Author Topic: Anhydrous AlCl3  (Read 361 times)

Amphetamine Chemist

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Anhydrous AlCl3
« on: August 11, 2009, 10:55:34 AM »
Now there are many ways to make this necessary and required lewis acid catalyst, the most promising is by passing chlorine gas into molten aluminium, or though you can also pump HCI gas into a solution of aluminium suspended in a particular solvent. I have no experience with the later, the first however, i do plan to engage in sometime soon, when i will be needing some anhydrous AlCl3, what are your methods and experiences in preparing this catalyst, and what way's would you recommend??

The material is of course a very vital part of the reaction between benzene and chloroacetone, known as friedel-crafts, which results in a very yummy amount of P2P, given the simplicity of the reaction. The aluminium chloride is destroyed in the process, but the benzene can easily be recovered and fed back through the reaction. The chloroacetone should react, all of it.

Thanks.
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Sedit

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Re: Anhydrous AlCl3
« Reply #1 on: August 11, 2009, 01:10:19 PM »
There is a recent threed here on AlCl3 that discloses a patent relative to the matter using DMSO to precipitate an AlCl3*DMSO complex which is dehydrated then decomposed back to anhydrous AlCl3 and Dimethylsulfoxide.

Aluminum in a solvent does not produce any AlCl3 at any worth while rate but small scale experiments using Hg activated Aluminum have proven that it may be worth while to scale up and see what results are had.
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Amphetamine Chemist

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Re: Anhydrous AlCl3
« Reply #2 on: August 11, 2009, 01:14:30 PM »
Apologies, i searched this part of the forum, and did not come across any thread on Aluminum Chloride, you may delete this thread if you so desire brother, in the interests of keeping the forum clean. I just though i would start this thread to be sure.

Have you ever had experience in bubbling chlorine gas through molten aluminum? I Am going to carry out this procedure soon, and i will see what results i get. They should be promising.

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- AmphChem.

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Re: Anhydrous AlCl3
« Reply #3 on: August 11, 2009, 01:29:01 PM »
No experiance there as the issue of AlCl3 sublimination seems like it would be a pain to deal with. Fucking with molten Al seems bad enough but to compound it with trying to catch any vapors comming off don't seem like much fun.

No need to delete this threed as its in acquisition and there are more ways then one to aquire AlCl3. The threed in question is more specific to a new method gathered from a patent.



Here is the threed on anhydrous metal salt potential,
http://127.0.0.1/talk/index.php/topic,195.0.html
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Amphetamine Chemist

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Re: Anhydrous AlCl3
« Reply #4 on: August 11, 2009, 01:44:00 PM »
But given enough time to cool, the vapours will form as a solid on the bottom of the receiving flask yeah?? I Mean, if you can contain the reaction for long enough, it should not be a problem. I Know that the aluminium doesn't have to be molten as such, just hot. Red hot, blow torch hot.

I Mean you can always buy aluminium chloride, i should have done that when i had the chance, i'll have to find another supplier if i need some though. If making it doesn't work.

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- AmphChem.

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Re: Anhydrous AlCl3
« Reply #5 on: August 11, 2009, 01:50:38 PM »
AlCl3 has a high vapor pressure and containing it in a flask would be a scary proposition if you ask me that sounds like someone would be asking for an explosion. If you can contain everything in a nice setup I would presume that condensing the vapors in a reciever flask would be more ideal then trying to contain them in the reaction flask. Keep in mind that AlCl3 subliminates very easy and at them temperatures a tube furnace would be ideal. Once you have some AlCl3 I have heard that the solvent method works well with a little bit of AlCl3 added as a catalyst.

I have been toying with the AlCl3 DMSO method but have been having problems precipitating the complex. I may just revive the threed to see what kind of luck V16 is having with that method.
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Amphetamine Chemist

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Re: Anhydrous AlCl3
« Reply #6 on: August 11, 2009, 01:59:08 PM »
Ha Ha, well I'll give it a shot anyway, hopefully i won't kill myself, lol. If i succeed i will post results and corresponding yield. I Hope i succeed anyway. :-\ Maybe some time next week.

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DaMoose

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Re: Anhydrous AlCl3
« Reply #7 on: September 06, 2009, 11:12:19 AM »
i wouldn't try this unless you have a metal shop at your disposal

make a custom crucible reactor of stainless steel with a gas feed in line and
condenser leg that is long enough to air cool to the point where you can connect a vaccum receiver


Ventillator

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Re: Anhydrous AlCl3
« Reply #8 on: February 11, 2010, 01:45:35 PM »
Back on the issue of the manufacture of this vital compound. It is actually something i feel is very important. Furthermore, it is difficult to obtain this compound from chemical suppliers. I like your idea of the steel crucible idea. You see as far as i am aware chemical plants manufacture anhydrous aluminum chloride by indeed bubbling chlorine gas into molten aluminum. This is suppose to create a very high purity product. And the yield seems almost 100%. I Think i'm going to have to manufacture such a device. Chlorine gas and aluminum metal are impossible to control and extremely plentiful. If we can make a device to manufacture this out of stainless steel, then we could potentially have an unlimited supply of anhydrous aluminum chloride. What do you say guys? Willing to give it a try? I Myself will! I Mean, if you can get aluminum metal into a molten state. Then just bubble chlorine through it, and watch the resulting crystals form. And you have nice pure Anhydrous Aluminum chloride crystals.
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lugh

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Re: Anhydrous AlCl3
« Reply #9 on: February 11, 2010, 04:46:16 PM »
You can prepare aluminum chloride from aluminum foil by treating it with chlorine at a high enough temperature to sublime the aluminum chloride  8)
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Ventillator

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Re: Anhydrous AlCl3
« Reply #10 on: February 11, 2010, 05:30:59 PM »
Ahh thanks lugh.. Your a genius.. Have you ever done this?? I Might try it myself very soon.. What would be the best setup? What is the exact temperature the foil needs to be heated to? Red hot heating point? I Mean. It would be difficult to do this in a glass erlenmeyer flask for instance.. yeah? Unless you blow torch the aluminum and drop it in a flask with a metal-fork then seal it and quickly pump chlorine gas into it... Or maybe just a stainless steel chamber. I'm not sure what would be the best setup. But it sounds like a plan stan. I'll have to get it up and running soon. And i'll post pics and results too.. So what do you say. Best chamber construction?

Obviously the construction of the heating mantle would be the most basic thing.. And at that temperature i assume it requires, you'd require a strong heat source.
« Last Edit: February 11, 2010, 05:35:08 PM by Ventillator »
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lugh

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Re: Anhydrous AlCl3
« Reply #11 on: February 11, 2010, 10:51:17 PM »
It seems that the method that was used was to use a wing tipped bunsen burner as the heat source to heat a test tube, but if you want the precise laboratory procedure you're going to have to wait until the information that was posted on the Hive long ago is retrieved again which may take a few days or more   ;)  Once you have a small amount of anhydrous aluminum chloride you can make a lot more using an old patented process, but again it's going to take time to dig up the information you need 8)
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Re: Anhydrous AlCl3
« Reply #12 on: February 12, 2010, 07:49:46 AM »
Some success was noted using a small amount of amalgamated aluminum in solvent with Cl2 feed into it. The experiments where never brought to conclusion but it was determined to warrent further investigation .... which I just never did.
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ausser_betrieb

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Re: Anhydrous AlCl3
« Reply #13 on: February 12, 2010, 01:05:01 PM »
Anyone with Friedels-Craft-Alkylation in mind should read the attatched PDF, they replaced AlCl3 with Graphite Powder, and yields sound good!

Ventillator

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Re: Anhydrous AlCl3
« Reply #14 on: February 12, 2010, 01:42:01 PM »
Hmmmm interesting.. Do you think graphite powder would work as a suitable substitute though for aluminum chloride? In the Friedels-Craft-Alkylation of benzene with chloroacetone? Graphite powder would no doubt be easy to obtain i should assume. There are so many threads here running the ranks for friedel-crafts Alkylation of benzene to P2P

I Should summarize them. I Myself am trying to of course. Once i get my equipment under way and everything else i will attempt these reactions, just have to get a few thing into place first. Namely obtaining the benzene, which is easy, but anyways, all of that kind of stuff you know. I Do plan to make a giant document summarizing all of the friedel-crafts or just generalized Alkylation methods of benzene to P2P. All more or less involving acetone in some way. Beautiful chemistry really, just beautiful.
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lugh

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Re: Anhydrous AlCl3
« Reply #15 on: February 12, 2010, 03:28:43 PM »
The patent:
Chemistry is our Covalent Bond

Baba_McKensey

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Re: Anhydrous AlCl3
« Reply #16 on: February 13, 2010, 05:14:14 PM »

Happyman

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Re: Anhydrous AlCl3
« Reply #17 on: February 14, 2010, 01:23:04 AM »
Oh boy, Pencil lead? And people thought matches were a pain! On that note, what do you think of coal being used? And isn't there a reasonable way to turn AlCl36H2O anhydrous aluminum chloride?
« Last Edit: February 14, 2010, 01:26:24 AM by Happyman »

Vesp

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Re: Anhydrous AlCl3
« Reply #18 on: February 14, 2010, 05:43:57 AM »
Graphite powder can be bought, your you could use carbon welding rods, which could easily be ground down with out any difficulty in a ball mill. Might need to be purified from glues, clay, etc but likley this wouldn't interfere much as I doubt there is very much at all.

What might be interesting is if one could possibly "activate" the graphite by using NaOH or a strong acid? Probably not likely, but activated carbon.. and be made more active in a similiar way -- I am just not sure of the mechanism.
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Re: Anhydrous AlCl3
« Reply #19 on: February 15, 2010, 05:36:26 AM »
Oh boy, Pencil lead? And people thought matches were a pain! On that note, what do you think of coal being used? And isn't there a reasonable way to turn AlCl36H2O anhydrous aluminum chloride?

Coal, No. Pencil lead, doubt it. Graphite has never been a very reactive chemical AFAIK and fine catalytic powder is more thne likely what we are talking about here although I haven't read the paper yet.

As far as a reasonable way to turn the hydrate into AlCl3... well use the fucking search engine ;D V16 and myself toyed with a method using DMSO but i must warn you it churns my stomach just smelling this shit. But the Anhydrous AlCl3 can be precipitated as a complex with DMSO and heated to decompose and sublime the AlCl3 off. I never completed the experiments but it is on my to do list no doubt.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!