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Author: Subject: Making Anhydrous Aluminium Chloride
EliasExperiments
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[*] posted on 2-10-2020 at 20:53
Making Anhydrous Aluminium Chloride


Hi,
I have tried to make some anhydrous aluminium chloride from the elements, by reacting chlorine gas with aluminium foil. You can see my process in this video:

https://youtu.be/ksIXZjbSOkQ

My yield was only 36 % however. Does anybody know how you can improve upon what I did?
Also has anybody tried this with HCl instead of Cl2 and got it to work better?
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Maurice VD 37
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[*] posted on 3-10-2020 at 01:42


Thank you for the trouble you had in making this video. It was quite impressive. It reminds my own experiments, when I made the same synthesis, a long time ago. I am not surprised about your poor yield. I even find it relatively high. When I made the same synthesis in my school lab, my yield was even lower. The majority of the aluminum chloride went away with the smoke.

But I had a fundamental remark. In the first part, concentrated HCl solution hd to react with aluminium metal. The reaction is violent, but it starts after a couple of minutes, because the protective layer of alumina Al2O3 has first to be destroyed, before aluminum metal can react. Anyway, with this reaction Al + conc. HCl, you will never obtain anhydrous AlCl3. You will only get AlCl3ยท6H2O, or [Al(H2O)6]Cl3, which is fundamentally different from AlCl3. AlCl3 is covalent, easily vaporized, and produces Al2Cl6 in the gaseous state. [Al(H2O)6]Cl3 is ionic and cannot be vaporized at all. If heated it is decomposed into HCl and Al(OH)3. [Al(H2O)6]Cl3 cannot be transformed into anhydrous AlCl3, except by adding thionyl chloride SOCl2. The inverse reaction is easy : AlCl3 reacts easily with water to produce [Al(H2O)6]Cl3, but this operation occurs in two steps. First AlCl3 reacts with water to produce Al(OH)3 and gaseous HCl. Then the gaseous HCl gets dissolved into water, and the HCl solution reacts with Al(OH)3 to produce [Al(H2O)6]Cl3 or its ions [Al(H2O)6]3+ and 3 Cl-.
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[*] posted on 3-10-2020 at 03:18


I suspect the idea of using alcohol to get anhydrous AlCl3 is impossible.
I think alcohol will react with AlCl3
It certainly looked like it reacted when you mixed them.


[Edited on 3-10-20 by unionised]
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Tsjerk
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[*] posted on 3-10-2020 at 03:51


I think it would help if you insulate the reaction vessel tightly with aluminium foil so more AlCl3 comes over and use way more chlorine. As you see from the wash bottle a lot of chlorine is passed unreacted. You could use cooling on the collection vessel if you think AlCl3 escapes.

You could also use more aluminium foil, this would increase the surface, catching more chlorine. The yield percentage would go down, but who cares? Both the hypochlorite and the metal are cheap.

Maybe in this reaction it is more appropriate to calculate the yield based on chlorine produced anyway, as in that case you know how efficient your setup was... I would stuff the reaction vessel with aluminium I think.
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EliasExperiments
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[*] posted on 3-10-2020 at 07:12


Thank you all for the feedback!
I am just really confused how a patent can get published with such a high ranking on google, even though it is more or less obvious that it can't work.

Of course when I use more reagents I get more AlCl3. :D But the limiting factor is more the size of the reaction vessel and my time. So the question is how to make the reaction more efficient.
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Tsjerk
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[*] posted on 3-10-2020 at 08:59


I think the reaction becomes more efficient when you stuff the reaction vessel with aluminum foil, not all aluminum will react but more chlorine will.

What patent? The ranking on Google depends on how well it corresponds to your search input, that has nothing to do with how trustworthy it is.

[Edited on 3-10-2020 by Tsjerk]
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[*] posted on 3-10-2020 at 11:35


Process for manufacturing anhydrous aluminum chloride
US1818839A

Anhydrous aluminum-sulfate + (anhy.) zinc-chloride

zinc-sulfate regeneration with fused sodium chloride/calcium chloride

CN103708518B
aluminum chloride hexahydrate + thionyl chloride

CN103803622B
A kind of by the method for Aluminum Chloride Hexahydrate Dehydration for Aluminum chloride anhydrous

The present invention discloses a kind of by the method for Aluminum Chloride Hexahydrate Dehydration for Aluminum chloride anhydrous, comprising: Aluminum Chloride Hexahydrate drying is sloughed most of crystal water by (1); (2) dried aluminum chloride is dissolved in alcohol the alcoholic solution configuring aluminum chloride, adopts the method for vacuum distilling to slough moisture in the alcoholic solution of aluminum chloride; (3) the aluminum chloride alcoholic solution after dehydration and ammonia react crystallization generate AlCl 3nH 3; (4) wash, filter, dry AlCl 3nH 3crystal, and dried heating crystals decomposition Study of Deamination is obtained Aluminum chloride anhydrous;

CN1683247A
dehydration with isopropanol

Anhydrous aluminum chloride by Oliver C. Ralston.
https://catalog.hathitrust.org/Record/006866955

Preparation of anhydrous aluminum chloride by Robert L. de Beauchamp
https://catalog.hathitrust.org/Record/006866195

aluminum + iron-chloride
Rev. Adv. Mater. Sci. 28 (2011) 40-43 Jei-Pil Wang, CHEMICAL SYNTHESIS OF ALUMINUM CHLORIDE (AlCl3)BY COST-EFFECTIVE REDUCTION PROCESS

Non of these procedures are really otc but it worth a try.
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