plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
Madness to the extreme, nickel teracarbonyl
I dessided to try to make nickel tetracarbonyl today. I used a equimolar supply of CO2 and CO from sulphuric acid dehydratation of oxalic acid. the
nickel was from 5 cent (canadian 99.9% Ni). I got something, but I'm not sure it is the desired compound, I think I may need to dissolve the nickel,
pyrolise the nitrate to the oxide and use it as a source of nickel, finer nickel.
I had an hoose going very, very far away, and the experiment was done outside.
I never asked for this.
|
|
|
Adas
National Hazard
Posts: 711
Registered: 21-9-2011
Location: Slovakia
Member Is Offline
Mood: Sensitive to shock and friction
|
|
Wow, very nice setup. But powdered Ni would be much better. Just be careful not to poison yourself. Or make iron pentacarbonyl instead.
Rest In Pieces!
|
|
|
garage chemist
chemical wizard
Posts: 1803
Registered: 16-8-2004
Location: Germany
Member Is Offline
Mood: No Mood
|
|
That's not going to work. You need a very pure carbon monoxide stream and freshly reduced nickel powder.
The carbon monoxide should be made from formic acid and sulfuric acid and dried. The nickel is produced by heating its oxide in a stream of hydrogen
and the gas stream then switched to CO.
Nickel tetracarbonyl vapors produce an intensely luminescent flame when fed into the air intake of a bunsen burner with non-luminescent flame. That's
the best way to detect its presence in a gas stream and simultaneously destroy the offgas from the synthesis.
And of course it deposits a nickel mirror when passed through a strongly heated glass tube.
|
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
10g of freshly made Nickel oxide, ready for reduction. I will keep you all updated.
EDIT
I reduced the nickel oxide with large carbon piece with water vapor (to make water gas). It gave me a light gray powder, which I guess is nickel.
[Edited on 4-5-2013 by plante1999]
I never asked for this.
|
|
|
blogfast25
International Hazard
Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by plante1999  | I reduced the nickel oxide with large carbon piece with water vapor (to make water gas). It gave me a light gray powder, which I guess is nickel.
|
Explain that bit a little more?
|
|
|
Eddygp
National Hazard
Posts: 858
Registered: 31-3-2012
Location: University of York, UK
Member Is Offline
Mood: Organometallic
|
|
Well, the purer the nickel, the better. Careful, you don't want to get near nicker tetracarbonyl... take obvious precautions and burn off any flaw.
there may be bugs in gfind
[ˌɛdidʒiˈpiː] IPA pronunciation for my Username |
|
|
plante1999
International Hazard
Posts: 1936
Registered: 27-12-2010
Member Is Offline
Mood: Mad as a hatter
|
|
Well, nickel oxide, and quite large (one cm to two round pieces). Were heated to about 600 C in a tube, and water vapor passed over it. After cooling,
the carbon pieces where sieved and the nickel put aside to make the carbonyl.
I never asked for this.
|
|
|
Wizzard
Hazard to Others
Posts: 337
Registered: 22-3-2010
Member Is Offline
Mood: No Mood
|
|
Why not decompose the tetracarbonyl at 200*C and generate nickel crystals in a continuous process?
One quantity of CO, an amount of nickel in the 'warm' end (to generate 50*C to 130*C), and a hotter top end to decompose the carbonyl (to Ni and CO at
180*C+) in a cycle.
Also, this way, you can cease forming carbonyl at the 'warm' side, and continue decomposing it at the hot side, anbd then purge the device hot and
release nothing but CO in a 'safe' way.
Basically, the Mond process. I have a to-do list including this.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
