Author Topic: Anhydrous metal salt - potential.  (Read 354 times)

2bfrank

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Anhydrous metal salt - potential.
« on: July 16, 2009, 08:12:25 AM »
Got it from somewhere, could of been SM or a literature reference.
US patent 3471250


2.75g ferric chloride hexahydrate(see electro preps Kings survival guide in various places for that) was dissolved in 30ml     EtOH, then 1.56g of DMSO added to provide an eventual precipitation of anhydrous FeCl3 complexed with 2 moles of DMSO, which is hydroscopic and stable at room temp. This can be heated in vaccum to a temp not increasing to 150C leaving anydrous FeCl3. The patent looks at NiCl2, MgCl2 and SnCl2.

The patent delves a little deeper, and perhaps could prove to be a useful way for ones FeCl3 etc, requirements.

Mr.Murphy

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Re: Anhydrous metal salt - potential.
« Reply #1 on: July 16, 2009, 10:08:44 AM »
It would be wise custom to provide the full reference at any time.

2bfrank

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Re: Anhydrous metal salt - potential.
« Reply #2 on: July 16, 2009, 11:38:53 AM »
Believe it or not, I dont know how. Its on the list, and untill I sort that out, at least I am giving a reference.

Mr.Murphy

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Re: Anhydrous metal salt - potential.
« Reply #3 on: July 16, 2009, 12:34:33 PM »
No problem, I uploaded the patent already in my first post in this thread.

Sedit

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Re: Anhydrous metal salt - potential.
« Reply #4 on: July 16, 2009, 01:44:06 PM »
2bfrank, When you are composing the post there is a link directly under the text box labled "Additional Options" when clicked on t will give you six other options and allow you to add attachments such as text files or pictures.
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2bfrank

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Re: Anhydrous metal salt - potential.
« Reply #5 on: July 17, 2009, 12:59:30 AM »
Thanks Sedit, and Mr Murphy for doing that, I got confused with thinking it was more than just an attatched pdf for some reason. Abit rattled when I wrote that.

Douchermann

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Re: Anhydrous metal salt - potential.
« Reply #6 on: July 17, 2009, 03:19:15 PM »
Hmmm, think this could be used on things such as AlCl3? That would be quite marvelous.

2bfrank

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Re: Anhydrous metal salt - potential.
« Reply #7 on: July 17, 2009, 10:35:12 PM »
I wonder indeed.

heisenberg

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Re: Anhydrous metal salt - potential.
« Reply #8 on: July 18, 2009, 01:19:33 AM »
Apparently it can be applied to AlCl3.

On page two of the patent it has AlCl3.6H2O in a list of applicable salts.
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xxx

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Re: Anhydrous metal salt - potential.
« Reply #9 on: July 21, 2009, 02:56:29 PM »
Now I hope this can work for MgSO4 or Mg(NO3)2 and such. It looks to have great potential!

v16

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Re: Anhydrous metal salt - potential.
« Reply #10 on: July 21, 2009, 04:22:17 PM »
Holy shit!!!

Time for some experimentation.


Time for some experimentation.  If anyone wants to do there own...

54g Al foil + 800 ml Hcl (36-38%) ADD AL FOIL VERY VERY VERY SLOWLY to the HCL.   Reaction will be violent.  If you hurt yourself its your fault.  The reaction releases H2 gas and enough heat to boil your HCL.  Go slow!!!

once all the Al has been consumed, add 100ml more of HCL, there should be NO further reaction.  If there is add further HCl over time until no reaction is seen.

Filter solution just to clear and pieces that did not fully break down.  Evaporate to 1/2 volume (about 400-450 ml) and cool in freezer, a large crop of crystals should drop out. Collect them, and reduce volume again by 1/2. Do a third time...

should yield about 400-450g of white crystals when dry. This is AlCl3*6H20

To make the anhydrous AlCl3  (first try...)

2.41 g of AlCl3*6H20 + 30 ml EtoH (Dry) (this can be changed down the line, 50g/100ml is the solubility of AlCl3 in ethanol)

add 1.56 g DMSO.  (I would add 2.34 your first time to ensure you get all the water displaced, again I would add until no more precipitate formed.)

Filter.  Dry under vacuum and low heat i would keep it at 80-100C


Resulting powder should react violently with water, and give off a arid fume.


If it works I would scale it up by 10 and use 3x amount of AlCl3 and DMSO for the same volume ETOH.  That 50g of Al foil should eventually get you about 200-225g of anhydrous AlCl3.  Should take no more than an afternoon of work.  Total cost 20$ maybe, less if you recover the DMSO.

Then you can make all the pipeonal you every wanted.


If this works, 2bfrank you win the "UC Literature Researcher of the Year"
















« Last Edit: July 21, 2009, 05:19:15 PM by v16 »

v16

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Re: Anhydrous metal salt - potential.
« Reply #11 on: July 21, 2009, 05:20:42 PM »
More thinking, maybe you want to scale back the AlCl3 hydrate production on your first try. I would really feel bad if someone got hurt.


Sedit

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Re: Anhydrous metal salt - potential.
« Reply #12 on: July 21, 2009, 05:48:24 PM »
Now I hope this can work for MgSO4 or Mg(NO3)2 and such. It looks to have great potential!

I can't help but ask Hex... HUH?

Are you talking about using this method to dry MgSO4?
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Vesp

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Re: Anhydrous metal salt - potential.
« Reply #13 on: July 21, 2009, 07:33:18 PM »
Alcohol should react with aluminum chloride shouldn't it? forming the alkoxide?

If it doesn't, why don't we just dissolve HCl gas into an alcohol, and add Al?

I guess the DMSO prevents this?
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v16

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Re: Anhydrous metal salt - potential.
« Reply #14 on: July 21, 2009, 08:16:42 PM »
Thats my understanding.  AlCl3-2DMSO complex is formed. It must protect the AlCL3, because the patent say the complex is non hygroscopic, its a great way to store AlCl3 untill you needed it. (You dry it then heat it to remove the DMSO (under vacuum) It ensures your material is 100% active when you go to use it, which is not the case with a typical AlCl3 in a jar.  By the time you are at the end of the material, it is not as active as when you started.

It appears the anhydrous AlCL3 is never produced in the EtOH.  This has huge possibilites guys, the more it rattles around in my brain.  Big ups, great work.

« Last Edit: July 21, 2009, 08:19:38 PM by v16 »

Vesp

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Re: Anhydrous metal salt - potential.
« Reply #15 on: July 21, 2009, 08:18:55 PM »
Noticed it was recently posted over at SM as well, it will be good to see what they think of it.
Where can one get OTC DMSO?
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v16

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Re: Anhydrous metal salt - potential.
« Reply #16 on: July 21, 2009, 08:23:06 PM »
I know green imp well.  ;)  We will make sure credit is given should it pan out.  Could be good advertising for the V if you guys want it.

99% DMSO is available at alternative health care stores.  It is used on swollen joints.  250 mls is like 10$.


Vesp

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Re: Anhydrous metal salt - potential.
« Reply #17 on: July 21, 2009, 08:28:49 PM »
Like how I know kclo4 well? ::)

I knew it was used to for that, but i figured they had mixed junk with it to make it useless for this purpose. I'm amazed it is 99%.
I believe I have heard it is also be used for horses for the same reasons and perhaps it would be cheaper and in larger quantities. I don't know if that is true though.
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v16

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Re: Anhydrous metal salt - potential.
« Reply #18 on: July 21, 2009, 08:33:35 PM »
I've used the 99% for methyleneation reactions, works fine.


Sedit

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Re: Anhydrous metal salt - potential.
« Reply #19 on: July 21, 2009, 08:44:40 PM »
My DMSO comes in the form of 70% DMSO from the health food stores. I have yet to figure out how to dry it well.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!