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plante1999
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Quote: Originally posted by Mixell  | So is there any acid or a way to make a solution of Ti (lll) ions that later could be added to a solution of NaF?
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heat titanium in HCl and take the TiCl3 with NaF WILL PRODUCE SODIUM HEXACHLOROTITANATE.
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Mixell
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And what about doing it in cold temperatures? But the yield will be quite low...
[Edited on 28-12-2010 by Mixell]
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plante1999
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| Quote: Originally posted by Mixell | | sodium hexachlorotitanate should be soluble (if I'm not mistaken), and the titanium fluoride should sink to the bottom of the flask as it is
insoluble. |
10ml for 35% TiCl3 you get this visible result0.02g of TiF3
undisolvend NaF
yellow sodium hexachlorotitanate
i dont know where is the F2 ion but i think it maked HF.
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Mixell
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And if the sodiumhexachlorotitanate will be formed (in a solution) you will still have half of the titanium turned into TiF3.
Anyway, I'm going to bed, goodnight to you all...
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plante1999
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| Quote: Originally posted by blogfast25 |
Brauer (see our library at the root of this site) describes a simple apparatus with a platinum cooler but the platinum is a little overkill I think.
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i dont find the ducument could you help me to find?
[Edited on 28-12-2010 by plante1999]
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Jor
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Talking about titanium halides, i have been wanting to prepare some TiCl3.6H2O. How oxidation sensitive is this? I was thinking of dissolving some
(1g) titanium powder in hot conc. HCl, followed by evaporation. I read somewhere that at some point one must saturated the solution with HCl gas, and
then cool, wich will result in the desired compound crystallising as purple crystals. 3 questions though, for anyone having experience with it's
preparation:
To what volume should the solution be evaporated before being saturated with HCl-gas (ml solution per gram of Ti).
How oxidation sensitive is this compound. Do I have to work under inert gas constantly or is it not that oxidation sensitive?
Can I also extract the chloride with a solvent, such as ether, followed by easy evaporation (maybe addition of a little ethanol to also easily
evaporate the water in the ether as the azeotrope).
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plante1999
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| Quote: Originally posted by Jor | Talking about titanium halides, i have been wanting to prepare some TiCl3.6H2O. How oxidation sensitive is this? I was thinking of dissolving some
(1g) titanium powder in hot conc. HCl, followed by evaporation. I read somewhere that at some point one must saturated the solution with HCl gas, and
then cool, wich will result in the desired compound crystallising as purple crystals. 3 questions though, for anyone having experience with it's
preparation:
To what volume should the solution be evaporated before being saturated with HCl-gas (ml solution per gram of Ti).
How oxidation sensitive is this compound. Do I have to work under inert gas constantly or is it not that oxidation sensitive?
Can I also extract the chloride with a solvent, such as ether, followed by easy evaporation (maybe addition of a little ethanol to also easily
evaporate the water in the ether as the azeotrope). |
titaiu trichloride coud be worcker in atmosfere for 5-10m without notice.
take 3ml 35-37% HCl and ad 1gram heat de mixture to boiling,lets it colt to room temp re-boil and re cold. i make this for 2,5hours befor saturation
and than use a dessicator bag, the crystal are beautifule i think is the fase A (t ave 4 differant fase witch onli 1 is other than violet.
[Edited on 29-12-2010 by plante1999]
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blogfast25
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Go here:
http://library.sciencemadness.org/library/index.html
Select: ‘Handbook of Preparative Inorganic Chemistry' by Georg Brauer. You’ll find the NH4F procedure there. I think he trick is
to heat the mixture NaF/NH4Cl to only just above the sublimation point of NH4F and to use quite an excess of NaF… The escaping NH4F then drives the
equilibrium to the right...
You made solid TiCl3 hydrate? Blimey, I didn’t even know you could! I had several liters of about 0.1 M TiCl3 (from Ti + HCl) and they stayed fine
for years but eventually did clear up due to hydrolytic oxidation.
[Edited on 29-12-2010 by blogfast25]
[Edited on 29-12-2010 by blogfast25]
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plante1999
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but we talk about 1week in very dry environement.
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plante1999
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and after i store it in dry argon atmosphere.
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plante1999
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| Quote: Originally posted by blogfast25 |
plante1999: what is your interest (end purpose) of these fluorides? TiF3 is a potential route to metallic Ti, via reduction with Mg
or Ca. That's MY interest in BOTH these fluorides...
[Edited on 28-12-2010 by blogfast25] |
after reading some of your post i ave find that you want to make the same fluoride than mine so wath is the apparatus you ave used for making the NH4F
, After some defeat I ave producted impure wihte crystal from this apparatus, I know this isn a chemist apparatus but it is the only apparatus i could
use because i dont ave Pt apparatus(where did you get your apparatus?), A1inch copper end pipe cleaned with HCl with a thick 1/4inch Cu sheet coled
withe snow (-20degren centigrade)yea i live in Canada)Befor using this apparatus I used hdpe sheet coled withe snow but the hdpe melted at the 100
degree centigrade needed.
thanks!
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blogfast25
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| Quote: Originally posted by plante1999 | after reading some of your post i ave find that you want to make the same fluoride than mine so wath is the apparatus you ave used for making the NH4F
, After some defeat I ave producted impure wihte crystal from this apparatus, I know this isn a chemist apparatus but it is the only apparatus i could
use because i dont ave Pt apparatus(where did you get your apparatus?), A1inch copper end pipe cleaned with HCl with a thick 1/4inch Cu sheet coled
withe snow (-20degren centigrade)yea i live in Canada)Befor using this apparatus I used hdpe sheet coled withe snow but the hdpe melted at the 100
degree centigrade needed.
thanks! |
I haven’t made any TiF3 or NH4F yet (as I stated above). Instead of NH4F I’ll be using NH4HF2 which is readily available where I am (UK).
But I did have plans for an ‘NH4F distiller’ based on the information on Brauer and one plan did involve a cooled copper pipe as a collector of
the sublimed NH4F! What about a small copper reactor (a capped off piece of pipe) with a longer, air or water cooled piece of copper pipe screwed onto
it? Heat one end in a sand bath to about 150C, hold the assembly nearly horizontal and the condensed NH4F should be collected in the cool part. Even a
transparent and rigid PP (MP ≈ 165C) tube (with rigorous temperature control!) should work…
If your reagents are sufficiently dry you may also get away with a glass assembly like a long test tube, because very dry HF gas doesn’t attack
glass. That would certainly be worth investigating on a small scale, possibly sacrificing the test tube if it fails…
What ratio of NaF/NH4Cl did you use?
Did you know you can apparently make NH4HF2 from crystallising NH4F, through loss of ammonia?
2 NH4F (aq) === > NH4HF2 (aq) + NH3 (g)
Or so I’ve been told… 
[Edited on 1-1-2011 by blogfast25]
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plante1999
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I dont know that we could make NH4HF2 from crystalising NH4F, bu7t i know it is imposible to crystalise pur NH4F from solution.
: I use 2NaFg for 0.75g of NH4Cl
[Edited on 1-1-2011 by plante1999]
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