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Paul St. Germain
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[*] posted on 27-7-2019 at 08:52
Anhydrous AlCl3


I need some anhydrous AlCl3. I have two options:
1. Make it from AlCl3.6H2O.
2. Make it from ZnCl2.

I don't know ho to prepare it with neither of the two.

I know that it's possible with ZnCl2 but I don't know how.

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icelake
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[*] posted on 27-7-2019 at 09:11


Chemplayer's archived video:

https://archive.org/download/ChemPlayer/Anhydrous%20aluminiu...
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[*] posted on 27-7-2019 at 11:10


First route is unknown for me. On paper, yes, but in practice how to remove the water? Refluxing with a water scavenging compound e.g. acetic anhydride or thionyl-chloride? Frankly, I've yet to see a viable synth that started from the hydrate.

Someone suggested that AlBr3 may be a better -more amateur friendly- alternative.
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[*] posted on 27-7-2019 at 11:36


i haven't tried,but ithing you can relapse anhydrous ZnCl2 with anhydrous FeCl3 in the Chemplayer video.which is easy to get from an electronics shops.( some times some shops sells hydrated stuff but i know a shop that doesn't)
you can't dehydrate ZnCl2 ,FeCl3 or AlCl3 because they will make HCl and Leaving the oxides behind.
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[*] posted on 27-7-2019 at 12:26


It's an odd thought, but can you use excess aluminium as a dehydrating agent?
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Paul St. Germain
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[*] posted on 27-7-2019 at 12:52


Quote: Originally posted by icelake  
Chemplayer's archived video:

https://archive.org/download/ChemPlayer/Anhydrous%20aluminiu...


thanks for the information.
Will the RBF made of borosilicate glass withstand the temperature?
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VSEPR_VOID
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[*] posted on 27-7-2019 at 13:25


Chlorine gas, that has been dried with CaCl2, and aluminium turnings is the best option I would guess. I have never tried this myself. but if you can get a good reaction vessel it should not be too hard. Make sure to purge well with either an inert gas or Cl2 before adding the turnings. Aluminium oxide might contaminate your product.

For a reaction vessel you might consider making something out of a flour pot, sand, and someting to put over the whole thing to seal it. Another route would be using a quartz tube.



[Edited on 27-7-2019 by VSEPR_VOID]




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icelake
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[*] posted on 27-7-2019 at 22:19


Quote: Originally posted by Paul St. Germain  
Quote: Originally posted by icelake  
Chemplayer's archived video:

https://archive.org/download/ChemPlayer/Anhydrous%20aluminiu...


thanks for the information.
Will the RBF made of borosilicate glass withstand the temperature?

Probably, yes.
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rockyit98
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[*] posted on 27-7-2019 at 23:56


i think if you reacted anhydrous HCl in ethanol abs (http://chemister.ru/Database/properties-en.php?dbid=1&id...)
with aluminium metal it could work. use table salt with 98% H2SO4 to generate Hcl and dry it by bubbling into a 98% H2SO4,disolve that in ethanol abs while cooling.use it drop wise with aluminium metal with strong cooling. vacuum distill the ethanol abs.
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[*] posted on 28-7-2019 at 00:53


Quote: Originally posted by rockyit98  
i think if you reacted anhydrous HCl in ethanol abs (http://chemister.ru/Database/properties-en.php?dbid=1&id...)
with aluminium metal it could work. use table salt with 98% H2SO4 to generate Hcl and dry it by bubbling into a 98% H2SO4,disolve that in ethanol abs while cooling.use it drop wise with aluminium metal with strong cooling. vacuum distill the ethanol abs.


I think AlCl3 reacts with alcohol.
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[*] posted on 28-7-2019 at 03:09


Quote: Originally posted by rockyit98  
i haven't tried,but ithing you can relapse anhydrous ZnCl2 with anhydrous FeCl3 in the Chemplayer video.which is easy to get from an electronics shops.( some times some shops sells hydrated stuff but i know a shop that doesn't)


FeCl3 boils/decomposes at 316 °C, but ZnCl2 is pretty stable and boils at 732 °C -- so Iron Chloride can/will contaminate the product.
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[*] posted on 28-7-2019 at 04:45


Has anyone considered CuCl?

Since CuCl isn't even soluble in water, it's not difficult to get it very dry.
I suspect the reaction might be violent.
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[*] posted on 28-7-2019 at 06:24


Quote: Originally posted by VSEPR_VOID  
Chlorine gas, that has been dried with CaCl2, and aluminium turnings is the best option I would guess. I have never tried this myself. but if you can get a good reaction vessel it should not be too hard. Make sure to purge well with either an inert gas or Cl2 before adding the turnings. Aluminium oxide might contaminate your product.

For a reaction vessel you might consider making something out of a flour pot, sand, and someting to put over the whole thing to seal it. Another route would be using a quartz tube.
[Edited on 27-7-2019 by VSEPR_VOID]


Actually, I was thinking of undried chlorine (perhaps safer in this experiment than dry Cl2) in a large wide mouth reaction vessel filled with Cl2 (from a chlorine generator since removed). I would wrap Reynold's Extra Strength Aluminum foil (which contains added iron for strength) around an inert stone, for example, creating a long filament that can be inserted into the vessel, so as it is standing up. Place a glass lid over the mouth of the chlorine (and some air) filled vessel, which is then placed in a microwave.

Start the camera rolling (if risking a glass vessel in this experiment) and turn on the microwave (MW) for say 10 seconds or less. Caution, I have actually experienced a porcelain disk shattering in a related experiment that was in touch with MW generated plasma arc. This is the rationale for constructing the Al filament, so as to reduce the likely contact of the extremely high temperature arc with the glass/ceramic vessel.

The Fe presence in the Al foil could create a very high temperature plasma arc (like 10,000 K, see https://www.sciencedirect.com/topics/physics-and-astronomy/p...) that is expected to result in near total consumption of the Al foil and chlorine, with spectacular pyrotechnics, in seconds. This is in contrast to minutes of a slow reaction per the Al/ZnCl2 video referenced above.

However, the AlCl3 may have some FeCl3 presence (perhaps removal by heating) and likely some Al(OH)2/Al2O3 impurity (from oxygen/water vapor, which may be chemically inert for the intended use of the AlCl3).
-----------------------------------------------

WARNING: Safety precautions a must, especially against corrosive fumes and having a fire extinguisher handy is always advisable in a lab. Do not use a new expensive microwave oven, intended for home cooking, in this proposed experiment, as it could suffer damage and/or be rendered unsafe for cooking.

[Edited on 28-7-2019 by AJKOER]
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[*] posted on 28-7-2019 at 08:47


Quote: Originally posted by AJKOER  
Do not use a new expensive microwave oven, intended for home cooking, in this proposed experiment, as it could suffer damage and/or be rendered unsafe for cooking.


That's the understatement of the year.

Please disregard AJKOER's post. If you follow his instructions, you'll have an exploded microwave and a cloud of chlorine. Even without the chlorine, putting aluminum foil in a microwave is a good way to destroy it.

I'm still not sure why AJKOER hasn't been banned yet . . . although I think the problem would solve itself if he actually tried out his proposed experiments

[Edited on 2019-7-28 by Metacelsus]




As below, so above.
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[*] posted on 28-7-2019 at 09:47


Quote: Originally posted by Metacelsus  
Quote: Originally posted by AJKOER  
Do not use a new expensive microwave oven, intended for home cooking, in this proposed experiment, as it could suffer damage and/or be rendered unsafe for cooking.


That's the understatement of the year.

Please disregard AJKOER's post. If you follow his instructions, you'll have an exploded microwave and a cloud of chlorine. Even without the chlorine, putting aluminum foil in a microwave is a good way to destroy it.[Edited on 2019-7-28 by Metacelsus]


I agree, Al foil in a microwave is a recipe for disaster.
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rockyit98
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[*] posted on 29-7-2019 at 09:04


Quote: Originally posted by icelake  
Quote: Originally posted by rockyit98  
i haven't tried,but ithing you can relapse anhydrous ZnCl2 with anhydrous FeCl3 in the Chemplayer video.which is easy to get from an electronics shops.( some times some shops sells hydrated stuff but i know a shop that doesn't)


FeCl3 boils/decomposes at 316 °C, but ZnCl2 is pretty stable and boils at 732 °C -- so Iron Chloride can/will contaminate the product.

so don't distill the mix till all FeCl3 react and no left out . even if it doesn't work make ZnCl2 first by FeCl3 with extra Zn metal.
-----------------------------------------------------------------------------------
my phone keeps Autocorrecting "FeCl3" to "Fecal".:D FeCl3 is better.
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[*] posted on 29-7-2019 at 10:13


You can't wait till all of the FeCl3 is reacted - this is an exothermic reaction.

Al + FeCl3 --> Fe + AlCl3

AlCl3: ΔfH° = -705.63 kJ/mol
FeCl3: ΔfH° = -399.5 kJ/mol

ΔH°rxn = -306.13 kJ (ignore the physical states of the reactants/products for now).

The ΔH value is huge and it could be a violent reaction.
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[*] posted on 29-7-2019 at 12:15


I didn't try, but I guess it has a good chance of working (AlBr3):

Make bromine with a bromide dissolved in diluted H2O2 by adding some diluted sulfuric acid in a separatory funnel while being over DCM. Get rid of the water layer and dry with concentrated sulfuric acid. DCM and sulfuric don't mix.

Now add aluminum and evaporate the DCM. Sounds easy in theory.

Ofcourse this should also work with a chloride, but at lower temperatures.

[Edited on 29-7-2019 by Tsjerk]
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[*] posted on 29-7-2019 at 13:07


Quote: Originally posted by Metacelsus  
Quote: Originally posted by AJKOER  
Do not use a new expensive microwave oven, intended for home cooking, in this proposed experiment, as it could suffer damage and/or be rendered unsafe for cooking.


That's the understatement of the year.

Please disregard AJKOER's post. If you follow his instructions, you'll have an exploded microwave and a cloud of chlorine. Even without the chlorine, putting aluminum foil in a microwave is a good way to destroy it.

I'm still not sure why AJKOER hasn't been banned yet . . . although I think the problem would solve itself if he actually tried out his proposed experiments

[Edited on 2019-7-28 by Metacelsus]


Really, a small Aluminum filament is going to destroy a microwave?

I know of so many instances of people trying to warm up leftovers in sizable aluminum containers, for minutes, by accident or ignorance, which seems to equally apply to your 'point'.

The largest possible vessel that can be placed into a microwave is less than 2 liters. So, you are claiming, at the high end, 2 liters of Cl2 equals a 'cloud of chlorine', a bit of an exaggeration perhaps.

Your comment, applying to my 7 MV second process, is without basis and is nothing more than a disguised personal attack.
-------------------------------------------------------------------

Interestingly, I have used the Al filament concept in other experiments to test its power in high temperature gas reactions with zero issues, and I still have a lab MW where I just did another prep reported on SM.

Nevertheless, I felt it was advisable to add a stern safety warning because some people do not follow directions on time exposure or the amount of Al. By the way, it is also dangerous to place too much water in your tub (just in case, there isn't an existing caution label already on your tub).

[Edited on 29-7-2019 by AJKOER]
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Tsjerk
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[*] posted on 29-7-2019 at 13:26


I'm perfectly fine with AJOEKER starting his own three week long threads with no other people's reactions, but can this guy be either restricted, banned or get a subscribtion saying "whatever I say is only going on in my mind"?
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Paul St. Germain
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[*] posted on 29-7-2019 at 14:19


I found this procedure of dehydration of aluminium chloride hexahydrate:
https://patents.google.com/patent/CN103803622A/en

As you guys can see it has been translated form Chinese.

I think i will try the Chemplayer's video because I think it's easier.



[Edited on 29-7-2019 by Paul St. Germain]

[Edited on 29-7-2019 by Paul St. Germain]
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AJKOER
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[*] posted on 29-7-2019 at 15:04


I have an suggestion:

"I believe aluminum foil, with a small iron impurity, to which is applied a microwave pulse, will burn in an atmosphere of damp chlorine gas tainted with air"

It is, after all, precisely the point of contention.
-----------------------------------------------------------

My contention is based on the presence of air and water vapor, as even if a radical chain reaction was somehow initiated with aluminum vapor, the presence of oxygen, from any air or even sourced from HOCl, along with HCl, created in a chlorine and water reaction, is a known inhibitor for the H2/Cl2 radical chain reaction explosion (see https://pubs.acs.org/doi/pdf/10.1021/ed020p41 ) as is apparently the presence of HCl also (see, for example, discussion at https://royalsocietypublishing.org/doi/abs/10.1098/rspa.1942... ) assuming in the current context, that Al is as reactive as H2.
--------------------------------------------------

By the way, I have actually employed N2O in the present of a small Al filament, to which I have applied a microwave pulse, to introduce NO into an HOCl mix (and as HOCl decomposes slowly to HCl, this mix undoubtedly contained some Cl2, so I have already perform this Cl2/Al reaction!) for chlorate creation: see https://www.sciencemadness.org/whisper/viewthread.php?tid=34... .

Here is a quote for those interested in the science:

"First, some theoretical background to provide understanding, promote safety and good yield.

One interesting paper is "Treatment of N2O impulsed microwave torch discharge " by M.Jasinski, et. al., April 2004 . To quote: "Results of using a moderate–power (several hundred Watts) pulsed microwave torch plasma (MTP) to the conversion of atmospheric-pressure nitrous oxide (N2O) into nitrogen oxides( NO, NO2 and N2O4) are presented." with a claimed efficiency between 70% to 90% depending on the power of the microwave. Link: https://www.google.com/url?sa=t&source=web&rct=j&...

This possible conversion of N2O is also cited in this source, "Focus on Hazardous Materials Research", edited by Leonora G. Mason, to quote : "In our previous study using microwave discharge, N2O could be efficiently decomposed into N2 and O2 at atomospheric pressure [8]. However, when N2O is diluted in N2/O2 mixtures was decomposed by microwave discharge, a large amount of NO was emitted due to fast reactions as N(2D,2P) + O2 --> NO + O link: http://books.google.com/books?id=8MXX01Qw_G0C&pg=PA144&a...

So, for the purpose of constructing a net reaction for the gas phase in the radiolysis of N2O diluted in N2 and a O2 enriched mixture in a microwave, I will assume, as an undoubted simplication, a reaction sequence that has one of the larger associated oxygen (which is supplied pre-run) and nitrogen demands:

1/2 N2 + pulse radiation ---> N(2D,2P)
N(2D,2P) + O2 --> NO + O
O + N2O ---> 2 NO

Simplied net reaction ignoring possible benefical formation of any NO2 and several other intermediate nitrogen and oxygen species:

1/2 N2 + O2 + N2O --pulse radiation--> 3 NO

With shaking of the pulsed radiated vessel, a reaction with Hypochlorous acid:

2 NO + 3 HOCl + H2O --> 3 HCl + 2 HNO3 "

[Edited on 30-7-2019 by AJKOER]
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