Re: Anhydrous metal salt - potential.
« Reply #20 on: July 21, 2009, 09:04:29 PM »
Topic: Anhydrous metal salt - potential. (Read 354 times)
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Douchermann
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Re: Anhydrous metal salt - potential.
« Reply #21 on: July 22, 2009, 12:55:45 AM »
Sedit, there is a patent out there that details the removal of water through azeotropic distillation. Don't know the number or anything, but take a look around. I've gotten my DMSO from www.kvvet.com, nice a pure, no problems getting the order to a residence.
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Re: Anhydrous metal salt - potential.
« Reply #22 on: July 22, 2009, 01:15:39 AM »
I tryed to dry it over MgSO4 but that lead to a gel like substance that I never got around to distilling to see if it was dryer then before. I suppose a dash of acetone,MEK or EtOH should also work wounders here to strip it of the water nicely.
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Re: Anhydrous metal salt - potential.
« Reply #23 on: July 22, 2009, 07:36:17 PM »
If the AlCl3-DMSO precipitate can be made anhydrous, why couldn't it be used directly for some reactions?
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Re: Anhydrous metal salt - potential.
« Reply #24 on: July 22, 2009, 08:08:08 PM »
I have feeling it is a pretty tight assoication, and will adversial effect the ablity of of AlCl3 to act as a lewis acid.
I will try this tomorrow, so we will no either way soon. I am going to do a small scale test on some anhydrous AlCl3 i have which is no longer really anhydrous....saves me the trouble of dissolving Al foil...
If the DMSO-AlCl3 precipitate forms, I feel it is a viable process, even if we have to sublime the AlCl3 to purify it. Under vacuum, I can get AlCl3 to sublime at about 68C, DMSO will not go off till about 110-200. As long as you have a really good cold finger, it could work.
The problem as I am thinking about it, is that you will have the heat the DMSO-AlCL3 to 110-120 under vacuum to get the DMSO to liberate. Then immediately afterwards, the AlCL3 will sublime. So you will need to somehow recover just the AlCL3.
Then again maybe something else is happening. I don't remember if AlCl3 sublimes due to a covalent reaction or inter-molecular forces. It is possible that heating the AlCL3-DMSO might cause it to react with itself....
But this process works for MgCL2 hydrate, and that gives me hope.
I will try this tomorrow, so we will no either way soon. I am going to do a small scale test on some anhydrous AlCl3 i have which is no longer really anhydrous....saves me the trouble of dissolving Al foil...
If the DMSO-AlCl3 precipitate forms, I feel it is a viable process, even if we have to sublime the AlCl3 to purify it. Under vacuum, I can get AlCl3 to sublime at about 68C, DMSO will not go off till about 110-200. As long as you have a really good cold finger, it could work.
The problem as I am thinking about it, is that you will have the heat the DMSO-AlCL3 to 110-120 under vacuum to get the DMSO to liberate. Then immediately afterwards, the AlCL3 will sublime. So you will need to somehow recover just the AlCL3.
Then again maybe something else is happening. I don't remember if AlCl3 sublimes due to a covalent reaction or inter-molecular forces. It is possible that heating the AlCL3-DMSO might cause it to react with itself....
But this process works for MgCL2 hydrate, and that gives me hope.
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Re: Anhydrous metal salt - potential.
« Reply #25 on: July 22, 2009, 09:15:09 PM »
I don't see why, if the DMSO is complexed with the AlCl3, that they would not leave at the same time, and form some sort of "azeotrope" thing. I'd think as the AlCl3 and the DMSO sublimate and precipitate/condense, they'll just form the same AlCl3-DMSO again.
If heating the AlCl3-DMSO leads to its decomposition into the 2 products, I'd think that heating it in, for example, boiling toluene (110*C -ish?) that it would free both of them, and allow for the AlCl3 to do its thing. I could be totally wrong though.
Perhaps another method to get pure anhydrous AlCl3, would be to use a compound that could trap the DMSO and free the AlCl3? For instance maybe a lewis acid that has a significantly higher sublimation temperature could allowe the reaction to shift towards free AlCl3 as it is heated, having the AlCl3 sublimate away.. So:
AlCl3-DMSO + X <=> X-DMSO + AlCl3
X = suitable lewis acid, such as FeCl3, etc.
If heating the AlCl3-DMSO leads to its decomposition into the 2 products, I'd think that heating it in, for example, boiling toluene (110*C -ish?) that it would free both of them, and allow for the AlCl3 to do its thing. I could be totally wrong though.
Perhaps another method to get pure anhydrous AlCl3, would be to use a compound that could trap the DMSO and free the AlCl3? For instance maybe a lewis acid that has a significantly higher sublimation temperature could allowe the reaction to shift towards free AlCl3 as it is heated, having the AlCl3 sublimate away.. So:
AlCl3-DMSO + X <=> X-DMSO + AlCl3
X = suitable lewis acid, such as FeCl3, etc.
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Re: Anhydrous metal salt - potential.
« Reply #26 on: July 22, 2009, 09:30:06 PM »
Seeing as how the DMSO is recoverable(correct me if Im wrong) then I could use this also to produce anhydrous DMSO also from my 70% shit right? Collect the precipitate then decompose the addition product to yeild dry DMSO and dry AlCl3.
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Re: Anhydrous metal salt - potential.
« Reply #27 on: July 22, 2009, 09:37:58 PM »
I would think so, but it seems like it would be one of the more difficult ways to obtain anhydrous DMSO, despite the wonderful by product.
Is DMSO really hard to dry or something?
Is DMSO really hard to dry or something?
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Re: Anhydrous metal salt - potential.
« Reply #28 on: July 22, 2009, 10:48:21 PM »
one property of dmso is that it solidifies at lower temp - above the freezing point of water. just a thought.
but then again, I;d imagine that a solution of DMSO and water, will only increase its melting point, hence not be applicable in seperation. Perhaps the gel that was obtained by drying it with MgSO4 is in fact dry and just needs heat. Time to stop rambling and do some experiments.
but then again, I;d imagine that a solution of DMSO and water, will only increase its melting point, hence not be applicable in seperation. Perhaps the gel that was obtained by drying it with MgSO4 is in fact dry and just needs heat. Time to stop rambling and do some experiments.
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Re: Anhydrous metal salt - potential.
« Reply #29 on: July 23, 2009, 12:11:02 AM »
Tune in tomorrow...ill have some numbers.
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Re: Anhydrous metal salt - potential.
« Reply #30 on: July 23, 2009, 12:11:59 AM »
Thats a good possibility that the gel was nothing more then the now dry DMSO solidifying but the way I see it if I get dry DMSO and dry AlCl3 as products why not give it a shot. It may just stay liquid in solution with H2O at low temperatures but when the H2O complexed with the MgSO4 is allowed the DMSO to solidify....hum can't believe I didn't think of that before.
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Re: Anhydrous metal salt - potential.
« Reply #31 on: July 23, 2009, 12:17:18 AM »
from patent - just above example 1.......it says aqueous solutions of DMSO can be used!!! at around 50%
that is typical of me not reading the patent in its entirety. I did so, when I wondered what other reagents could be used to form a complex, that could be removed as such. So my bad for posting a procedure and not highlighting requirements. With that said, seeing the possibility of being able to use less than pure DMSO, etc, is somewhat GOOD. That is unless the patent is full of shit. I think I will abstain from presenting any procedures, unless I feel certain that they are not runaround's
that is typical of me not reading the patent in its entirety. I did so, when I wondered what other reagents could be used to form a complex, that could be removed as such. So my bad for posting a procedure and not highlighting requirements. With that said, seeing the possibility of being able to use less than pure DMSO, etc, is somewhat GOOD. That is unless the patent is full of shit. I think I will abstain from presenting any procedures, unless I feel certain that they are not runaround's
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Re: Anhydrous metal salt - potential.
« Reply #32 on: July 23, 2009, 12:44:33 AM »
no thats what we are here for, in part to bounce ideas off each other...
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Re: Anhydrous metal salt - potential.
« Reply #33 on: July 23, 2009, 02:43:40 AM »
yes agreed, but dont like seeing time-anyones time-wasted due to lack of necessary info, yet it is surely good to bounce things around.
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Re: Anhydrous metal salt - potential.
« Reply #34 on: July 23, 2009, 02:49:45 AM »
Understandable but thats one of the great things about here, We don't waste our time with lack of info because im sure I can speak for 90% here if someone presents us with an idea were going to find the necessary information ourselfs as well before attempting it. We have a very literate group of people here so no fear of us wasting out time.
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Re: Anhydrous metal salt - potential.
« Reply #35 on: July 23, 2009, 06:24:33 PM »
Report on first stage of this:
4g anhydrous AlCl3 added to 50 ml H20, very slowly. After all the solid had been dissolved, heat was applied and the water was removed at atmospheric pressure. A white crystalline solid remained. This was resuspended in 50 ml of 95% Etoh.
After it was resuspended 50 ml of 99.9% DMSO was slowly added to the EtoH solution. No ppt was seen. The DMSO-EtOH solution was heated to remove the EtoH, the solution went from clear to yellow as the EtoH was removed. After about 45 ml of EtOH was removed, the solution turned white and and a snowy ppt was seen. The solution was cooled and the ppt collected by filtration.
Will attempt to removed DMSO tonight.
I think it may have worked....can't believe I got the ppt.
4g anhydrous AlCl3 added to 50 ml H20, very slowly. After all the solid had been dissolved, heat was applied and the water was removed at atmospheric pressure. A white crystalline solid remained. This was resuspended in 50 ml of 95% Etoh.
After it was resuspended 50 ml of 99.9% DMSO was slowly added to the EtoH solution. No ppt was seen. The DMSO-EtOH solution was heated to remove the EtoH, the solution went from clear to yellow as the EtoH was removed. After about 45 ml of EtOH was removed, the solution turned white and and a snowy ppt was seen. The solution was cooled and the ppt collected by filtration.
Will attempt to removed DMSO tonight.
I think it may have worked....can't believe I got the ppt.
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Re: Anhydrous metal salt - potential.
« Reply #36 on: July 28, 2009, 05:58:01 PM »
AlCl3 hydrates can be dried to unhydrous AlCl3 by heating with excess NH4Cl. That is uneasy, a great excess of NH4Cl is needed, and time/energy consuming. But i imagined, if there could be some option to recycle NH4Cl and optimise the procedure in time and energy needed. Nothing comes to mind still.
Sorry, just realised the matter of discussion is bit different
Sorry, just realised the matter of discussion is bit different
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Re: Anhydrous metal salt - potential.
« Reply #37 on: July 28, 2009, 06:10:01 PM »
I have heard this is a method to anhydrous zinc chloride, as well as passing over dry HCl on the heated chloride hydrate.
Do you have a reference for this method of dehydrating AlCl3?
Do you have a reference for this method of dehydrating AlCl3?
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Re: Anhydrous metal salt - potential.
« Reply #38 on: July 28, 2009, 06:12:40 PM »
Surely i've seen it for AlCl3. Ok, i'll try to find the refference
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Re: Anhydrous metal salt - potential.
« Reply #39 on: July 28, 2009, 10:31:07 PM »
Enkidu I will post the patent here as well for you and everyone else on the production of anhydrous AlCl3 from Aluminum sulfate and NaCl or CaCl ect...ect...
Aluminum Chloride.pdf
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