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sonogashira
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Anhydrous AlCl3??
Hey everyone.
I want to make anhydrous aluminum chloride to use as a catalyst in a reaction i am working on.
I have found a procedure which requires passing dry HCl over heated aluminum powder....
http://designer-drugs.com/pte/12.162.180.114/dcd/chemistry/a...
Does anyone have any experience of this? Are there any problems which may occur with this method? Would Cl2 work better than HCl?
I was also wondering whether powdering kitchen foil would be a suitable source for the Al powder.. in other words, how pure is aluminum foil?... do
they use some sort of alloy or is it pure enough for this reaction.
Any help will be very much appreciated...
[Edited on 11-9-2006 by sonogashira]
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12AX7
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Foil is something like 98% pure, the remainder is mostly iron and silicon IIRC.
If you wanted to be sure, you could sublimate the AlCl3 I suppose.
Tim
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unionised
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FeCl3 and SiCl4 are reasonable substitues for AlCl3 in many cases (at least if you are just using it as a catalyst). Purification might be more
trouble than it's worth.
Cl2 and HCl both work and they are both nasty to work with. The reaction with HCl gives rise to H2 which complicates things because it's flammable.
What experience do you have with this sort of reaction?
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Maja
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I faced with that kind of problem ,because of AlCl3.. I just bought 100gr of Anhydrous AlCl3 and then made much more myself by bubbling HCl gas thru
inert solvent where Al powder was suspended. You need to initiate reaction with small amount of AlCl3, otherwise it won't work. Now I would make small
amount of AlCl3 myself. I don't know for what you will use that, but you can substitute it with FeCl3 or SiCl4 as unionised said. Thanks.
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sonogashira
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Do you not think that the product will be reasonably pure? Perhaps if i found a better source of Al than Al foil would that solve the purity
concerns?.... Do you see the problem arising from the contaminants in the aluminum or does the process itself lead to an impure product?...
The flammability issue is not a huge concern, i will take suitable precautions.
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unionised
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The product will be pretty pure and the impurities probably won't matter much for most things.
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Nick F
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Does the procedure not involve sublimation itself? If so, that would purify it. I haven't read the procedure, because I'm at a friend's house and he
might not want designer-drugs.com on his computer....
But as unionised said, iron and silicon impurities shouldn't matter.
I'd prefer to use HCl than Cl2. Hydrogen isn't a problem to deal with, HCl is a bit less nasty, and it's easier to make anhydrous.
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sonogashira
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Thanks for your help.... Will give it a try and report back.
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sonogashira
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"Does the procedure not involve sublimation itself?"
It basically involves passing a stream of dry HCl over heated Al powder in a tube.
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hodges
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One idea which I have never heard proposed before but seems like it might work would be to react hexachloroethane (C2Cl6, available as a pyrotechnic
supply) with aluminum powder in a sealed container. This should be self-sustaining once started; experiment starting with a small amount of reactants
on the size of the aluminum particles to get a rate that is not too fast.
You will end up with some carbon as well but might not be a problem; depending on your reaction you could filter it off later.
Hodges
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Nicodem
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| Quote: | Originally posted by hodges
One idea which I have never heard proposed before but seems like it might work would be to react hexachloroethane (C2Cl6, available as a pyrotechnic
supply) with aluminum powder in a sealed container. This should be self-sustaining once started; experiment starting with a small amount of reactants
on the size of the aluminum particles to get a rate that is not too fast.
You will end up with some carbon as well but might not be a problem; depending on your reaction you could filter it off later.
Hodges |
https://sciencemadness.org/talk/viewthread.php?tid=1542#pid3...
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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matei
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In "Vogel's Practical Organic Chemistry" you can find the procedure for obtaining anhydrous AlCl3 by sublimation. This should be sufficiently dry for
catalytic purposes.
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sonogashira
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Thanks a lot matei!!
I have the 5th edition... I had a little look but couldn't find it. Could you give me a page number (or say what section it is under if you have a
different edition).. Many thanks for your help!!
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ethan_c
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| Quote: | Originally posted by unionised
The product will be pretty pure and the impurities probably won't matter much for most things. |
Look at the website he is sourcing from. Although I guess if you're dumb enough to be making drugs either to sell or for your own consumption,
impurities are probably the least of your worries.
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sonogashira
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wtf??
Who said anything about making drugs... If you can find another anhydrous AlCl3 synthesis on the internet i would be very interested..
Please don't be so judgemental...
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ethan_c
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| Quote: | Originally posted by sonogashira
wtf??
Who said anything about making drugs... If you can find another anhydrous AlCl3 synthesis on the internet i would be very interested..
Please don't be so judgemental... |
You're right, a google search did turn that particular procedure up immediately. However, it took 35 seconds fliping pages to find out… that
synthesis is copied word for word from Brauer. The internet can be helpful, but I would personally much prefer actual literature to a site like that.
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Nicodem
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| Quote: | Originally posted by ethan_c
… that synthesis is copied word for word from Brauer. The internet can be helpful, but I would personally much prefer actual literature to a site
like that. |
All Rhodium pages have references to where the procedure was taken from and this one is no exception (check the end of the page). Among the hundreds
pages, there are only a couple of errors which can be easily spotted by checking the original papers.
So, I do agree that one should take the information from the original literature, but more because there is often some additional information there
that can be of use. Otherwise, the Rhodium's archive is pretty much trustworthy for the part that is the transcription from academic literature as
well as most (but not all) of the part that originated from amateur experimenters.
I know several friends that work in academic laboratories that sometimes source references and procedures from that incredibly rich archive. Not
surprisingly, given that it takes a couple of seconds to check the net when compared to going to the library for a reference search and then looking
up for the papers.
PS: What has AlCl3 to do with drugs?
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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unionised
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Whether the chemicals he hopes to produce are drugs or not I presume that, at some stage, there would be an isolation procedure that would remove the
product from the leftover catalyst. I'd have to think about it to come up with a procedure such that SiCl4 or FeCl3 would be carried into the organic
product but AlCl3 would be removed.
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sonogashira
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Any idea how i would do this?.. what common solvents is AlCl3 soluble or insoluble in?
(by the way i am most certainly not making any drugs... i just happened to find that procedure using google.. not my fault if it happens to have
"designer drugs" as a webpage!!)
Also, am i right in thinking that AlCl3 can be hydrolysed to Al(OH)3 which would be safe to ingest anyway?
(by the way matei, i am still interested in more info on that vogel reference if you have it... i haven't been able to find it as yet....)
[Edited on 17-9-2006 by sonogashira]
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12AX7
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Yes, but HCl isn't exactly safe. Plus lots of heat (see also CaCl2 MSDS). You get AlCl3 + 6H2O = AlCl3.6H2O followed by AlCl3 + 3H2O = Al(OH)3 +
3HCl (plus H2O of hydration).
Tim
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The_Davster
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http://www.sciencemadness.org/library/books/vogel_practical_...
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sonogashira
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Thanks a lot rogue chemist thats fantastic!!
Maybe i'm being slow but i cant find the AlCl3 sublimation procedure in this edition either... I've looked in the contents, index, and preparing
inorganic solids but still cant find it....
Thanks for the link.. It seems even more useful than the 5th edition for my needs...
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matei
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Sonogashira,
The purification procedure for AlCl3 is in Vogel's 5th Ed. on page 416.
I'm pretty sure AlCl3 is soluble in aromatic hydrocarbons (like benzene or toluene).
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sonogashira
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Many thanks!!
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sonogashira
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Does anyone know what solvents i can use with anhydrous aluminum chloride. i have seen a paper where they used 1,2-dichloroethane; would
dichloromethane be ok, or would it react with it? Out of interest does anyone know why it doesn't react with 1,2-dichloroethane?
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