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Author: Subject: anhydrous alcl3 with cucl2 ?
Mn2Dc
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[*] posted on 26-11-2017 at 13:13
anhydrous alcl3 with cucl2 ?



i need to know where cupperchloride dissolves in to form anhydrous
alcl3. If i have absolute ethanol and react some aluminium with cucl2 and than remove the ethanol by evaporation wil i have some anhydrous alcl3 ?? is it possible to heat alcl3 in a solvent to make it
anhydrous ??

thx
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clearly_not_atara
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[*] posted on 26-11-2017 at 13:23


Does ethanol react with AlCl3? That should be your first question. Otherwise, reacting solvated CuCl2 with Al seems like a clever idea. Maybe find a nonpolar solvent that will dissolve CuCl2. Wikipedia tells ms CuCl2 is soluble in acetone... Maybe use acetone instead of ethanol?



[Edited on 04-20-1969 by clearly_not_atara]
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Mn2Dc
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biggrin.gif posted on 26-11-2017 at 14:51


yeah i will try acetone and chloroform and dcm
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[*] posted on 27-11-2017 at 06:36


CuCl2 indeed dissolves in acetone, giving a brown solution.
Such solutions are not very stable though. I once kept such a solution around for many days, and when I came back to it the liquid was colorless and there was a thin layer of a white solid at the bottom. I think that the white material is CuCl, but I did not test it.

So, if you do your experiment, the reaction between Al and CuCl2 must be fast, otherwise the reaction between CuCl2 and acetone interferes.

If any AlCl3 is formed, are you sure that AlCl3 does not react with acetone? It is nasty stuff and horrible on storage (almost as nasty as PCl5, PCl3 and POCl3).




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[*] posted on 27-11-2017 at 07:18


I have also dissolved copper (II) chloride in acetone, but I didn't have any luck reacting the solution with aluminum, though I didn't pursue that line of experimentation for very long. Things that might work (and vary in their levels of danger) are heat, iodine, or amalgamation.

I have read that AlCl3 can cause acetone to polymerize at room temperature over the course of a few days, and I have also read that it is very difficult to separate it from acetone.

I tried making AlCl3 reacting hydrogen chloride with aluminum at around 700 C, but although there was some white sublimate and a weight increase, liquid aluminum flowed out of hot zone and contaminated the aluminum chloride. This could probably be avoided most conveniently by putting the aluminum into a boat, but I didn't have one that would fit into the quartz tube at the time, and I grew weary of gassing myself repeatedly with HCl. I have a fume hood now and I'm getting some ground quartz tubes and a PID controller next week and might attempt AlCl3 in a tube furnace again, but on paper, aluminum bromide looks easier to make and purify.

ZnCl2 reacts less vigorously with aluminum than CuCl2, and useful amounts of AlCl3 can be produced with it. And for some reason that I do not fully understand, ZnCl2 is easier to find than AlCl3.




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[*] posted on 27-11-2017 at 07:30


Anhydrous ZnCl2 is quite mild compared with anhydrous AlC3. It can be stored in a normal plastic container (HDPE). AlCl3 on the other hand is very hard on storage. It can only be stored for a,long time in a glass bottle with a teflon-lined cap or in fully sealed glass ampoules. Standard plastic bottles rot away with AlCl3 in it. They become blistered in a few weeks of storage and leak a lot of HCl and on the outside they feel wet.

If I open my bottle of AlCl3, then a big cloud of HCl-fumes escape from it, when I unscrew its cap. The bottle also is pressurized of HCl gas.




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[*] posted on 27-11-2017 at 07:35


That makes sense. I have always stored AlCl3 in a glass media bottle with a PTFE-lined cap, but I've never had more than 10 grams of it at a time. I didn't notice any fumes, but it did degrade noticeably in storage.



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[*] posted on 27-11-2017 at 11:53


@Mn2Dc, you'd better try the chemplayer's experiment at You Tube, since he used aluminium powder and anhydrous zinc chloride to make anhydrous aluminium cloride with 36% yield:

https://www.youtube.com/watch?v=g7sS69fQMsk

I think Chemplayer lost a substancial amount of the product when it fumes out the reciever flask while it's condensing. The yield could be better. May be he should have used a longer tube that went inside the reciever flask until the bottom.
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[*] posted on 27-11-2017 at 12:08


Quote: Originally posted by Mn2Dc  
yeah i will try acetone and chloroform and dcm

Cool !

I'll await with breath abated until the photos of those experiments are posted.




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[*] posted on 27-11-2017 at 12:41


Quote: Originally posted by aga  
Quote: Originally posted by Mn2Dc  
yeah i will try acetone and chloroform and dcm

Cool !

I'll await with breath abated until the photos of those experiments are posted.


I won't.
I will post a reminder that those solvents can react with aluminium (potentially, dangerously so)
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[*] posted on 27-11-2017 at 19:15


@ Mn2Dc - Have you seen these threads..........? Much information has been posted here already

Search for posts by Blogfast25, and others

"Chlorothermal reactions (chloride thermites) for preparing AlCl3 and KAlCl4"
https://www.sciencemadness.org/talk/viewthread.php?tid=30150...

"Anhydrous Aluminum Chloride prepration"
https://www.sciencemadness.org/whisper/viewthread.php?tid=14...



/CJ






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[*] posted on 28-11-2017 at 07:40


The hard part of doing this reaction in the liquid phase is finding a solvent that will dissolve AlCl3 without reacting with it, or with aluminum metal. Those are some tough criteria to meet, and the only solvent I had that met them was diethyl ether. I'm pretty sure I got something by reacting an aluminum/galinstan alloy with anhydrous HCl in diethyl ether, but I had no way of quantifying yields at the time.

edit: Best source I could find regarding AlCl3 solubility:

http://chemister.ru/Database/properties-en.php?dbid=1&id=353

Note that this does not specify whether the solvent reacts with aluminum metal.

[Edited on 11/28/17 by Melgar]




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[*] posted on 28-11-2017 at 11:47


Nitrobenzene might be a winner. I know that sodium can be electrolyzed from NaAlCl4 in nitrobenzene so Al is probably safe. I would definitely start on a small scale, though.



[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 28-11-2017 at 18:49


Quote: Originally posted by clearly_not_atara  
Nitrobenzene might be a winner. I know that sodium can be electrolyzed from NaAlCl4 in nitrobenzene so Al is probably safe. I would definitely start on a small scale, though.

I'd expect the aluminum to reduce the nitro group, producing aniline, no? It can reduce aliphatic nitro groups easily enough, and aromatic nitro groups are even easier to reduce.

[Edited on 11/29/17 by Melgar]




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[*] posted on 28-11-2017 at 19:38


I absorbed that information from BromicAcid's post several years ago. I was unable to find the reference he cited, although I did find out that Chem. Zentr. is Chemisches Zentralblatt and that Mem. Inst. Chem. Acad. Sci. Ukrain, SSSR is Memoirs of the Institute of Chemistry published by the Ukrainian Academy of Sciences.

https://www.sciencemadness.org/talk/viewthread.php?tid=2105#...

I saw some other papers citing Plotnikov's other work related to electrodeposition of metals from organic solvents, including this:

http://www.sciencedirect.com/science/article/pii/03764583809...

I think that nitrobenzene may not be so easy to reduce in the absence of protons. With protons it is probably reduced quickly by aluminum. The 1980 paper by Galova may help us here.

[Edited on 29-11-2017 by clearly_not_atara]

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[Edited on 04-20-1969 by clearly_not_atara]
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