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Cou
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Do u guys make glacial acetic acid from 5% vinegar?
5% vinegar is very cheap. 1 gallon of 5% white vinegar for $3 at most, contains about 3.15 moles of acetic acid, can make about 180 mL of glacial
acetic acid. I think u could just react the gallon of 5% vinegar with baking soda, boil it down to sodium acetate, and then use sulfuric acid to make
acetic acid from that. Probly a lot cheaper than using the haloform reaction.
[Edited on 26-11-2019 by Cou]
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DavidJR
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That's an awful lot of work to get glacial acetic acid, which isn't all that expensive to just buy. So no, I wouldn't do this.
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Cou
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I enjoy the challenge of making things OTC only (not even amazon or ebay)
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j_sum1
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Find out why ot is called glacial acetic acid and take it from there.
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SWIM
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Getting glacial acetic acid by distillation would require a pretty good distillation column.
15 or 20 plates perhaps?
Don't even bother with a 400 mm Vigreux.
And consider this: A gallon of 5% vinegar has 187 ml of acetic acid in it.
That means with a perfect still you'd still need to distill 3563 ml of water to get that acid, and with a real-world pretty good still you'd maybe
get 100 ml of acid for all that work.
And a lot of work it would be, because water and acetic acid are very hard to separate.
Why not neutralize that vinegar with baking soda and boil it down instead?
Dry the powder and add sulfuric acid to liberate the acetic acid in a still.
(dry powder goes in boiling flask, add H2SO4 from a dropping funnel. Freed acid will boil from heat of reaction.)
In my experience it's still hard to get high purity that way. Maybe I didn't dry the acetate enough.
Only tried it a couple of times.
If you just need really strong, but not totally dry acid I recommend you puzzle over the words of our local Edward Nygma: j_sum1.
A bit of search engine searching may help.
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XeonTheMGPony
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You can refine the product of neutralization by using Methanol.
Acetate will dissolve non acetate wont.
Dissolve then filter, then evaporate.
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DavidJR
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Yeah, you can concentrate vinegar quite significantly by fractional freezing.
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G-Coupled
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From what I've gathered, it's a total ballache to distill to GAA from weak white vinegar because of azeotropes or something - hard to distill to any
useful degree IIRC. Yiou can achieve some progress towards it by freeze distilling it as someone mentioned, but the yields are paltry, also IIRC.
I looked into this some time back and concluded that even with the ruinous 'hazardous handling' delivery surcharge, and the fact that it's not very
cheap, it's still worth it to just purchase some if you're only needing a litre or two IMO.
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S.C. Wack
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Everyone has missed the never before seen flaw in this brilliant, unheard of plan.
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G-Coupled
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lol, indeed. 
NEXT UP - 'Is there any way to make Acetic Anhydride from vinegar and old bootlaces?'
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S.C. Wack
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The plan may work in some countries but not with vinegar in the USA among others.
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G-Coupled
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I thought it was more to do with physics, enthalpy and all that good stuff, and not the location one attempts it in? o_0
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S.C. Wack
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Vinegar is not the same thing worldwide. Vinegar may (USA) or may not have a certain legal definition.
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Ubya
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i bought some vinegar from east europe that is 25% acetic acid
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feel free to correct my grammar, or any mistakes i make
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G-Coupled
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Stronk winegar.
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TheMrbunGee
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Did Cou change the original post? He mentions reacting it with baking soda and then with sulfuric acid, I don't see any wrong in doing that to get the
concentrated acetic. I have done that in the past and it worked, even with no lab equipment what so ever at that time. boiling off 3 + liter of water
will be time consuming and actually adds significant cost to end product, but If you have curiosity to go trough that - go ahead.
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G-Coupled
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Quote: Originally posted by TheMrbunGee  | | Did Cou change the original post? He mentions reacting it with baking soda and then with sulfuric acid, I don't see any wrong in doing that to get the
concentrated acetic. I have done that in the past and it worked, even with no lab equipment what so ever at that time. boiling off 3 + liter of water
will be time consuming and actually adds significant cost to end product, but If you have curiosity to go trough that - go ahead.
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Did you end up with an appreciable amount of actual Glacial Acetic Acid doing that?
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TheMrbunGee
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Keep in mind, that I was 17, did no calculations, my distilation setup was champange bottle with polipropilene tube in glycerine bath, and as a
condenser I used a jar in ice bath. It was incredibly bad design, tube probably added many impurities, a lot of acid did not condense and fumed in the
air.
in the end I still got about 80 ml of quite strong stuff, form 1 liter of 7% vinegar. it froze up in fridge (+3°C), was not 100% for sure. I was not
aiming for 100% tho, so it is not like I tried and failed, my goal was to get it way stronger.
But with a decent setup and at least some experience - it seem very doable.
EDIT: Actually found a picture of said setup, all warped in foil. you can see the tube going in "condenser jar".
[Edited on 29-11-2019 by TheMrbunGee]
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S.C. Wack
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USA vinegar leaves a yucky residue when distilled to dryness or is neutralized and evaporated. A sticky brownish problem turning black with sulfuric
acid, which can be easily avoided without a silly recrystallization from organic solvents...as I've only hinted at, since it's all been talked about
before and there's no reason to start a new thread IMHO.
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G-Coupled
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Cool - you must've purified it quite a ways if it froze near the temps that pure GAA does.
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beta4
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A few years ago, I tried making a few copper salts just for fun, and wanting to make copper acetate I had the idea to make concentrated acetic acid
from vinegar. Turned out a mess and I gave up. The fallback was to buy sodium acetate and make acetic acid from it, which worked quite well.
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TheMrbunGee
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| Quote: |
Cool - you must've purified it quite a ways if it froze near the temps that pure GAA does.
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I might have freezed and poured off the liquid part few times, but nothing much else was done (That was long ago, hardly remember the facts).
| Quote: Originally posted by beta4 | | A few years ago, I tried making a few copper salts just for fun, and wanting to make copper acetate I had the idea to make concentrated acetic acid
from vinegar. Turned out a mess and I gave up. The fallback was to buy sodium acetate and make acetic acid from it, which worked quite well.
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That is Why I needed acetic acid.
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AJKOER
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I prepare copper acetate quickly by adding solid Cu metal (from a plumbing pipe) to 5% vinegar + 3 % H2O2 and a touch of sea salt. Jumpstart in a
microwave (avoids the electrochemically induced inception period) for less than a minute. Replenish the H2O2 as needed.
The radicals formed (including the acetate radical) produce an energetic reaction that exceeds even your strongest standard chemical reaction
expectations with strong acid acting on Copper metal.
Don't believe? Give it a try, or continue to waste your time and money!
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Cou
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| Quote: Originally posted by AJKOER | I prepare copper acetate quickly by adding solid Cu metal (from a plumbing pipe) to 5% vinegar + 3 % H2O2 and a touch of sea salt. Jumpstart in a
microwave (avoids the electrochemically induced inception period) for less than a minute. Replenish the H2O2 as needed.
The radicals formed (including the acetate radical) produce an energetic reaction that exceeds even your strongest standard chemical reaction
expectations with strong acid acting on Copper metal.
Don't believe? Give it a try, or continue to waste your time and money! |
Wow!
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TheMrbunGee
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| Quote: Originally posted by AJKOER | I prepare copper acetate quickly by adding solid Cu metal (from a plumbing pipe) to 5% vinegar + 3 % H2O2 and a touch of sea salt. Jumpstart in a
microwave (avoids the electrochemically induced inception period) for less than a minute. Replenish the H2O2 as needed.
The radicals formed (including the acetate radical) produce an energetic reaction that exceeds even your strongest standard chemical reaction
expectations with strong acid acting on Copper metal.
Don't believe? Give it a try, or continue to waste your time and money! |
That is just another way to it, easier, cheaper, but well - it is not about expenses of time and money, at least for me- its about the journey,
learning and sense of accomplishment. but next time I'll need copper acetate, I will for sure try that! 
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