plante1999
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Titanium tetrabromide synthesis
Today I made a successfull synthesis of TiBr4 , when i was starting in inorganic titanium chemistry i was thinking that make easily an anydrous IV
titanium compound was almost imposible (think to TiCl4). The synthesis is very easy but is very ineficient (about 23% theorical yield).
do this outside!
short of my synthesis , i will made a revised version with picture if i get 60% theorical yield).
Chemical:
Bromine , dried with H2SO4
Titanium piece 99.99% (my last piece of Ti...)
Liquid butane fuel (very poor man liquid nitrogen)
Chloroform triple distilled
material:
large test tube
teste tube to fit inside the first test tube but not to small to fall into the first one.
propane torch (or 1000-1300 degree c heat source)
test tube clamp
experimentals:
take a small amount of bromine and drop it in the large test tube, take the clamp to hold the test tube.
fill your small test tube with L butane (i know it could burn but with test i can confirm it doesn burn)
heat with a torch the Ti piece to white glow ( it will fume) and drop it in the bromine IMEDIATLY put the L butane filled test tube, run away. waith
and ad 5ml of CHCl3 to disolve the tetrabromide.
lets it evaporate in a watch glass and store it in amber vials.
improuvements:
find a better solvent than CHCl3 , almost all the TiBr4 doesn disolve so this could be a great improuvement.
thanks
[Edited on 8-6-2011 by plante1999]
[Edited on 8-6-2011 by plante1999]
[Edited on 8-6-2011 by plante1999]
[Edited on 8-6-2011 by plante1999]
[Edited on 8-6-2011 by plante1999]
[Edited on 8-6-2011 by plante1999]
I never asked for this.
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The WiZard is In
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Quote: Originally posted by plante1999  | | Today I made a successfull synthesis of TiBr4 , when i was starting in inorganic titanium chemistry i was thinking that make easily an anydrous IV
titanium compound was almost imposible (think to TiCl4). The synthesis is very easy but is very ineficient (about 23% theorical yield).
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This interest me only to the extent that I would mention in passing —
synthesis of TiB4 is in Brauer (the book is in the forms
library). My Collective Index for Inorganic Syntheses sez
it dobe in 2:114, 6:60 and 9:46.
2:114 uses TiO2, C, and Br2.
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mewrox99
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Maybe you could try DCM as a solvent. It's available online and some hardware stores have it
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The WiZard is In
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| Quote: Originally posted by plante1999 | | Today I made a successfull synthesis of TiBr4 , when i was starting in inorganic titanium chemistry i was thinking that make easily an anydrous IV
titanium compound was almost imposible (think to TiCl4). The synthesis is very easy but is very ineficient (about 23% theorical yield).
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O. Ruff and F. Eisner made it....
http://tinyurl.com/3hnf2zg
I used this as it saves me the trouble of retyping/scanning
my copy.
R&E Ber. 41. 2260, 1908.
Make titanous bromide -
http://tinyurl.com/3obxtm5
A. Stähler, Ber. 37. 4409, 1904
Said to be soluble in dry alcohol and ether - yellow liquid.
A Rosenheim and O. Schütte, Zeit. anog. Chem.,
24. 238, 1900 ; 26. 247, 1901.
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hkparker
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exactly like the syntesis of SnI4, or TiI4
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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blogfast25
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I don’t understand this set up. Dropping bromine onto white heat Ti? You got a death wish?!?
And liquid butane: what’s that all about? n-butane boils at about 0C… And all this in the presence of a full throttle propane flame. Madness! I
suspect the butane is some kind of coolant in your set up. Try CaCl2/ice mixes, keep in a freezer: it’ll give you at least - 18 C, safely and w/o
almost any cost. 
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plante1999
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I think you dont understand my set up , i will post a photo this weekend , i ad a white hot ti piece to a small amount of bromine in a test tube with
a test tube filled with L butane that fit inside the first one but DONT fall into the first one as a reflux , the propane flame is about 4 meters away
from the set up...
Atlest i should use CaCl2/ice cooling in place of L butane.
I never asked for this.
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blogfast25
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Yeah, a photo would be nice. I see that you heat the Ti in one place and then drop it onto the liquid bromine, so the propane flame is far from the
butane/bromine.
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plante1999
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here the promised picture:
no more bromine left... and the tiny test tube filled with ice/CaCl2
finnaly the Ti piece is white hot .
and when the reaction is going:
[Edited on 17-6-2011 by plante1999]
[Edited on 17-6-2011 by plante1999]
[Edited on 17-6-2011 by plante1999]
[Edited on 17-6-2011 by plante1999]
I never asked for this.
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