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happyfooddance
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Cleaning vinegar is usually only 6% acetic. Cooking vinegar is 5%. Not much difference. The bigger problem is that vinegar has a significant amount of
organic contaminants, upon removing water you will find that you have brown rather than crystalline products.
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S.C. Wack
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> The bigger problem is that vinegar has a significant amount of organic contaminants
What is this cleaning vinegar though? Not for food use may mean it's diluted GAA? Only? That would be too cool.
> My only concern is the decomposition temp of the C2H3NaO2 since the trihydrate is meant to decompose at a temp of 122c so wouldn’t it decompose
in the solution which is in contact with a very hot hot plate surface?
122C IDK maybe that's a dehydration temp though in practice it's usually up to 320C.
The old lit. mentions diacetate mixture of acid and K acetate, higher boiling and giving weak acetic acid distillate until heated to 200-300C.
[Edited on 24-2-2018 by S.C. Wack]
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Sedit
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I always had the best results just using Sodium Acetate and Sulfuric acid and extracted using Dichloromethane. This was dried, filtered then the DCM
boiled off and gave me Crystals of Acetic acid every single time on a single distillation.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Magpie
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Sedit, this is very nice, thanks for sharing. I don't make my acetic acid anymore, but buy it.
The single most important condition for a successful synthesis is good mixing - Nicodem
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happyfooddance
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Heinz brand cleaning vinegar is the same product as their "food" vinegar, just slightly concentrated. It says so on the bottle.
Sedit, that is indeed a convenient method.
Glacial acetic is indeed dirt cheap, though.
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Sedit
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NP, I posted a more detailed version somewhere in one of the endless Glacial Acetic acid threads around here sometime back. The DCM acts as a diluting
agent so that Magnesium Sulfate could readily dry the Acetic acid and it is removed with ease. Also DCM never seemed to have any surface tension
really so Filtering was a breeze unlike some filter jobs. Good thing is your DCM is reusable. And Im sure if someone really wanted they could take the
formed Sodium Sulfate and dry it to reuse that as the drying agent for the next batch.
Long time no see Magpie, good to see people still around, I have not really been around for sometime really.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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ninhydric1
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Sedit I assume any nonpolar solvent would work for the procedure you mentioned?
I don't have a lot a DCM right now but I do have a lot of heptane, which is why I'm asking.
The philosophy of one century is the common sense of the next.
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S.C. Wack
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Yes eventually you have to be careful boiling neutralized vinegar down but at first a rolling boil in a stock pot on the stove is fine. Best to stop
and cool and decant from crystal every now and then before it gets caramelized. IIRC I recrystallized some darker acetate from denatured alcohol,
though carbon or bleach has been recommended.
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Sedit
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Quote: Originally posted by ninhydric1  | Sedit I assume any nonpolar solvent would work for the procedure you mentioned?
I don't have a lot a DCM right now but I do have a lot of heptane, which is why I'm asking. |
I believe so, if you look in one of the GAA threads around here there is a paper about liquid liquid extraction of Acetic acid and I believe Heptane
and Toluene are used as well. I just like how quick and easy it is to use DCM. As long as the boiling points are different enough, GAA is soluble in,
and your solvent is pure enough I see no reason why it would not work.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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happyfooddance
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| Quote: Originally posted by Sedit |
I believe so, if you look in one of the GAA threads around here there is a paper about liquid liquid extraction of Acetic acid and I believe Heptane
and Toluene are used as well. I just like how quick and easy it is to use DCM. As long as the boiling points are different enough, GAA is soluble in,
and your solvent is pure enough I see no reason why it would not work. |
I posted a link on the first page of this thread, to a thread in which Sedit details a few experiments, and yes, there are papers on liquid-liquid
extractions.
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ninhydric1
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I ought to try it then. Getting GAA without distilling acetic acid itself would be relatively simple. I wouldn't have to rely on online sourced GAA.
The philosophy of one century is the common sense of the next.
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symboom
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What about calcium acetate and concentrated sulfuric acid that should also work calcium sulfate percipitates
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Sedit
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| Quote: Originally posted by happyfooddance | | Quote: Originally posted by Sedit |
I believe so, if you look in one of the GAA threads around here there is a paper about liquid liquid extraction of Acetic acid and I believe Heptane
and Toluene are used as well. I just like how quick and easy it is to use DCM. As long as the boiling points are different enough, GAA is soluble in,
and your solvent is pure enough I see no reason why it would not work. |
I posted a link on the first page of this thread, to a thread in which Sedit details a few experiments, and yes, there are papers on liquid-liquid
extractions. |
Yes, here are some more. I also toyed with Oxidation of EtOH using Dilute Nitric acid which I feel has some potential but I never fully perfected it
either. I think Ethyl acetate and NaOH could be a cheep way to Sodium acetate also instead of boiling GALLONS of water which friggin takes forever.
So many ways, just use what works for you.
http://www.sciencemadness.org/talk/viewthread.php?tid=17976
http://www.sciencemadness.org/talk/viewthread.php?tid=4122&a...
http://www.sciencemadness.org/talk/viewthread.php?tid=12898&...
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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