| Pages:
1
2 |
Polverone
Now celebrating 21 years of madness
Posts: 3186
Registered: 19-5-2002
Location: The Sunny Pacific Northwest
Member Is Offline
Mood: Waiting for spring
|
|
Beautiful! Al + Br2
There's a gorgeous picture in one of my chemistry books of a strip of aluminum burning in bromine. Today, I recreated that image in miniature.
I mixed a small quantity of sodium bromide with an excess of phosphoric acid and an ice cube. I added calcium hypochlorite to this mixture while
swirling, giving rise to fumes of bromine above the icy mixture and causing the temperature to rise somewhat. I decided that placing the cooling
directly in the jar wasn't the best idea I'd ever had, so I then placed the jar in a bowl of ice water.
I noticed that I could see dark droplets collecting at the bottom of the jar. Ah-ha! Bromine!
Putting on protective gloves for the first time in months, I used a disposable plastic pipet to suck a mL or so of bromine from the bottom of the
vessel and place it in a pyrex test tube. Upon nervously adding a twist of aluminum foil to the test tube, I observed a vigorous reaction accompanied
by occasional sparks and a thick plume of bromine vapor exiting the test tube. I turned the bathroom fan and shower on and exited the room, closing
the door and hoping that the metal in the room wouldn't corrode too much more.
I don't know how soluble water is in bromine. Would it be possible to prepare dry bromine from the crude liquid without distilling it?
Bromine is easier to handle than chlorine, since it is more easily tamed by cold, and someone with more courage than money might be able to produce
substantial amounts of anhydrous AlBr3 from homebrewed bromine.
[Edited on 8-12-2004 by Polverone]
PGP Key and corresponding e-mail address
|
|
|
vulture
Forum Gatekeeper
Posts: 3330
Registered: 25-5-2002
Location: France
Member Is Offline
Mood: No Mood
|
|
I've been tempted to perform this reaction too, but my current lack of bromine and time prevents it.
I wonder what Al + I2 will do? I doubt it's spontaneous, but maybe with some heating?
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
|
|
|
sylla
Alchimiste Belge Notoire
Posts: 110
Registered: 2-8-2003
Location: Belgium
Member Is Offline
Mood: No Mood
|
|
Al/I2 isn't spontaneus but still very easy to ignite.
Just add a drop of water on the mix ; it will first fume (nice I2 vapors) and then ignite with a bright white color
|
|
|
Esplosivo
Hazard to Others
Posts: 491
Registered: 7-2-2004
Location: Mediterranean
Member Is Offline
Mood: Quantized
|
|
Vulture, I guess you already know but anyway the rxn between Al and I2 can be started by a drop of water and it then continues reacting on its own.
Its quite nice really  Both the Al and I2 should be finely ground fo this to
work.
Theory guides, experiment decides.
|
|
|
vulture
Forum Gatekeeper
Posts: 3330
Registered: 25-5-2002
Location: France
Member Is Offline
Mood: No Mood
|
|
Interesting, I still have a sample of german dark Al laying around...
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
|
|
|
BromicAcid
International Hazard
Posts: 3253
Registered: 13-7-2003
Location: Wisconsin
Member Is Offline
Mood: Rock n' Roll
|
|
| Quote: | | I don't know how soluble water is in bromine. Would it be possible to prepare dry bromine from the crude liquid without distilling it?
|
When doing my bromine research I found that bromine distilled from a mixture has about 2% water that carries over that is not a 'true'
azeotrope. From what I remember bromine is easy to dry but I've never needed dry bromine so I've never tried it.
|
|
|
vulture
Forum Gatekeeper
Posts: 3330
Registered: 25-5-2002
Location: France
Member Is Offline
Mood: No Mood
|
|
Bromine can be easily dried by shaking with conc. sulfuric acid. If your bromine contains much water cooling will be necessary ofcourse.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
|
|
|
Nick F
Hazard to Others
Posts: 439
Registered: 7-9-2002
Member Is Offline
Mood: No Mood
|
|
Is there anything wrong with simply adding crushed fused sodium sulphate, shaking and filtering (using a glass fibre filter)?
|
|
|
vulture
Forum Gatekeeper
Posts: 3330
Registered: 25-5-2002
Location: France
Member Is Offline
Mood: No Mood
|
|
That'll work too, but with sulfuric acid you have a much more intimate contact since it's a fluid too. You'll have trouble to get out
all the water in one pass with the sodium sulphate or any other solid drying agent (with the exception of P4O10 perhaps).
How about phosphoric acid?
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
|
|
|
Hang-Man
Hazard to Self
Posts: 70
Registered: 16-1-2004
Location: Canada
Member Is Offline
Mood: Wasted
|
|
| Quote: | | I wonder what Al + I2 will do |
I wonder what Al + HIO3 will do. Iodic acid is a very powerfull oxidizer if I remember corectly.
|
|
|
MadHatter
International Hazard
Posts: 1347
Registered: 9-7-2004
Location: Maine
Member Is Offline
Mood: Enjoying retirement
|
|
German Dark
Vulture, you said you still have some German Dark Al powder. Mixed with
finely powdered iodine, that should make for an interesting "flash" powder.
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
|
|
|
vulture
Forum Gatekeeper
Posts: 3330
Registered: 25-5-2002
Location: France
Member Is Offline
Mood: No Mood
|
|
Very possibly, that's why I'll test smallscale first. My primary concern is to fetch the resulting AlI3, as this can be of extraordinary
use.
My main problem is that I don't have a good way of drying my iodine without loosing too much, it's expensive as hell.
[Edited on 12-8-2004 by vulture]
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
|
|
|
thunderfvck
Hazard to Others
Posts: 347
Registered: 30-1-2004
Location: noitacoL
Member Is Offline
Mood: No Mood
|
|
Can AlBr3/AlI3 be used to replace AlCl3?
|
|
|
Esplosivo
Hazard to Others
Posts: 491
Registered: 7-2-2004
Location: Mediterranean
Member Is Offline
Mood: Quantized
|
|
| Quote: | Originally posted by thunderfvck
Can AlBr3/AlI3 be used to replace AlCl3? |
In which procedure/reaction? I suppose that AlCl3 possess some different chemical properties when compared to AlBr3 and AlI3.
Theory guides, experiment decides.
|
|
|
Hang-Man
Hazard to Self
Posts: 70
Registered: 16-1-2004
Location: Canada
Member Is Offline
Mood: Wasted
|
|
AlCl3 is used as a deliquescent and as a catylst in cracking oils and other organic reactions, specifically the Friedel-Crafts rxn (acylation of
aromatic compounds)
Seing as the latter isn't usefull to many home chemists, I assume he means as a deliquescent.
|
|
|
thunderfvck
Hazard to Others
Posts: 347
Registered: 30-1-2004
Location: noitacoL
Member Is Offline
Mood: No Mood
|
|
Actually I was wondering if they could be used to replace AlCl3 in Friedel Crafts akylations.
C6H6 + R-X --AlCl3--> C6H5-R + HX
R=alkyl group
X=halogen
I've also seen it mentioned in other reactions as well, although I can't remember which...Anyways, I was just wondering if I could
substitute this with AlBr3/AlI3?
[Edited on 13-8-2004 by thunderfvck]
|
|
|
BromicAcid
International Hazard
Posts: 3253
Registered: 13-7-2003
Location: Wisconsin
Member Is Offline
Mood: Rock n' Roll
|
|
I did aluminum turnings (which were oxidized on one side) with bromine dried under H2SO4 today and took pictures every 10 seconds or so, attached is
the series of pictures I ended up with. I had to use a stir rod as the aluminum turnings reacted that got smaller and smaller and sunk to the bottom
forming a lump. When I pulled out the stirring rod it was covered in a black slime, the tube was mildly hot. When I put the stirring rod in Xylene
it crackeled like it was red hot and the AlBr3 started to flake off and colored the Xylene greyish/redish. Overall it looked neat but I didn't
get any sparks or anything, I think the aluminum was too thick. Might have to try it again as I did it for my book project and wanted a near picture,
I guess I'll just do chlorine and sodium, always a crowd pleaser 
Edit: Just some notes, when I was drying my Br2 with H2SO4 white choking fumes kept coming off, a mixture of HBr and SO2 I would guess. This could
come from any of a number of sources, NaBr dissolved in my Br2 (although the solubility of NaBr in Br2 is incredibly low). KBrO3 in my Br2, and any
of a number of impurities in my drain cleaner H2SO4 or maybe just bromines action on the dyes present or any of a number of things. There was inital
quick gas evolution then it slacked off, it looks like less Br2 vapor comes off the mixture then just bromine stored under H2O so I might have to try
this and just store my bromine under H2SO4, should really distill it all first considering it appears to react with it though, might be a good way to
get rid of whatever is in there that is reacting. Oh well, back on topic.
[Edited on 3/26/2005 by BromicAcid]
|
|
|
kryss
Hazard to Self
Posts: 77
Registered: 11-7-2003
Location: N Ireland
Member Is Offline
Mood: No Mood
|
|
Aluminium & Iodine
This is impressive too, we did it at school years ago - you can grind them up together then nothing happens until you add a couple of drops of water
which starts a vigourous reaction - I'd do this outside unless you have a fume hood! You get I2 vapour and AlI3 vapour coming off - loads of
corrosive smoke!!
|
|
|
BromicAcid
International Hazard
Posts: 3253
Registered: 13-7-2003
Location: Wisconsin
Member Is Offline
Mood: Rock n' Roll
|
|
Being that anhydrous aluminum bromide is so useful I decided to make a quantity of it today. I added 6 or 7 grams of aluminum turnings to a large
Pyrex test tube and added 20 ml or so of bromine to a sepretory funnel along with 30 ml concentrated H2SO4 and shook it up to dry the bromine. After
drying I took the stem of the sepretory funnel and put it into the test tube, using some duct tape around the opening. I turned the stopcock to allow
a drop to fall in every few seconds.
Each drop was accompanied by some white/yellow fumes, I'm assuming they were Al2Br6 vapors mixed with some HBr and Al2O3 and such. The reaction
continued and after a while I had a deep black liquid at the bottom of the test tube. I figured this was unreacted bromine but I couldn't figure
out why the aluminum left inside wasn't reacting so I ruled that out, I later found out the melting point of aluminum bromide is <100C so due
to the heat of reaction this was probably mostly molten aluminum bromide. Anyway, the reaction continued and ever once in a while the aluminum would
catch on fire, it would burn like a strip of magnesium, melting onto itself and sending deep red fumes out of the cracks in the duct tape. Eventually
the bottom portion of the test tube solidified and the top was in a puddle of Br2/AlBr3 and was reacting away merrily. And finally the whole thing
was solidified, looking similar to metal where the crystals were in contact with the side of the test tube, the mass was very heavy.
To this I added some benzene cautiously, hoping there wasn't much unreacted Br2 in the mix, and hoping that there wasn't copious amounts of
some complex like AlBr4<sup>+</sup>Br<sup>-</sup> present in large amounts. There was some bubbling but nothing major so I
added more, the mixture became black from the AlBr3 dissolving and the bubbling ceased. Hopefully most will dissolve and I can filter and evaporate
my benzene to get my product.
Some neat things about AlBr3:
1) Technically it could furnish anhydrous HBr gas:
AlBr3 + 3H2O ---> Al(OH)3 + 3HBr
Water would be a contaminate but one could simply use a drying tube of AlBr3 to convert excess water to HBr. Unlike organic methods of producing HBr,
all the bromine used to make the AlBr3 would be recovered as HBr.
2) Electroplating Aluminum:
I found a few articles on electroplating aluminum from toluene. Turns out that over 25g of AlBr3 will dissolve in 100 ml toluene and this can be used
as a bath to electroplate shiny aluminum on objects. Aluminum powder would not be much of a stretch from here.
3) Of course it can be a catalyst in alkylations and other organic reactions.
4) Drying agent
5) Produce the alkali metals though non-aqueous electrolysis of fused AlBr3 with an alkali halide in nitrobenzene.
Never the less, the reaction of bromine with aluminum is indeed beautiful, just be wary it heats up very hot rapidly if there is lots of aluminum
present, there is a sort of induction period with dry Br2 at room temp so don't over do it.
|
|
|
a123x
Hazard to Self
Posts: 87
Registered: 12-1-2003
Member Is Offline
Mood: No Mood
|
|
I've recently been experimenting with making alkoxides by the electrolysis of solutions of NaBr in methanol or ethanol. In one chamber of the
electrolytic cell the alkoxide is formed and in the other, a solution of bromine in alcohol is formed. This solution of bromine in alcohol reacts
readily enough with iron powder to produce FeBr3. The reaction isn't very reapid with Fe but does get fairly warm. I figure aluminum should react
well enough with such a bromine solution. The alcohol can then be distilled off to leave the anhydrous AlBr3.
|
|
|
tom haggen
Hazard to Others
Posts: 488
Registered: 29-11-2003
Location: PNW
Member Is Offline
Mood: a better mood
|
|
Just out of curiosity, would the manufacture of bromine go something like this.
3NaBr + H3PO4 <====> 3HBr + Na3PO4
2HBr + NaOCl <====> 2Br + NaCl + H2O
N/A
|
|
|
Lambda
National Hazard
Posts: 566
Registered: 15-4-2005
Location: Netherlands
Member Is Offline
Mood: Euforic Online
|
|
| Quote: | Originally posted by sylla
Al/I2 isn't spontaneus but still very easy to ignite.
Just add a drop of water on the mix ; it will first fume (nice I2 vapors) and then ignite with a bright white color |
Quit a few decades ago, a teacher wanted to demonstrate to his students, the redox reaction between aluminium powder and silver nitrate.
He demonstrated this experiment on a hot summer day. It was so warm that day that sweat-drops accumulated on his forehead. While mixing these two
ingredients together in a pestill, a drop of sweat fell into it. The bright flash that resulted from this catalytic induced reaction, blinded this
poor old chump for more than two weeks.
During this periode he was hospitalized.
| Quote: | We can't live without water, but it shoure can make life short sometimes !
|
[Edited on 20-6-2005 by Lambda]
|
|
|
Madandcrazy
Hazard to Others
Posts: 117
Registered: 11-5-2005
Member Is Offline
Mood: annoyed
|
|
Tell the teacher too, redox composites with Al are hard to ignite and a few nitrates being qualified for this.
When the powder fine, the reaction can be ignited with a electric arc or carbon
arc.
Polverone, i wondering about the tread of the sticky production of AlBr3 by
sodium bromide in a homebrewed process.
|
|
|
blip
Hazard to Others
Posts: 133
Registered: 16-3-2003
Member Is Offline
Mood: absorbed
|
|
| Quote: | Originally posetd by a123x
I've recently been experimenting with making alkoxides by the electrolysis of solutions of NaBr in methanol or ethanol. In one chamber of the
electrolytic cell the alkoxide is formed and in the other, a solution of bromine in alcohol is formed. This solution of bromine in alcohol reacts
readily enough with iron powder to produce FeBr3. The reaction isn't very reapid with Fe but does get fairly warm. I figure aluminum should react
well enough with such a bromine solution. The alcohol can then be distilled off to leave the anhydrous AlBr3. |
I think AlBr<sub>3</sub> would react with the alcohol to produce the aluminum alkoxide and HBr since alcohol is protic, similar to the
reaction with water.
|
|
|
verode
Harmless
Posts: 32
Registered: 22-3-2005
Member Is Offline
Mood: No Mood
|
|
| Quote: | Originally posted by blip
| Quote: | Originally posetd by a123x
I've recently been experimenting with making alkoxides by the electrolysis of solutions of NaBr in methanol or ethanol. In one chamber of the
electrolytic cell the alkoxide is formed and in the other, a solution of bromine in alcohol is formed. This solution of bromine in alcohol reacts
readily enough with iron powder to produce FeBr3. The reaction isn't very reapid with Fe but does get fairly warm. I figure aluminum should react
well enough with such a bromine solution. The alcohol can then be distilled off to leave the anhydrous AlBr3. |
I think AlBr<sub>3</sub> would react with the alcohol to produce the aluminum alkoxide and HBr since alcohol is protic, similar to the
reaction with water. |
`Try with dry NH4Cl + Al + heating
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
