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Sedit
International Hazard
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Don't know how useful they might be to anyone here because they both seem out of my league(allthough the last one seems doable to some extent) but I
thought I would post them anyway because they are different then the methods I hear about the most.
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(c) removing all soluble iron chloride from said liquor to obtain a substantially iron free, aluminum hloride-containing pregnant liquor;
(d) crystallizing said pregnant liquor to produce a separable slurry of phosphorous or magnesium-containing aluminum hexahydrate (ACH) crystals;
(e) heating said phosphorous or magnesium-containing ACH crystals from said slurry to a temperature of about 200° C. to 450° C. to produce partially
calcined ACH (PCACH);
(f) chlorinating said PCACH in the presence of chlorine and a reductant to produce said anhydrous aluminum chloride; |
Reference:http://www.patentstorm.us/patents/4465566/claims.html
US Patent 4096234 - Production of anhydrous aluminum chloride from clay using catalyst and recycling of silicon chloride
| Quote: | This invention relates to the production of aluminum chloride from clay. More particularly, this invention relates to an improved process for the
chlorination of clays containing silicon oxide as well as aluminum oxide whereby the aluminum oxideis chlorinated while the chlorination of the
silicon oxide is suppressed.
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Reference: http://www.patentstorm.us/patents/4096234/description.html
@Len I have been meaning to ask you but never remebered to do so. You called the DMSO method "economically silly" but I fail to see how it is so. The
DMSO is recovered and is only used to complexe with the AlCl3 long enough to dehydrate it and the two are seperated with heat to recover the
dehydrated AlCl3 and DMSO. Since the only thing that leaves the reaction is H2O I don't see how this is a non economical means to dry your AlCl3.
Am I missing something?
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
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kmno4
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Kirk-Othmer Encyclopedia of Chemical Technology - for those who want to know how AlCl3 is produced idustrially. Brauer etc. - for laboratory methods.
Patents - is somebody likes stories in kind of "making hexogen or opium from sugar, water, DMSO, muriatic acid and simple kitchen devices". Sometimes
it works, but only at times.
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Bolt
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Quote: Originally posted by len1  | Ah yes, I was rather thinking that two. Two possibilities come to mind
1) The patent is obscure - so those passing HCl over Al dont know better
2) It doesnt work and the patent author is a lier - my concern is the Al sulphate getting covered by insoluble CaSO4 stopping reaction.
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Which patent is this?
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Sedit
International Hazard
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The one posted on Hyperlab with the link supplied by Vogelzang,
Its ironic because I was thinking about something along the same lines using Aluminum, H2SO4 and NaCl to attempt to produce it when I first heard of
the DMSO patant but starting with the sulfate on this one seems like a better way to go.
Ill link the one PDF here,
Patent US1818839:
Process for manufacturing anhydrous aluminum chloride
Attachment: Aluminum Chloride.pdf (140kB)
This file has been downloaded 881 times
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
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SunlightChemist
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Thanks guys, from what i hear, it would seem that making it by simply passing chlorine gas through hot/molten aluminium is the easiest way to go. I'll
do that me thinks.
- T.
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not_important
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Using molten aluminum is overkill, hot solid aluminium will ignite in chlorine, running Cl2 into molten Al should be reasonably exciting.
Simply take aluminium in the form of chips, turnings, or chopped wire, washing it free from grease with acetone, then fill most of the length of a
borosilicate tube a cm or two in diameter with the Al, using borosilicate glass wool or the similar high temperature wool used in kilns. Mount the
tube horizontally, arrange to heat it, except for the end section (which should be empty), to about 300 C. One end should exit through a stopper into
a wide mouth bottle, which will be cooled with an air blast, and with a second tube in the stopper for removing excess HCl gas. The other end is
connected to a generator of dry HCl, and has an additional input to pass in dry CO2 or N2.
Turn on the N2 or CO2, pass it through the apparatus for 5 or 10 minutes, then turn on the heat to raise the Al containing section of the tube to ~300
C, and again wait a few minutes. Then start passing dry HCl through the tube. Watch out for AlCl3 condensing inside the exit end of the tube, apply
heat using a burner or hot air gun to sublimate any solid forming, forcing it into the condensing bottle.
It should be noted that the gases leaving the condensing bottle via the exit tube will contain H2 and HCl, so must be properly vented or if you are a
clever lad, washed and the H2 collected.
Turn off the HCl feed when there is only a few cm of unreacted Al metal remaining, while providing a flow of dry N2 or CO2. This section serves as a
trap for alloying metals in the aluminium that have volatile chlorides, most of their chlorides will react with the Al metal and be reduced back to
their original metallic form.
Keep the dry N2 flowing, turn off the heaters, and allow the apparatus to cool somewhat. While still warm remove the condensing bottle with its load
of AlCl3, and tightly stopper it.
There's an older version of this in Thorp's Inorganic Chemical Preparations, which is out of copyright and can be downloaded from the
Internet Archive or Google Books.
[Edited on 11-8-2009 by not_important]
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Eclectic
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I have seen a patent involving the purification of AlCl3 by distilling the AlCl3:Et2O adduct. I'm having some trouble finding it as http://gb.espacenet.com seems to be having issues. Ether solutions maybe a more convenient way to store and use AlCl3.
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bbartlog
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As I recently prepared about 500g of cupric chloride (CuCl2), I wondered whether it would be possible to produce anhydrous AlCl3 via reaction of
aluminum with anhydrous CuCl2. There are of course various chlorides that could theoretically by reduced by aluminum, but CuCl2 is fairly easy both to
prepare and to dry. If this approach were practical it would be one way to avoid the use of gaseous chlorine and/or HCl.
The difference in heats of formation (706kJ/mol for AlCl3 versus 358kJ/mol for CuCl2) suggests that the reaction would be exothermic but not to my
mind dangerously so. My thought would be to add some aluminum foil and powdered CuCl2 to one glass vessel, connect this by glass tube to a receiver,
and put the entire arrangement in an oven with the receiver set in water to keep its temperature down around 100C. The oven being possibly necessary
to keep the AlCl3 from condensing before it reaches the receiver.
The first question that occurred to me was whether I should use a mole ratio of 3:2 (CuCl2 to Al) or 3:1. While the aluminum should be able to fully
reduce the copper, it occurs to me that the reaction might not proceed to completion if all that is left is aluminum coated with copper alongside CuCl
and AlCl3, so a 3:1 mole ratio is probably better.
On doing further searching, I came across this paper: http://www.dtic.mil/cgi-bin/GetTRDoc?AD=AD277616&Locatio...
It's not directly applicable to my interest, but it has some interesting data on a mixture of AlCl3 and CuCl (which I will surely end up with at some
point during this reaction). Notably, the vapor pressure of the mixed AlCl3/CuCl is higher than expected (see table 5 on page 16). This at first seems
advantageous (the AlCl3 should vaporize at a lower temperature), but on further reflection it sounds like there may be a minimum boiling azeotrope of
these two chloride salts. In which case this approach would result in some mixture of CuCl and AlCl3 rather than pure AlCl3 condensing in the
receiver.
Can anyone point me to further information on possible azeotropes of AlCl3 and CuCl, or for that matter just some reading on azeotropes of chloride
salts generally? I have found numerous references to eutectics but almost nothing on azeotropes. Also, besides this possible problem of separating
CuCl and AlCl3, can anyone point out problems in the proposed approach for preparing AlCl3?
[Edited on 22-3-2010 by bbartlog]
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Polverone
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Some years ago I was able to make a self-sustaining exothermic mixture that burned with visible flame from anhydrous CuCl2 rolled inside aluminum
foil. This may be because I had a mixture of oxygen-containing species along with the chloride after simply heating CuCl2 to dryness. Still, I would
be cautious not to underestimate the potential exotherm.
PGP Key and corresponding e-mail address
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bbartlog
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Interesting. I suspect that oxygen was involved, that is, the chloride reaction served mainly to continuously strip the passivation from the aluminum,
and most of the energy came from the formation of oxides. In that case I'll make sure to start small, and try to exclude oxygen as best I can...
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peach
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I can forgive any negative vibes emanating from len in other posts due to this, the rest of his posts here and particularly the mention of a spectrum
within the hard / soft definitions, something I've become very familiar with. Not forgetting the DIY sodium.
I have a liter of DMSO handy, so I could give it a go, but I'd prefer to go to the effort of whipping some ether up so I have that around if I need it
for anything else. I expect it'll also be far easier to work with than DMSO given the massive BP difference. Producing AlCl3 by a hot method isn't the
issue for me, it's dealing with the clogs and lumps it produces. The clogs mean problems. Poking around with sticks is asking for broken glass and
it'll never be clean or particularly free of BroLow acids with that much atmospheric exposure.
These AlCl3 threads are getting busy. Don't forget FeCl3, which can be dried to anhydrous under a stream of HCl(g) without it subliming all over the
place.
If you don't need a hard acid, things get even easier. Metal oxides feature Lewis acid sites. Microwave irradiation of some aryls, particularly those
with halides attached to the opposite side of the ring to the ether linkage, show potentially useful charge shifting in response to microwaves, which
appears to allow softer Lewis acids to attack it's lone pair when they normally wouldn't be bothered; hard Lewis acids attack hard Lewis bases, and
soft attack soft, preferentially. By making something like the lone pair on an oxygen appear softer than it would normally, softer acids attack more
efficiently.
[Edited on 31-8-2010 by peach]
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