Ba(ClO3)2
Harmless
Posts: 33
Registered: 30-4-2016
Member Is Offline
Mood: No Mood
|
|
Making Thorium metal
we recently obtained some thorium dioxide from tungsten electrodes. We purified it and were left with a white powder.
We were wondering how easy it would be to make thorium metal from this.
After a bit of searching we found it can be made by reducing the ThO2 with calcium.
ThO2 + 2 Ca ==> 2 CaO + Th
How easy would it be to remove the calcium oxide by-product?
We were thinking maybe boiling the resulting slag from the reaction in mineral oil. Would this be an effective way to remove the CaO?
If not, any other ideas.
|
|
|
blogfast25
International Hazard
Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by Ba(ClO3)2  |
How easy would it be to remove the calcium oxide by-product?
We were thinking maybe boiling the resulting slag from the reaction in mineral oil. Would this be an effective way to remove the CaO?
|
Basically, yes.
Very long and detailed thread on Th production, here:
http://www.sciencemadness.org/talk/viewthread.php?tid=29927
|
|
|
Ba(ClO3)2
Harmless
Posts: 33
Registered: 30-4-2016
Member Is Offline
Mood: No Mood
|
|
Thanks
That looks doable. Sadly we only have enough ThO2 for one attempt.
guess we'll just have to plan it really well.
So basically baking stioceiometric amounts of ThO2 and Ca together with a bit of CaCl2
In a steel tube will work?
The thorium sinks to the bottom of the tube and is protected from oxygen. So presumably the thorium would would be in one solid piece?
And one more question. Can thorium be stored under mineral oil like
sodium/potassium?
[Edited on 10-5-2016 by Ba(ClO3)2]
|
|
|
careysub
International Hazard
Posts: 1339
Registered: 4-8-2014
Location: Coastal Sage Scrub Biome
Member Is Offline
Mood: Lowest quantum state
|
|
Look up the Ames Process developed for uranium reduction in a steel "bomb" (sealed vessel). Particularly look for refs on how it was done on the gram
scale. There is a fair amount of literature available on this. Thorium reduction would handled in a similar manner.
What you probably want to do is place your ThO2 and calcium in a small threaded steel pipe which you will seal with a cap (just like a "pipe bomb")
after flushing with inert gas, then heat the bomb up to the reaction temperature in furnace (a small unit like this will not be significantly self
heat).
When reducing uranium they would often add a little iodine as an initiator, but I doubt that would be necessary if you can heat to a high temperature.
The iodine was used in a large bombs were reaction self-heating largely drove it to completion.
Unlike uranium, which melts below the melting temperature of steel, thorium does not. A ceramic vessel would be needed to melt thorium.
[Edited on 10-5-2016 by careysub]
|
|
|
j_sum1
Administrator
Posts: 6220
Registered: 4-10-2014
Location: Unmoved
Member Is Offline
Mood: Organised
|
|
I highly recommend reading Dan Vizine's thread cited by blogfast. It really lets you know what you are in for. I doubt you will find anything
straightforward unfortunately.
|
|
|
Ba(ClO3)2
Harmless
Posts: 33
Registered: 30-4-2016
Member Is Offline
Mood: No Mood
|
|
We have read most of Dan Vizine's thread.
He obtained the thorium in powder form. We think this would probably be the form we made as well.
So based on Dan vizine's work and the information careysub provided we are thinking on doing something like this:
Add stoichiometric quantities of ThO2 and Ca mixed intimately into a steel tube ("bomb") flushed with CO2. Seal the tube. Heat the tube to 450 C for
30-60 minutes. Let the mixture cool down then quickly open the "bomb" and empty the contents into dilute acetic acid.
The CaO should dissolve as Ca(CH3COO)2 and the thorium powder should remain undissolved. Filter off the thorium then quickly transfer it to a vial of
mineral oil for storage.
As we understand it thorium is only slowly attacked by water and does not react with acetic acid.
All in all does it sound feasible?
We understand powdered thorium is pyrophoric
Thanks to all you guys
Sorry if we've missed something.
[Edited on 10-5-2016 by Ba(ClO3)2]
[Edited on 10-5-2016 by Ba(ClO3)2]
|
|
|
Ba(ClO3)2
Harmless
Posts: 33
Registered: 30-4-2016
Member Is Offline
Mood: No Mood
|
|
Would CO2 work as an innert gas?
We can get hold of argon but CO2 would be a lot cheaper.
As far as we can tell CO2 does not react with thorium or
Calcium.
|
|
|
blogfast25
International Hazard
Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by Ba(ClO3)2 | Would CO2 work as an innert gas?
We can get hold of argon but CO2 would be a lot cheaper.
As far as we can tell CO2 does not react with thorium or
Calcium. |
Calcium is probably capable of reducing CO2 because:
2 Ca + CO2 ===> 2 CaO + 2 C
... is certainly highly thermodynamically favourable.
Considering the low cost of Ar welding gas today, I think it would be foolish to skimp on that little extra cost of Ar v. CO2.
[Edited on 12-5-2016 by blogfast25]
|
|
|
Ba(ClO3)2
Harmless
Posts: 33
Registered: 30-4-2016
Member Is Offline
Mood: No Mood
|
|
Oh well. Guess we'll have to get hold of some argon.
Thanks. You seem to know a lot.
|
|
|
blogfast25
International Hazard
Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline
Mood: No Mood
|
|
I don't know about that.  Many would dispute it.
Welding argon really isn't expensive. And useful in a variety of other chemical circumstances too...
[Edited on 12-5-2016 by blogfast25]
|
|
|
Ba(ClO3)2
Harmless
Posts: 33
Registered: 30-4-2016
Member Is Offline
Mood: No Mood
|
|
We have found a fairly cheap source of argon and are currently making a pipe-bomb for the reaction.
Thanks to everyone for there help and suggestions so far .
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
