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plante1999
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SnI4 and TiI4
today i made this experiment : http://81.207.88.128/science/chem/exps/SnI4/index.html
but with some change , i use CHCl3 instead of CS2 ( i made it frome acetone + sodium hypochlorite 4%). i boil it with a tube outside the lab.
now i want to repeat this experiment but in the place of making tin tetraiodide , i want to make titanium tetraiodide ( if it work i will made a
youtube video about it , tomorow).
solvent: 95-96% CHCl3
iodine 95-98%
and 1/4 to 1/2inch pellet of 99.999% titanium
but the problem is i need titanium powder for this reaction , i tried to grind it with a file but it is nearly impossible.
thanks!!
[Edited on 19-2-2011 by plante1999]
[Edited on 19-2-2011 by plante1999]
[Edited on 19-2-2011 by plante1999]
[Edited on 19-2-2011 by plante1999]
[Edited on 19-2-2011 by plante1999]
[Edited on 20-2-2011 by plante1999]
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plante1999
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solvent: 95-96% CHCl3
iodine 95-98%
and titanium powder
Finally I grind the titanium mecanicly with aluminia oxide sand paper.
the powder was very fine and i ad the conssentred iodine solution ( in CHCl3 ) to it at temperature piece and no reation occured ( not like the Sn +
I2 reaction , arroun 30 second and it is finish) so i heated it , the titanium make tiny effervescence and nothing more after 2 hour wath do you thing
do i need to heat 60degree C with reflux for 1-2hour? or ad a catalist? Al powder ( 2Al + 3I2 -> 2AlI3 --------------------- 3 Ti + 4 AlI3
= 3 TiI4 + 4 Al and the al could be filtered)?
[Edited on 20-2-2011 by plante1999]
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hkparker
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Thanks for drawing my attention to this, hopefully ill do a video on SnI4 for my youtube channel soon.
As for your reaction I'm not so sure it will react. You could try to reflux it but how are you sure iodine solution will attack titanium?, a pretty
corrosion resistant metal. As for it displacing aluminum, check the reactivity series. I always though of titanium as pretty noble but it could just
be passivation that prevents reactions. Let me know how it goes, cool stuff.
My YouTube Channel
"Nothing is too wonderful to be true if it be consistent with the laws of nature." -Michael Faraday
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plante1999
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titanium is a prety reactive element (think pyro) but the dioxide layer protect it ,brauer said that Ti react with I2 , fast at 200degree C. for the
al reactivity sery , brauer said a method with al/ti alloy in iodine solution.
[Edited on 20-2-2011 by plante1999]
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blogfast25
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Quote: Originally posted by hkparker  | Thanks for drawing my attention to this, hopefully ill do a video on SnI4 for my youtube channel soon.
As for your reaction I'm not so sure it will react. You could try to reflux it but how are you sure iodine solution will attack titanium?, a pretty
corrosion resistant metal. As for it displacing aluminum, check the reactivity series. I always though of titanium as pretty noble but it could just
be passivation that prevents reactions. Let me know how it goes, cool stuff. |
Forget the potential series for a minute: that’s very useful for electrochemistry in watery solution but it says very little about reactions like
this one.
Plante is correct in saying that titanium is in fact a very reactive metal: it can be made to burn in air for instance. But it passivates very
efficiently, protecting the metal against corrosion. Commercial Ti metal dissolves fairly easily in hot conc. HCl, to TiCl3 (aq)…
In the Van Arkel and De Boer crystal bar method, very pure Zr or Ti is obtained by decomposing the resp. tetra iodides (ZrI4 or TiI4) on a hot
filament (about 1200 C). New, pure ZrI4 or TiI4 is constantly formed in situ and constantly decomposed to very pure metal at the filament (the I2 is
thus constantly being recycled).
TiI4 is a non-ionic material albeit with probably a sizeable heat of formation, which drives the reaction Ti + 2I2 === > TiI4.
I feel TiI4 probably can be made similar to SnI4 but obtaining or making powdered Ti is hard.
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plante1999
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after testing the Ti react with I2 when refluxed. I will post a video later.
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blogfast25
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Yes, you do that.
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plante1999
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here a qick review of the video that i will made . (this is only a 14 day trial)I will re-try to make it in 14day ( I REALY NEED TO IMPROUVE MY WAY TO
MAKE TiI4). also it as some missing parts.
as you can see at the end it is not like I2 its is dark violet brown-red , with some heating no I2 vapor form but a very dense darck red-brown fume
are formed at high temperature)
<iframe sandbox title="YouTube video player" width="480" height="390" src="http://www.youtube.com/embed/JX1jCrbdivM" frameborder="0"
allowfullscreen></iframe>
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plante1999
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sorry for the double post.
here how i made my solvent , i take very long time to make an usable amount of solvent. I know it is the same music but the first video will be
delleted in 14day , so....
<iframe sandbox title="YouTube video player" width="480" height="390" src="http://www.youtube.com/embed/u8vfuqzG8l8" frameborder="0"
allowfullscreen></iframe>
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hkparker
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I did a video on SnI4 if anyone wants to see, its on my channel.
My YouTube Channel
"Nothing is too wonderful to be true if it be consistent with the laws of nature." -Michael Faraday
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Jor
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Plante1999, I can't see your video on TiI4, because it is private.
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plante1999
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i will change that take note this is just a report of the experiment not the final guide.
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blogfast25
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Yes, you seem to have made TiI4. But your claim of seeing TiI4 vapour is dubious: it has a boiling point of 377 C.
Have you tried hydrolysing some of it?
[Edited on 21-2-2011 by blogfast25]
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plante1999
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i will do tonight. 99 post!!
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plante1999
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sorry for the double post
this ismy 100th post!
my hot plate haet to 900degree C so....but with amiante sheat it it to 500 degree c.
in 13 day i will improuve my methode , i am in working of a self made ( glass bowing with already made glass part) appartus for making TiI4 , TiCl4
and many other inorganic titanium syntesis.
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blogfast25
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'amiante' (wonderful word!) = asbestos.
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plante1999
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sorry for the mistake . i hydrolise te TiI4 and after 2minute a ligth yellow solution is formed i will lets it hydrolise more time.
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blogfast25
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Interesting test could be to add some NaF solution to TiI4, you should get TiF4! Dry mixing TiI4 with NaF should also yield TiF4 with some mild
heating: TiI4 + 4 NaF ---> TiF4 + 4 NaI, driven by the higher HoF of TiF4.
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plante1999
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yes this woul be a good idee but in wath solvent do you think i should use?
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blogfast25
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Try heating an intimate dry mix. TiF4 is highly prone to hydrolysis (HF alert!) so separting the NaI and TiF4 may be difficult unless there exists an
aprotic solvent for NaI...
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Lambda-Eyde
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Acetone?
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blogfast25
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If NaI is soluble in acetone (is it?) then heating an intimate mix of TiI4 with NaF in a closed reactor, followed by leaching out the NaI with acetone
could indeed be a way to make small amounts of TiF4 (quite a nasty substance from what little I've read about it...)
[Edited on 22-2-2011 by blogfast25]
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Lambda-Eyde
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Well, it's the basis for the Finkelstein reaction, so that would make sense.
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blogfast25
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Interesting Lambda-Eyde, never heard of that one before...
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plante1999
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This is a plan of the apparatus i will make for making majority of Ti and Zr compound (i made just Zr and Ti compound. it will cost arround 5dollar us
, for all glass reflux it is cheap.
[Edited on 23-2-2011 by plante1999]
I never asked for this.
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