Sciencemadness Discussion Board

Titanium tetrabromide synthesis

plante1999 - 8-6-2011 at 14:38

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]

The WiZard is In - 8-6-2011 at 19:03

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).



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.

mewrox99 - 8-6-2011 at 21:58

Maybe you could try DCM as a solvent. It's available online and some hardware stores have it

The WiZard is In - 9-6-2011 at 07:42

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).



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.







hkparker - 9-6-2011 at 14:04

Quote: Originally posted by mewrox99  
Maybe you could try DCM as a solvent. It's available online and some hardware stores have it


exactly like the syntesis of SnI4, or TiI4

blogfast25 - 10-6-2011 at 04:49

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. :)

plante1999 - 10-6-2011 at 08:54

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.

blogfast25 - 10-6-2011 at 09:44

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.

plante1999 - 17-6-2011 at 04:15

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]