Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1  2
Author: Subject: How to make relatively pure AlCl3
ScienceSquirrel
International Hazard
*****




Posts: 1863
Registered: 18-6-2008
Location: Brittany
Member Is Offline

Mood: Dogs are pets but cats are little furry humans with four feet and self determination! :(

[*] posted on 17-10-2011 at 08:22


Aliphatic halogenated solvents and reactive metals are always a bad idea.
Chloroform explodes when mixed with quite a few eg aluminium,
magnesium, sodium, lithium, potassium, iron and zinc! :(
View user's profile View All Posts By User
Vogelzang
Banned





Posts: 662
Registered: 26-4-2008
Member Is Offline

Mood: No Mood

[*] posted on 23-10-2011 at 06:20


Has anyone here tried aluminum in the Friedel-Crafts reaction? See attachment.



Attachment: JCE1989p0176Friedel-Crafts-Al.pdf (1.4MB)
This file has been downloaded 1028 times

View user's profile View All Posts By User
Sedit
International Hazard
*****




Posts: 1939
Registered: 23-11-2008
Member Is Offline

Mood: Manic Expressive

[*] posted on 23-10-2011 at 09:12


Over at The Vespiary some time back a member I believe it was V16 posted a means of extracting Anhydrous AlCl3 from an (aq) solution by using DMSO which would precipitate as a complex with the AlCl3 and would release under mild heating, anhydrous AlCl3. I once started to attempt the procedure however the complete disdain I have for the smell of heated DMSO prevented me from going any further.




Knowledge is useless to useless people...

"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story before."~Maynard James Keenan
View user's profile View All Posts By User
Lambda-Eyde
International Hazard
*****




Posts: 856
Registered: 20-11-2008
Location: Norway
Member Is Offline

Mood: Cleaved

[*] posted on 23-10-2011 at 09:25


Quote: Originally posted by Sedit  
Over at The Vespiary some time back a member I believe it was V16 posted a means of extracting Anhydrous AlCl3 from an (aq) solution by using DMSO which would precipitate as a complex with the AlCl3 and would release under mild heating, anhydrous AlCl3. I once started to attempt the procedure however the complete disdain I have for the smell of heated DMSO prevented me from going any further.


For those interested in the procedure, see the attached reference.

Attachment: 3471250 PREPARATION OF ANHYDROUS INORGANIC METAL HALIDES.pdf (127kB)
This file has been downloaded 1579 times





This just in: 95,5 % of the world population lives outside the USA
You should really listen to ABBA
Please drop by our IRC channel: #sciencemadness @ irc.efnet.org
View user's profile View All Posts By User
smaerd
International Hazard
*****




Posts: 1262
Registered: 23-1-2010
Member Is Offline

Mood: hmm...

[*] posted on 24-10-2011 at 07:32


If no one else has confirmed that this works I will conduct tests replacing ethanol with methanol in the very near future.

[Edited on 24-10-2011 by smaerd]




View user's profile View All Posts By User
Vogelzang
Banned





Posts: 662
Registered: 26-4-2008
Member Is Offline

Mood: No Mood

[*] posted on 24-10-2011 at 13:18


Here's an interesting AlCl3 synthesis. I wonder if it would work with tetrachloroethylene (dry cleaning fluid). It looks like it could be scaled up.

http://www.sciencemadness.org/scipics/AlCl3prep1.gif

http://www.sciencemadness.org/scipics/AlCl3prep2.gif
View user's profile View All Posts By User
Vogelzang
Banned





Posts: 662
Registered: 26-4-2008
Member Is Offline

Mood: No Mood

[*] posted on 24-10-2011 at 13:49


Aluminum and bromine can react at room temperature. How about making and using aluminum tribromide in place of the trichloride?

http://en.wikipedia.org/wiki/Aluminium_bromide

http://pubs.acs.org/doi/abs/10.1021/j150498a017
View user's profile View All Posts By User
Adas
International Hazard
*****




Posts: 711
Registered: 21-9-2011
Location: Slovakia
Member Is Offline

Mood: Sensitive to shock and friction

[*] posted on 25-10-2011 at 04:18


Thanks, guys. But I think that dissociation is not a problem. So, what do you think? How pure is Al foil? 98% Al?
View user's profile Visit user's homepage View All Posts By User
Sedit
International Hazard
*****




Posts: 1939
Registered: 23-11-2008
Member Is Offline

Mood: Manic Expressive

[*] posted on 25-10-2011 at 07:56


Quote: Originally posted by Vogelzang  
Here's an interesting AlCl3 synthesis. I wonder if it would work with tetrachloroethylene (dry cleaning fluid). It looks like it could be scaled up.

http://www.sciencemadness.org/scipics/AlCl3prep1.gif

http://www.sciencemadness.org/scipics/AlCl3prep2.gif



I ran simple test a while back on the feasibility of this reaction and IIRC someone either here or over at The vespiary again attempted this without very good results. I see no reason to use Tetrachloroethylene when the Dichloromethane they use is so available.

My results showed that when the DCM contained Cl2 it would be yellow... Placing Al into this solution did next to nothing and the yellow persisted overnight, however when a small amount of amalgumated Al was used the yellow color quickly faded.

See the problem with the solvent synthesis of AlCl3 seems to be that AlCl3 is needed as a catalyst for the reaction. This problem CAN be avoided using a small amount of Hg to get the ball rolling. I hope someone can make it work but I have yet to hear great results from the solvent methods of generating AlCl3.

If you fear Hg then perhaps Iodine would work to get things going.





Knowledge is useless to useless people...

"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story before."~Maynard James Keenan
View user's profile View All Posts By User
SHADYCHASE54
Hazard to Others
***




Posts: 148
Registered: 16-12-2010
Location: CaNaDay!
Member Is Offline

Mood: No Mood

[*] posted on 1-11-2011 at 18:19


I was just wondering if refluxing aluminium chloride hydrate with a chlorinating agent like thionyl chloride would dehydrate it into an anhydrous state? If SOCl2 converts carboxylic acids to their respective chloride wouln't the same hold true in this case?
View user's profile View All Posts By User
Adas
International Hazard
*****




Posts: 711
Registered: 21-9-2011
Location: Slovakia
Member Is Offline

Mood: Sensitive to shock and friction

[*] posted on 2-11-2011 at 09:40


Quote: Originally posted by SHADYCHASE54  
I was just wondering if refluxing aluminium chloride hydrate with a chlorinating agent like thionyl chloride would dehydrate it into an anhydrous state? If SOCl2 converts carboxylic acids to their respective chloride wouln't the same hold true in this case?


I think it's a good idea. Not impossible.
View user's profile Visit user's homepage View All Posts By User
thanos thanatos
Harmless
*




Posts: 23
Registered: 8-9-2011
Member Is Offline

Mood: No Mood

[*] posted on 3-11-2011 at 18:23


Quote: Originally posted by SHADYCHASE54  
I was just wondering if refluxing aluminium chloride hydrate with a chlorinating agent like thionyl chloride would dehydrate it into an anhydrous state? If SOCl2 converts carboxylic acids to their respective chloride wouln't the same hold true in this case?


Yes, you can use SOCl2 to produce anhydrous AlCl3, but I suspect if someone needs to produce anhydrous AlCl3 because they cannot purchase it (and it is not a listed chemical), then I think in that case it is even more likely that that same person would not be able to buy thionyl chloride (or PCl3 or PCl5, for that matter), as it is a watched chemical and more expensive than anhydrous AlCl3.
View user's profile View All Posts By User
Nicodem
Super Moderator
*******




Posts: 4230
Registered: 28-12-2004
Member Is Offline

Mood: No Mood

[*] posted on 4-11-2011 at 11:25


Quote: Originally posted by Sedit  
I ran simple test a while back on the feasibility of this reaction and IIRC someone either here or over at The vespiary again attempted this without very good results. I see no reason to use Tetrachloroethylene when the Dichloromethane they use is so available.

Sedit, the referred reaction is something totally different from what you describe. It is apparently an SN1 reaction between AlI<sub>3</sub> and CH<sub>2</sub>Cl<sub>2</sub>. Its peculiarity is in that the aluminium iodide acts at the same time as the acid catalyst and as the source of the iodide while dichloromethane acts as a reaction substrate and the solvent. AlI<sub>3</sub> forms by the oxidation of aluminium with iodine. (This type of nucleophilic substitution on dichloromethane was already mentioned in the 5th paragraph of this post.)




…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!
View user's profile View All Posts By User
radiance88
Hazard to Self
**




Posts: 64
Registered: 18-12-2014
Location: underground volcano fortress
Member Is Offline

Mood: a little less evil than usual

[*] posted on 18-3-2015 at 03:52


I recently just did this experiment because it's probably the easiest to get ahold of materials for and I'm a complete noob at all this. So I placed Al foil into HCl.. What remained after the considerably vigorous emission of gas (which i assume is Hydrogen), was just metallic looking precipitate, very similar in color to the aluminum foil.

I assume that this isn't AlCl3? If so... then what was the dark gray precipitate? If there was AlCl3, was it suspended in solution? What exactly am I looking at in the beaker then?
View user's profile View All Posts By User
Texium
Administrator
********




Posts: 3802
Registered: 11-1-2014
Location: Salt Lake City
Member Is Offline

Mood: Triturated

[*] posted on 18-3-2015 at 08:41


The gray stuff is excess aluminum, and possibly some impurities in the foil. The aluminum chloride is in solution as hydrated aluminum ions and chloride ions. If you're going for anhydrous AlCl3 you're barking up the wrong tree, if you just wanted some hydrated AlCl3, filter and crystallize. Don't boil it down, or it will decompose giving off HCl and leaving you with aluminum hydroxide/oxide.



Come check out the Official Sciencemadness Wiki
They're not really active right now, but here's my YouTube channel and my blog.
View user's profile Visit user's homepage View All Posts By User
Rhodanide
National Hazard
****




Posts: 348
Registered: 23-7-2015
Location: The 80s
Member Is Offline

Mood: That retro aesthetic

[*] posted on 5-5-2016 at 05:38


One great way is to heat Anh. Zinc Chloride with aluminum powder and sort of "Distilling" the subliming AlCl3 into a very cold (and closed) container. The YouTube channel "Chem Player" has an awesome video on this.
Cheers!
~T
View user's profile View All Posts By User
gdflp
Super Moderator
*******




Posts: 1320
Registered: 14-2-2014
Location: NY, USA
Member Is Offline

Mood: Staring at code

[*] posted on 5-5-2016 at 06:29


That method originated from SciMad http://www.sciencemadness.org/talk/viewthread.php?tid=30150#...



View user's profile View All Posts By User
chemplayer...
Hazard to Others
***




Posts: 191
Registered: 25-4-2016
Location: Away from the secret island
Member Is Offline

Mood: No Mood

[*] posted on 5-5-2016 at 07:32


It was someone on this site who posted the original blog posting we found. Can't remember which user though. We just kept playing with it until we had an acceptable yield.

Only caveat is that the product works great for some reactions (e.g. Friedel Crafts acylation it's superb), but for others we're getting substandard results (vanillin demethylation). It's quite possible there's some subliming ZnCl2 passed over in the product and this has a detrimental effect on some uses. The reason we suspect this is because we've controlled all variables in some reactions and they're still way below literature yield - the AlCl3 source is the only thing left to blame.




Watch some vintage ChemPlayer: https://www.bitchute.com/channel/chemplayer/
View user's profile View All Posts By User
blogfast25
Thought-provoking Teacher
*****




Posts: 10340
Registered: 3-2-2008
Location: Old Blighty
Member Is Offline

Mood: No Mood

[*] posted on 5-5-2016 at 07:56


Quote: Originally posted by chemplayer...  
It was someone on this site who posted the original blog posting we found. Can't remember which user though. We just kept playing with it until we had an acceptable yield.

Only caveat is that the product works great for some reactions (e.g. Friedel Crafts acylation it's superb), but for others we're getting substandard results (vanillin demethylation). It's quite possible there's some subliming ZnCl2 passed over in the product and this has a detrimental effect on some uses. The reason we suspect this is because we've controlled all variables in some reactions and they're still way below literature yield - the AlCl3 source is the only thing left to blame.


That user was me. I first published it here, then on my blog (where you found it).

Re. your purity point, the only way to 'blame' the AlCl3 conclusively is by comparing it to a commercial grade.

Re-sublimation may be the cure here. I've a feeling that most catalytic grade commercial AlCl3 has been re-sublimated too.

[Edited on 5-5-2016 by blogfast25]




View user's profile Visit user's homepage View All Posts By User
JJay
International Hazard
*****




Posts: 3440
Registered: 15-10-2015
Member Is Offline


[*] posted on 5-5-2016 at 08:19


I made some aluminum chloride in a quartz tube by gassing aluminum with hydrogen chloride, but there was still a lot of unreacted aluminum left in it. I think that putting the aluminum into a boat and gassing with a larger quantity of HCl would have produced better results.



View user's profile View All Posts By User
 Pages:  1  2

  Go To Top