary azeotrope with benzene to break the azeotrope is one method of producing anhydrous ethanol but such ethanol is no longer potable.

The azeotrope can be dehydrated with molecular sieves, corn meal, calcium oxide, etc. But no one bothers to take ethanol to anhydrous state for drinking purposes, there's no point. Anhydrous ethanol is a solvent or reagent only, and for that purpose, the trace of benzene from the ternary azeotrope technique is not usually a problem.

Just don't use that ethanol to make Purple Passion punch.

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MagicJigPipe
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I couldn't even imagine attempting to consume 100% EtOH (you're not even supposed to consume 95% and THAT is a hard burden to bear, especially if you're no longer a teenager ).

Did I mention that there is actually a Sunday alcohol market in my area where people buy alcohol during the week and sell it at nearly double the price on Sundays? Alcoholics LOVE Everclear (most bang for the buck) and it would probably be profitable to sell the EtOH on Sundays for an awesome profit here. Unfortunately, I consider that no different than peddling pure meth so I won't have any returns but...

EtOH production sounds very cool to me. Thanks for the link, Sauron. I do believe this will be one of my projects in the near future! (I mean, no it won't, that would be illegal...)

I have a strong interest in setting up dedicated "stills" and such for the synthesis of certain compounds (my next project is to set up a dedicated sodium benzoate/base to benzene "still"). It's just awesome to know that, no matter what, I can always have benzene, EtOH etc... whenever I need it.

OT
Speaking of which, has anyone else in the US noticed that benzene seems about as hard to get as 55 gallon drums of phenylacetone (not that I've tried but I can imagine)? What the hell is up with that? I mean, cigarettes and gasoline are still around and they cause cancer! I don't know, it just seems like everyone is WAY too paranoid. I thought I scored once with this Canadian company but, in the end, they told me that they could not ship benzene to the US. I mean, for a chemical so widely used in industry (styrene production) it is exeedingly difficult to obtain. Hell, until I get my benzene "still" set up I would be willing to pay HAZMAT charges for it...

[Edited on 5-8-2008 by MagicJigPipe]

"There must be no barriers to freedom of inquiry ... There is no place for dogma in science. The scientist is free, and must be free to ask any question, to doubt any assertion, to seek for any evidence, to correct any errors. ... We know that the only way to avoid error is to detect it and that the only way to detect it is to be free to inquire. And we know that as long as men are free to ask what they must, free to say what they think, free to think what they will, freedom can never be lost, and science can never regress." -J. Robert Oppenheimer
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Jig,

Here's 1of 4 listings from chemsavers. Their ACS is $35 + shipping. However they seem to be out of stock on all 4. They sent me a liter a couple months ago. Benzene 71-43-2 Grade Purity DOT Formula View for organic residue extraction (GC) min. 99.5 % Benzene, 3, UN1114, II, ORM-D. C6H6 Size Price Shipping 1L$48.99 $10.50 500mL$32.62 $8.50 Did you get your car fixed? Using a DVOM at the starter will tell you if you are getting current from the ignition switch. If not, it could be the switch. Same thing at the headlights. Pull off the connector and make sure current is not getting to front. If its not, check for continuity from the fuse and then the relay to the light connector. [Edited on 8-5-2008 by shadow] MagicJigPipe International Hazard Posts: 1554 Registered: 19-9-2007 Location: USA Member Is Offline Mood: Suspicious Yes, I finally just said "fuck it" and rigged a switch that ran from the positive terminal of the battery to the the starter and then into the car (to switch it on). I did the same with the headlights. Now, basically I have a push button switch in the car to activate the starter and a toggle switch for the headlights. I made it look as professional as I could. It's not bad, I can live with it. I mean, I'm probably gonna drive it 'til it falls apart anyway (I'm not going to sell it). That way I can take the A/C and various fans and the radiator/condenser out for lab use once it's no longer drivable. Oh yeah, I figured out it was most likely the ignition or the wires. Both of those things I really didn't want to mess with replacing. I mean, everything works fine now and I only spent$15 (I had most of the wires and electronics tools already).

I'm sorry, but $60 for a liter of benzene is insane. Did you say it was ACS Reagent? If it is I suppose that's okay, but I really don't need reagent grade. The place in Canada was selling it for$80 a gallon including shipping.

[Edited on 5-8-2008 by MagicJigPipe]

"There must be no barriers to freedom of inquiry ... There is no place for dogma in science. The scientist is free, and must be free to ask any question, to doubt any assertion, to seek for any evidence, to correct any errors. ... We know that the only way to avoid error is to detect it and that the only way to detect it is to be free to inquire. And we know that as long as men are free to ask what they must, free to say what they think, free to think what they will, freedom can never be lost, and science can never regress." -J. Robert Oppenheimer
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 Sciencemadness Discussion Board » Fundamentals » Reagents and Apparatus Acquisition » New synthesis of Ethanol Select A Forum Fundamentals   » Chemistry in General   » Organic Chemistry   » Reagents and Apparatus Acquisition   » Beginnings   » Responsible Practices   » Miscellaneous   » The Wiki Special topics   » Technochemistry   » Energetic Materials   » Biochemistry   » Radiochemistry   » Computational Models and Techniques   » Prepublication Non-chemistry   » Forum Matters   » Legal and Societal Issues