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peach
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@Spong
"Someone at some point has decided the general public has no use for paint thinners."
That made me laugh. 
If you can squeeze 100g out in one run, I'd be happy with that. That's a perfectly usable quantity and you may find it more effort to
spend weeks / months working out a continuous system than you would to just open it up, pour some more in, purge and rerun it. You don't even need a
cylinder of inert gas if you're starting the tube from cold, just displace the atmosphere with HCl(g) and warm the tube up.
Look at the solvent problem this way, if you ever need a BBQ on a rainy day, it's not going to be very hard to get the shed going. 
20L isn't too bad, just don't drop your cigarettes in the bottles when you're done. And, if the shed is in the sun and it's hot there, those bottles
may get fairly warm and fill the shed with vapours, so some ventilation would be an idea.
@Jig pipe
Sell it on eBay. 
[Edited on 22-9-2010 by peach]
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spong
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Quote: Originally posted by peach  |
Look at the solvent problem this way, if you ever need a BBQ on a rainy day, it's not going to be very hard to get the shed going.
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Hehe, or if I ever run out of petrol
I got some turnings today, I'm a big fan of metal recycling businesses, 300g Al, 650g Mg blocks, 200g Cu and 200g steel for $10
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peach
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That's a great haul of magnesium for $10 compared to what it'd normally cost.
You can find documents online for getting those up to really high purities as well if that's yar thing.
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spong
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Should it be ok for things like gringards or formylations? There's a layer of green backing on each of the pieces I'll have to remove.
I was thinking of making some magnalium too.
The Al turnings aren't as dense as I would have liked, they're almost similar to the foil, they should still work ok provided I wash them and pack the
tube pretty tight.
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noone
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Is it possible to make the hexa hydrate anhy?
AlCl3 H2O6 to ALCl3 ? How maybe oven @ 400 for an hr? dessicator w/H2SO4? Dean Stark trap? just wondering why all the trouble you guys are going
through to make it when you can buy it very cheap?
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DJF90
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You think if it was that easy we would have done it by now right... So what does that infer to you?
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noone
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I would think not, but some people cant get things because of restrictions in their country or just like chemistry & also like a challenge or
being selfsufficient. That's what I was getting at. Anyway I found sublimation would be the best way actually & I tried to edit my post before
anyone saw it ,but was to late. Oh well
btw That infers to me you are quite the smartass DJF90
Thanks for the warm welcom to your board!!!
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starman
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| Quote: Originally posted by spong | Yeah I've already bought 20l of toluene and methanol because that's the only reasonable way to get them. The shed is a big enough fire hazard without
another 20L of flammable liquids Getting acetone from a chemical supplier is
actually cheaper than from the hardware store *facepalm*
I think it's mainly Australia. Someone at some point has decided the general public has no use for paint thinners. |
20Lt methanol?Is it of reasonable purity.Care to share your source?
Chemistry- The journey from the end of physics to the beginning of life.(starman)
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DJF90
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noone - I'm almost certain it is not as simple as you suggest - drying at high temperature requires a brisk flow of HCl(g) to carry away the water
vapour and ensure the material remains as the trichloride. If you read through the other threads here on AlCl3 production (theres quite a few now!)
then you'll be much more informed about the subject.
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spirocycle
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| Quote: Originally posted by starman | | Quote: Originally posted by spong | Yeah I've already bought 20l of toluene and methanol because that's the only reasonable way to get them. The shed is a big enough fire hazard without
another 20L of flammable liquids Getting acetone from a chemical supplier is
actually cheaper than from the hardware store *facepalm*
I think it's mainly Australia. Someone at some point has decided the general public has no use for paint thinners. |
20Lt methanol?Is it of reasonable purity.Care to share your source? |
i can get it for $35/5gals at VP racing
http://www.vpracingfuels.com/
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peach
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DJF is quite the smartass, but for good reasons, e.g. he's right and you're wrong. He is also quite smart.
You can't dry things like that with heat alone, or any other common drying method. Drying with sulphuric won't work, neither will doing it under
vacuum. A Dean-Stark hasn't got a snowballs chance in hell of working. Neither will sublimation, that's for purifying an already dry Lewis acid of
other metal halides. AlCl3 decomposes as the water tries to leave.
Lots of the harder Lewis acids do it.
And it's quite likely the form you're looking at is the hexahydrate, which absolutely will not function as anhydrous forms of it will; the water
destroys the Lewis acid potential, which is quite important for a lot of work. Added to that, moisture in the solvents (those not dried over sodium)
or absorbed from the air (and it will visibly suck it up from the air and emit clouds of hydrogen chloride) will begin rapidly contaminating the Lewis
acid with a Bronsted Lowry acid, and the two are quite different. Having the latter around for your Lewis acid work can turn the flask into tar, or at
least what's not supposed to be in there. E.g. you'll have halogens adding themselves across bonds and all sorts of nuncing around going on. AlCl3 is
particularly good at it, as it is an aggressive Lewis acid. The iodides are less bothered about it. The fluorides are so bothered they need cooling
with a dry ice bath to stop them overheating and ripping things to bits.
It's quite ironic that for many BR acids, you want some water around to disassociate them. You don't want any water
for most Lewis acid work; although, I'm sure there are some Lewis reactions that do, or will be found to, benefit from being tinted with a little
water to catalyze them.
Everyday oxides also function as Lewis acids, but only very weakly. And the strength is important for Lewis acids. A hard acid will attack a hard base
site but not be all that interested in a weak site, and vice versa. So a weak base will attack a weak acid site first, even if there's a hard site
present. There is also a spectrum within the hard / soft definitions. The definitions are based on the ionization state of the metal, but the finer
spectrum is based on the halides, their electro-negativity and so on. E.g. AlI3 is most definitely not as harsh as AlCl3. But they're both in the hard
way of looking at things.
You can get softer Lewis acids to react with harder sites, and vice versa, by subjecting the substrate to things like microwaves, to shift the charges
around in the molecule. Extra halogens sticking off the opposite end usually help with that.
BR acids add hydrogens. Lewis acids take electrons.
To give you a more usable reply, you'd need to dry it under a stream of sulphuric dried, carbon filtered hydrogen chloride gas, so the water can be
swept out but not with the chlorides at the same time. That's a possibility I'm considering. Producing the hydrate with hydrochloRIC acid and then
drying under hydrogen chloRIDE, as it works at lower temperatures.
You have to meet hard, anhydrous Lewis acids in person to appreciate the difference with your senses.
I can assure you, the effort is for a reason.
As for a warm welcome, shit... you've just got to get used to that on SM. I got the same response. You WILL get a mouthful back if you're being an
idiot. And probably quite a lot if someone disagrees. But... if you want to talk to people who actually know what they're doing, it's about the only
place to do it online. Just put up with it for a while. If you're posting rubbish, it'll never end. If you post something novel, it will.
[Edited on 16-10-2010 by peach]
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spong
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| Quote: Originally posted by starman | | Quote: Originally posted by spong | Yeah I've already bought 20l of toluene and methanol because that's the only reasonable way to get them. The shed is a big enough fire hazard without
another 20L of flammable liquids Getting acetone from a chemical supplier is
actually cheaper than from the hardware store *facepalm*
I think it's mainly Australia. Someone at some point has decided the general public has no use for paint thinners. |
20Lt methanol?Is it of reasonable purity.Care to share your source? |
http://www.oilchem.com.au/products/alcohols
That's just the alcohols page, they have such a great range of chemicals but they're in 20L minimums, it would be great if some Australians could
arrange some kind of a group buy for them, with 10 or 20 people in on it we could get a great deal on some awesome solvents and reagents, I've been
looking for benzyl alcohol for ages and they have it...in 20L drums 
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DJF90
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Thanks peach. You're quite smart too...
Anyway my point was, that I'm fairly certain you've covered all of that in one of the other threads (why can't we just have one thread dedicated to
AlCl3, as opposed to having to wade through the current 3-4+?), but it was nice of you to go into detail again here. Other than the dehydration at
temperature with HCl(g), the method utilising DMSO and other Lewis bases (R3N, R3P, R3P=O, etc) also looks decent, although you'll need a decent
vacuum pump to get it to work I suspect. The patent is provided in one of the other threads, but I can attach it if necessary. Have you tried it? If
you're lacking the DMSO I know where you can find that (no, not at toolstation lol).
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peach
Bon Vivant
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I just was at toolstation. Having sanded the floor from it's previous nicotine amber stain to pristine white, it's now pitch black, momentarily.
I have a litre of DMSO, but have been so busy I haven't had time to do a lot of chemistry fun. I also need to pick up a new receiver bend before any
distilling is happening.
Sorry for not getting back to your PM. I did read it but, as with the experiments, got carried away with tidying up and kept forgetting.
Yes, the repetition is bad.
I don't mind typing the Lewis acid stuff out once or twice, since they're something people usually don't deal with, don't behave as you might expect
and have some quirky traits that aren't discussed all that much in what I've read - so I had to gain it first hand, and experience the defunct results
with my pocket money.
AlCl3, the discussions of it here, are a prime candidate for compression. This has already been discussed as well. The BBQ method, we have photos of,
I'll have a go at forming it with hydrochloric then drying it, and perhaps the DMSO idea as well. Once that's done, the threads all need a battering
down into one in the pre-publications section.
[Edited on 17-10-2010 by peach]
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redfox87
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I was curious if this method could be used to make anhydrous AlCl3.
http://www.youtube.com/watch?v=F4IC_B9i4Sg
I thought if the chlorine gas was piped in through some CaCl2 that it would be free of moisture, and if the receiving flask and foil was heated that
there would be little moisture to worry about.
Is this a possibility? It seems a lot easier from my perspective then the DMSO method.
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spong
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It would work but recovering the AlCl3 would be a pain, it's going to be coating whatever flask you did it in and mixed with Al2O3 ash left over from
the foil. Plus a lot of it would escape, you need quite a bit of cold glass for it to sublime onto, if the entire flask was heated then it's going to
go straight out the top and end up as fumes once it hits the moist air.
If it did work you could perhaps vacuum sublime it straight from the flask into a receiver to purify it but it's hard to get a good yield from the
sublimation. Another option could be dissolving it in Et2O in which it is supposedly quite soluble in, you could swirl some dry Et2O in the flask and
filter it to remove the unreacted Al and Al2O3 then distill it off.
Once my exams are done I'll have more time than I know what to do with so I'll work on getting the process to run more efficiently, I'll also make
some ether to see how that works for purifying it.
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neptunium
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has anyone bubbled Cl2 in carbon tetrachloride with aluminum foil in it?
and distilled off the CCl4?
i wanna try that
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