nannah
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Purification of OTC solvents.
Hi, its me again with yet another question. 
I saw a clip on youtube of one guy that purified store bought acetone by distillation. I am interested in doing the same thing. My local hardware
store have a bunch of different paint thinners, I havent checked them all, but there are two different paint thinners that contain toluene and the
other xylene.
I am thinking of buying a liter of each and try to purify those by vacuum distillation after i bought a pump.
EtOH from mash, and EtOAc from nail polish remover are two other OTC solvents that i want to purify.
Those two have (together with acetone) have a low boiling point and toluene has a bp of 111°C, and Xylene 138,5°C.
Vacuum distillation should be applied right?
What should i keep in mind if i choose to pursue this?
Where are MeOH found (or made)? I know its used in racing fuel but thats too damn expensive.
It seems to be very useful for recrystallisations.
If anybody know of a compiled text, or can recommend a book on the subject i would be super excited.
Thanks in advance. I know that you will straighten out my question marks like you always do (almost always).
I hope that in the future i will be able to do the same and pass on my knowledge, and my experiences to beginners.
/Nannah.
[Edited on 29-9-2014 by nannah]
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macckone
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Distilling OTC solvents is not a simple question.
There are a bunch of threads on this.
Each thread is usually about a particular solvent.
There is also a lot of information on the web.
Paint shop toluene, xylene and acetone are usually
pretty pure (99% or so). Other stuff is going
to require a different process due to mixtures.
Also make sure you are using good equipment and
take appropriate precautions as the distillation of
flammable liquids can result in flames of the vigorous kind.
Ie. it probably won't be a true explosion but the difference
may not matter much on the way to the hospital.
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chemrox
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And don't bother with mixtures or alcohol water mixtures unless they are better than 90% alcohol. Look up the solvent in one of the chemical
purification manuals and follow a procedure. For example methanol can be treated with molecular sieves, Na, Mg & I2, etc. Depends on how pure you
need it. Hardware store toluene has proved quite pure in the past but I distill it anyway. Special still heads are used for solvent recycling..
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
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aga
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If you got a Mixed paint thinners, one thing i learned on SM is that you can add about the same volume of water, and shake really hard.
Leave to settle (a minute or two) and the Toluene floats to the top.
Separate, repeat 5 or 6 times.
Leave to stand for a while for the bulk of the remaining water to settle out. Separate.
Then chuck in some lumps of CaO to mop up the trace water, and filter.
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Metacelsus
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Paint thinners don't only have toluene; they can have many aliphatic hydrocarbons, and sometimes DCM. All these are insoluble in water.
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aga
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Not a bad start though eh ?
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macckone
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In most paint places you can buy industrial grade toluene, xylene and acetone in cans.
Toluene is a bit less available than xylene.
Most of the paint strippers are a witches brew of solvents and emulsifiers.
Paint thinners vary but are often just acetone or ethyl acetate.
You really have to look at an msds to know what you are dealing with
and even then you get things like 30% proprietary emulsifier.
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Brain&Force
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I've seem high quality toluene, xylene, acetone, and mineral oil at Ace hardware stores in the US. Toluene seems to only come in large sizes.
At the end of the day, simulating atoms doesn't beat working with the real things...
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macckone
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As for a source of methanol, winter grade windshield washer fluid is usually a high concentration of methanol. Treatments to remove water from a gas
tank are also usually methanol. Finally it is sometimes sold at paint supply stores in cans. These cans will be labelled methanol.
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nannah
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Thanks to all you guys for helping me. I aporeciate it.
Im sorry that i started yet another thread on the subject. I just wanted to be thorough in my research, so it wont happen any accidents. I hope its
ok.
I have been checking out a solvent stillhead at Laboy.com. I should rather use a stillhead thats designed for that purpose, but until the day i have
the money to get one then i have to do without.
The one i bought today has Toluene, 1-butanol and acetone in it. Could it be a problem separating them? The toluene and the 1-butanol is pretty close
in bp, but with a little patience it will probably work great.
Another thing, the acetone i looked at say just "acetone" and nothing else. Do you think is it pure then, ?
Thanks again.
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Amos
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The hardware store acetone I come by is impressively pure considering the price. As far as I can tell from distillation, there's no water in it, it's
flawlessly transparent, and it smells great.
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Oxirane
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Acetone is usually supplied very pure and I've never found any impurities in them. Xylene and toluene, on the other hand, may contain substantial
portions of other chemicals, like acetone. Since they're nearly insoluble in water, it is sometimes handy to wash these with large amount of water,
separate and distill. I never used vacuum to distill toluene and xylene, not even speaking of acetone which comes over very nicely even with hot water
bath. Acetone is one of my favorite solvents. 
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aga
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I got a 1 litre bottle of acetone from a store and assumed it polluted.
It is Horrible to distill, mostly because Acetone Loves to spill itself everywhere.
It is so 'thin' (v. low viscosity) that it runs down the edge of any container, no matter what angle you hold it at.
At the end of the distillation i had ~100% acetone in the RBF, AND the receiving flask.
The 10% or so that Spilt just evaporated, and was lost.
It appears (to me) that Acetone is an OTC chemical that is too hard to 'pollute' so nobody bothers, they just sell 100% Acetone.
[Edited on 1-10-2014 by aga]
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aga
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Where on the planet are you nannah ?
Perhaps someone can direct you to pure acetone supply by buying the Right brand etc.
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nannah
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Oxirane: Acetone is starting to become my favorite too, when reading this about how pure it is already at the hardware store. I will ofcourse try try
to purify it first to see if its anything else in it.
Aga: I live in the northern parts of europe.
Molecular sieves sounds interesting. Which ones would you advice me to get? There is a whole bunch of em on ebay.
Thanks guys.
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nannah
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From the little i have read about sieves the 3A is used for drying EtOH and MeOH, and the 4A is not suitable for that.
Are the 3A suitable for toluene/xylene?
Its nice that they are re-usable too.
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nannah
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The paint thinner i have contains a mix of toluene, 1-butanol and acetone. I am wondering if the 1-butanol could be extracted with water? It is an
alcohol, but its maybe different? Then you could distill off the acetone from the toluene/acetone mixture.
And then dry the toluene.
What do you guys think, how does it sound?
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macckone
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1-butanol is only slightly soluble in water unlike lower alcohols.
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Little_Ghost_again
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Found a strange one.
In the supermarket is a wood floor cleaner (I will find brand later), it only lists one ingredient...... It says contains d limonene ! the thing is
its really cheap! £2.10 for a litre. I will grab a bottle and see if I can find what else is in it.
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plante1999
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D-limonene can be used to reduce material in conjunction with palladium on carbon. Nitro groupes, double bonds etc. It is called catalytic transfert
hydrogenation
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aga
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Pyrolise a chunk of old rubber tyre ...
Not as cheap, and will certainly not smell as good, but much more fun.
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Little_Ghost_again
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Quote: Originally posted by aga  |
Pyrolise a chunk of old rubber tyre ...
Not as cheap, and will certainly not smell as good, but much more fun. |
Funny enough mum has a tyre in the boot of her car she dosnt use much
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aga
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NOOOOOO !
That's there in case of emergencies !
... and YES, she will miss a 4 inch chunk of it ...
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nannah
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Wikipedia say that it is very soluable in acetone. Maybe it can be separated together with the acetone in the mixture?
All of the components in this mixture is disirable to me.
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