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Author: Subject: Anhydrous Aluminum Chloride prepration
Chainhit222
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thumbup.gif posted on 26-7-2010 at 15:22
Anhydrous Aluminum Chloride prepration


I just made anhydrous aluminum chloride. You will need:

-aluminum foil
-a barby
-chlorine or hcl gas source
-a piece of metal pipe (i used copper)
-some way to connect it all together (i afro rigged it)

my setup was:
1) flask connected to a addition funnel (ground glass 24/40)
2) a hose (i used tygon, vinyl is fine) leading from the hose barb on the flask to a ground glass vacuum take off thing wrapped in electrical tape and wedged into a copper tube filled with aluminum foil from the food store laid across the barby
3) a liebig condenser cooled with room temp water with one end wrapped in electrical tape wedged into the end of the pipe

I preheated the barby as high as it would go (seems to be like 450c) (take off the flame guard if it has one) and then laid the pipe on it. At this point the pipe was being flooded with argon gas so the aluminum would not oxidize (i dont think it was necessary, but why not if you got a tank). After I was confident that the pipe and reactants were hot enough I switched the hose from argon to the hcl gas generator and turned it on.

AlCl3 began to sublime and condense in the liebig. Once I ran out of hcl gas I took the liebig off and put it over a container. I then took a clean plastic glassware brush and pushed/twisted it through the liebig, which caused the alcl3 to fall out into my container. Id recommend a large chlorine gas generator, I ran out of chlorine so I just got a few grams of AlCl3 which is very slightly contaminated with burnt electrical tape.

If you actually wanna do this, I would recommend adding a drying tube for the chlorine or HCl gas, and using some kind of heat resistant material (maybe muffler tape?) to make a connection between your glassware and the copper pipe.

http://img807.imageshack.us/img807/241/thugfurnace.jpg (picture of setup)
http://www.youtube.com/watch?v=bpi7cX5d0iw (youtube video of reaction)

Why not use a quarts tube you ask? Because I cannot afford a quarts tube or a tube furnace. I have 12$ in my wallet.

[Edited on 26-7-2010 by Chainhit222]

[Edited on 26-7-2010 by Chainhit222]




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[*] posted on 26-7-2010 at 15:34


Why does it not form CuCl2?



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Chainhit222
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[*] posted on 26-7-2010 at 15:43


Quote: Originally posted by 12AX7  
Why does it not form CuCl2?


Because its subliming away, the melting point of CuCl2 is 500c, so I suppose its plausible that there could be a bit of cucl2 contamination. The AlCl3 sublimes at 200c, way before the CuCl2 even melts.

Not to mention it would turn water blue if it was contaminated with CuCl2 (and it did not seem to do so in my test). Not to mention you can vacuum sublime the AlCl3 to purify it if you want to :)

Additionally you can easily use a thin steel pipe (like say a broom stick) instead.



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copper does not react with HCl :P
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[Edited on 26-7-2010 by Chainhit222]




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[*] posted on 27-7-2010 at 13:48


Ok, so if nothing else, you're doing thermal seperation. Like distilling TiCl4 from FeCl3 and etc. That works, and as a bonus, aluminum reacts with CuCl2 and most others, so if you have an excess of metal, you should get excellent results.

Does steel passivate to hot HCl? FeCl3 is more volatile, though still not as much as AlCl3. Not that that's a big deal, most of the time AlCl3 and FeCl3 can be substituted as Lewis acids.

If used as a long-term apparatus, I wonder if there would be any erosion of the pipe (steel or copper). Meh, can probably get more than a few pounds of AlCl3 out of it by then.

Tim




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Chainhit222
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[*] posted on 27-7-2010 at 14:22


Quote: Originally posted by 12AX7  
Ok, so if nothing else, you're doing thermal seperation. Like distilling TiCl4 from FeCl3 and etc. That works, and as a bonus, aluminum reacts with CuCl2 and most others, so if you have an excess of metal, you should get excellent results.

Does steel passivate to hot HCl? FeCl3 is more volatile, though still not as much as AlCl3. Not that that's a big deal, most of the time AlCl3 and FeCl3 can be substituted as Lewis acids.

If used as a long-term apparatus, I wonder if there would be any erosion of the pipe (steel or copper). Meh, can probably get more than a few pounds of AlCl3 out of it by then.

Tim


im gonna try this with a piece of steel fence post in a little bit, gonna use tightly wrapped aluminum foil to make the glass fit. I will put a bit of vac grease on the end which will not be hot too.

[Edited on 27-7-2010 by Chainhit222]




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[*] posted on 27-7-2010 at 14:42


Yars could just be usin' a piece o' glass if contamination be an issue. Doesn't even need to be ground.

Crack open the yellow pages, or your proximal equivalent, and look for neon signs. Then call them all and ask if they could sell you a bit of borosilicate tubing.

In terms of demethylations, it won't matter much if you have contaminant FeCl3 in there, as it'll act as a Lewis acid as well, as me valve lovin' salt be pointin' out already.

But, if you be lookin' at me own thread on a DCM based method, yar be seein' some horrible brown shit be coatin' me commercial acid. Iron contamination in yar AlCl3 be givin' her a yellow tint, which be similar to slightly hydrated AlCl3. Hydration o' the acid yields B/L acids, which be alterin' the properties o' the Lewis acid with regards to some things, so the pure white colour be a good assurance of yar startin' reagents and something yar should be aftar.... Ar....

I still be unsure of what that brown on me commercial grade be and suspect it be some form of Iron compound. And she be causin' havoc with potential tar producin' results, as it be lookin' identical.

[Edited on 27-7-2010 by peach]




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[*] posted on 27-7-2010 at 16:52


fence post = mad fecl3 contamination, its no good. The way to go is copper pipe + hcl generated from h2so4/nacl or h2so4/cacl2

if you use copper pipe then the product is fairly pure. I am going to resublime it as soon as i drill this stopper. I recommend a 400mm liebig to cool, the 20cm aint doing a good enough job, i was running around my yard with a leaf blower in a gas mask shooing clouds of alcl3 away so my neighbors would not get suspicious if the cloud traveled into their yard :x
I hope they did not see me


btw peach, what is your aluminum from, is it pyrotechnic aluminum by any chance? If so, that stuff is coated to prevent reactivity.



wow, vacuum sublimation is such fucking bullshit. I never imagined it would be such a long boring inefficient process, my god.

[Edited on 28-7-2010 by Chainhit222]




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[*] posted on 27-7-2010 at 17:52


You guys are crazy

I have a mental image of chainhit's Thug Furnace smoking away and him running around frantically with a gas mask and leaf blower.

I always thought the hard part would be to get the sublimed fumes to condense properly and into a container.




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[*] posted on 27-7-2010 at 18:03


Im just gonna condense it into a frederichs condenser and then wash it out with anhydrous ethanol or something, the current situation is unacceptable.

I got 8 grams of crude off white shit at the moment. I am wondering if i can get very pure stuff if I take a new long copper tube, wash all the oxides out with aq HCl so its mad clean, use aluminum foil end plugs (which work well). I just have the condenser problem now, I wish I had a 600mm liebig.

Protip: get ready to stand there with a long wire and unclog that shit every couple of minutes. I also had to flush out the AlCl3 by pumping argon at around 4-5 psi through the thing, otherwise it would just chill in the pipe.


This is defiantly doable on a better scale, I just need to work out the kinks in the operation. For all my work so far I got 8grams, but I noticed I had quite severe losses due to inefficient cooling. Next run tommorow or middle of the night tonight im gonna daisy chain the liebig and the frederichs condenser, then when its done just pour some anhydrous solvent into it after setting it into a flask and dissolve it out of the condensers instead of scraping, though, this poses the problem of clogs. Maybe I can put a clansien conector between the frederichs and liebig and leave it capped, but uncap it once in a while so I can poke at the clog with a steel wire...

[Edited on 28-7-2010 by Chainhit222]

[Edited on 28-7-2010 by Chainhit222]




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[*] posted on 27-7-2010 at 19:03


everybody except me already knew that a "barby" is a gas-fired barbecue oven? where have I been? I must however protest the substitution of the plural of an British/American volume unit for the conmon term for pure silica glass. Having got my little barns in, why do this, AlCl3 is cheap. It does need to be pure for most purposes ....



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[*] posted on 27-7-2010 at 19:17


Quote: Originally posted by chemrox  
everybody except me already knew that a "barby" is a gas-fired barbecue oven? where have I been? I must however protest the substitution of the plural of an British/American volume unit for the conmon term for pure silica glass. Having got my little barns in, why do this, AlCl3 is cheap. It does need to be pure for most purposes ....


I don't know of a source of anhydrous AlCl3 that will sell to a house in the suburbs.

Why can I not just recrystallize AlCl3 in a solvent? Why must it be sublimed?

[Edited on 28-7-2010 by Chainhit222]




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[*] posted on 28-7-2010 at 03:08


Wow that's a really good setup, even if the yields aren't the best who cares, it costs a few dollars to set up.
I'm definitely giving that a shot once we get a new gas cylinder for the BBQ :D
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[*] posted on 28-7-2010 at 04:49


Quote: Originally posted by Chainhit222  
i was running around my yard with a leaf blower in a gas mask shooing clouds of alcl3 away so my neighbors would not get suspicious if the cloud traveled into their yard :x
I hope they did not see me
[Edited on 28-7-2010 by Chainhit222]


If you see my DCM method for this, that's pretty much what I ended up doing with the results when the neoprene was in contact with the acid and solvent. The smoking was stupid. I was standing in my undercrackers on the lawn trying to wash huge plumes of persistent white smoke out of the air before the fire brigade arrived, for about two or three hours.

I don't know what grade the aluminium is, other than that it's aluminised. They make it by spraying molten aluminium through a nozzle to make a fog which is then cooled and solidified as it is in a spray dryer. They break the particles up by playing ultrasonic vibrations through it as it leaves the nozzle to form micronic aluminium droplets; like a cold humidifier.

The aluminium you might be thinking of is German blackhead / Indian black. Spheres distribute heat / pressure etc over their surface better than any other shape. So spherical, atomic aluminium doesn't ignite so well at low temperatures. The pyrotechnic grades are made by putting it through rollers between pieces of paper, to squash it flat. That flattens it to square like shapes with sharp edges, where heat will concentrate to raise the temperature and cause ignition. The paper is burnt off afterwards, leaving a carbon coating. Hence it's name 'black'.

It took me a good amount of google searching to find out that precise reasoning.

I would suggest, if you have a glass wash head, you try my solvent method again. I'll be trying it again.

It's the neoprene that caused the problem, it was working fine before that, and I'll try it again once I have my glass back.

The reason I'm trying it over the hot method is, like you say, it'll solidify and clump up in the glass. Since it doesn't melt and only sublimes at 100C+, you can't simply pump warm water through the condenser.

The only thing I can suggest is hooking it up to the fridge pump. You could stick the receiver bend into the flask and extend it with some tubing, then fill the flask with some broken glass and put the flask in some ice water. The AlCl3 may make it through to the flask, where it'll solidify and wait for you to dissolve it afterwards.

But, as I say, this is why the glass DCM method would be so nice, because it'd be extremely pure and precipitates as a fine deposit, see; those pictures of the amber bottle. That is AlCl3, whatever BlogGimp wishes to think.

Quote: Originally posted by chemrox  
everybody except me already knew that a "barby" is a gas-fired barbecue oven? where have I been? I must however protest the substitution of the plural of an British/American volume unit for the conmon term for pure silica glass. Having got my little barns in, why do this, AlCl3 is cheap. It does need to be pure for most purposes ....


Jumpin' jelly beans! You didn't realize a barby was a BBQ. Shit.... :P

As chainhit says, the anhydrous salt is not at all easily available without accounts.

I agree that FeCl3 etc contaminated Lewis acid will function for a lot of things. But, when it's being used for experimentals where I don't know what colours or changes to look for, they do not help at all. E.g. My commcercial grade acid stained my solvents of choice so dark brown I couldn't see through them with it held up to a light. That instantly increases the chances of incorrectly identifying something as intractable tar.

As I've said on other forums, I can order a huge number of things from genuine suppliers. I wouldn't mind if they spontaneously phoned me or asked to visit if they were bothered about an order, but I hate the idea of them closing the road off, getting their suits out and smashing the door down at 3am because I'm a member of the public and they think I'm churning out drugs or bombs.

It's also part of the fun, seeing what I can make at home better than the lab suppliers. It's not all that hard to surpass what gets passed off at CP grade, and it can be done for not a lot of effort and similar or lower price.

The AlCl3 depositing in my amber bottle was pure white. The CP grade was yellow, after weeks of rinsing the near opaque brown shit off it. I'd make it at home even if it was more expensive than the CP grade to be sure of what I had.

If we just ordered what we liked form suppliers, this forum wouldn't exist.

[Edited on 28-7-2010 by peach]




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[*] posted on 28-7-2010 at 04:57


I'm curious about the temperature seemingly required for this reaction. AlCl3 sublimes around 180C. Why push the tube to 450C? Does it actually need to be that hot for the reaction to proceed to completion, or are you just making it that hot so that the vapor reaches your condenser without condensing prematurely? 200C would be more easily managed in some respects - for example, you could use PTFE in places where a hotter setup would destroy it, and it seems like vapors would be less likely to escape your condenser.
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[*] posted on 28-7-2010 at 05:15


I don't know what the precise temperature is for the hot, solvent free HCl(g) + Al method, but just that the result sublimes at 180C does not mean the compound will form at 180C; e.g. NaOH takes hundreds of degrees to melt, with the extracted sodium melting more than three times below that.

I'd prefer to see more people trying the cold method personally. If it reaches a similar efficiency, why cook the equipment and have to put up with clogs over fine precipitates.




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[*] posted on 28-7-2010 at 05:35


When I had the flame guard on the bbq (it would only reach 300c or so) there was no reaction between HCl and Al foil. It seems as if the temperature has to be around 400c before it begins to react



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[*] posted on 29-7-2010 at 15:23


I managed to make a bit more today:
http://img202.imageshack.us/img202/9938/hitthatshit.jpg

This stuff is much cleaner (copper pipe + hcl w/drying tube and aluminum foil plugs). It seems to have a slight discoloration still, not perfect white. Vacuum sublimation is my only hope D:




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[*] posted on 30-7-2010 at 04:25


You've got way too much angry bird contamination thar pirate!

If it's tinted limey green, that'll be moisture or iron contamination (more so the iron if it has a yellowy tint). The iron could be from traces in the pipe or the aluminium source.

If it's moisture, you didn't mention what the drying tube was full of, using 98% sulphuric may help with that.

If it's brown, that may be iron again, but I don't know why it'd be brown. Leaving it to soak in just enough DCM to cover it for hours or days will help remove that; rapid rinsing with excess doesn't seem to work anywhere near as well. It's not particularly soluble in DCM either.

Take care with your tapers, as I've had glass to glass seize when DCM + AlCl3 has come into contact with them for prolonged periods. To the point that it needed smashing open; no solvent, heating, tapping or reagent treatment would get it open again (I spent three weeks gently teasing it to no avail).

When you store it, use a screw top bottle and wrap the threads with PTFE tape. If they're not wrapped, it can escape; my sealed commercial bottle rotted it's own label without me even breaking the seal, so taping the threads is a good idea.

I'm just doing some AlI3 demethylation work now and making a gigantic video blog of the process. Seems to be behaving finally. You get a mention in the video and I'll probably give this a go with some copper myself, or a rogue pipette you'll see in the video. I'm going to try with a DeWalt hot air gun and one of those pipe sweating nozzles. I don't have a thermometer that'll read to 400C, but I do have one to 300C. So I'll be able to investigate how linear the temperature rise is on the infinitely adjustable dial and then work out roughly where the temperatures are above that based on the dial position. That may allow me to find a more exact temperature.

400C is getting close to the maximum recommended for borosilicate, so copper pipe may actually be a good choice if you're not going for quartz. Particularly if it's going on the barby, might go over that temperature and the glass is ground.

[Edited on 30-7-2010 by peach]




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[*] posted on 30-7-2010 at 06:27


Anhydrous CuCl2 is brown. Damp FeCl3 likewise. FeCl2 hydrate *would* be green but I would not expect it to be able to grab the water before the AlCl3 did.
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[*] posted on 30-7-2010 at 12:54


I seem to have alot of hydrate in my product. I vacuum sublimed some, and the left behind stuff is not particularly reactive with water. I might just have to do the iodine method :(

It must be reacting with the atmosphere during production. I wonder if pumping a mixture of argon and hcl would help. There is also some FeCl3 in my product (nice yellow color), I assume this means the pipe is impure.

Any idea what else is in aluminum foil or copper pipe? What kind of contaminants am I dealing with?

[Edited on 30-7-2010 by Chainhit222]




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[*] posted on 30-7-2010 at 15:19


Copper pipe is about 99.9% or better, it's very pure stuff.

Aluminum foil is not particularly pure, perhaps 97%. The main impurities are Si and Fe.

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[*] posted on 30-7-2010 at 16:39


Would a slight contamination of iron chloride (from the foil) effect the gatterman reaction? Specifically 1,4-dimethoxybenzene to 2,5 dimethoxybenzaldehyde (benzene with alcl3 + hcn/hcl)

[Edited on 31-7-2010 by Chainhit222]




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[*] posted on 13-8-2010 at 04:50


In Organic Reactions v5 (from the library section) it says "An industrial grade of aluminum chloride may be employed as catalyst. Its chief impurity is ferric chloride.....There are no statements in the literature which report any advantage in using highly purified aluminum chloride."
Although that is talking about the method that uses CO not HCN but is there really that much of a difference between the two? Is there any advantage to HCN? I'd be much more comfortable using CO.
What size copper pipe did you use? 3/4" or 1"?
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[*] posted on 13-8-2010 at 05:59


Some arenes can be formylated with a Gatterman using zinc cyanide and gassing with HCl, thus avoiding the need to gas with either CO or HCN. There will of course be some HCN byproduct, but with good ventilation I think it is safer than gassing with HCN + CO. (Isn't everything?)
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[*] posted on 13-8-2010 at 13:53


I am trying the 1,4-dmb with glyoxylic acid route for now, but I want to do gatterman too and compare them. Aparrantly it works much better with 2-bromo-1,4-dmb, but I don't really want the bromine atom there :(

My pipe is 1 inch ID.
I suggest you use something thicker then a 24/40 liebig condenser to condense the AlCl3, it clogs up WAY too easily. I was thinking a 300mm glass 24/40 tube, then put a liebig on the end of that, hopefully it would be a more even distribution and not clog so much. Then you could simply use a pipe cleaning brush to get your AlCl3 out. When a clog forms its pretty hard to unclog...

[Edited on 13-8-2010 by Chainhit222]




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