metalresearcher
National Hazard
Posts: 758
Registered: 7-9-2010
Member Is Offline
Mood: Reactive
|
|
Finally I got K metal from KOH + Mg
Still tiny amounts but it is the beginning. I have to improve the shielding of the retort after cooling it down.
<iframe sandbox width="425" height="349" src="http://www.youtube.com/embed/qxS9uKvHWks?hl=en&fs=1" frameborder="0"
allowfullscreen></iframe>
|
|
Adas
National Hazard
Posts: 711
Registered: 21-9-2011
Location: Slovakia
Member Is Offline
Mood: Sensitive to shock and friction
|
|
Very nice. The only problem is, that the reaction is very fast. Next time you can try to purify the K by melting in inert gas.
|
|
cyanureeves
National Hazard
Posts: 744
Registered: 29-8-2010
Location: Mars
Member Is Offline
Mood: No Mood
|
|
congrats! and boy you are stubborn,with as many attempts from the start with sodium and now potassium,you were bound for success. a taller oil can
should trap more metal dont you think? the last video with the huge fireball would have scared me enough to stop further experimenting and so i have
no kalium. i think kalium means balls.
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
I have always wondered why argon is always used as the "inert" atomsphere for storing potassium. Would not nitrogen work instead? I think perhaps
since it is common knowledge that magnesium can burn in nitrogen, everyone just automatically assumed that potassium would also be reactive towards
nitrogen, when in fact it is not.
Nitrogen actually can dissolve in molten sodium without reaction, even at 500degC. Na3N is only formed if the two elements are subject to
electric discharge under low pressure.
Phase Diagram Evaluations, N-Na (Nitrogen-Sodium) System
James Sangster
[Edited on 12-10-2011 by AndersHoveland]
I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
|
|
fledarmus
Hazard to Others
Posts: 187
Registered: 23-6-2011
Member Is Offline
Mood: No Mood
|
|
Mostly, argon is used because it is heavier than air and is a little better about staying put. Nitrogen is just a touch lighter than the average (air
being 78% nitrogen and 21% oxygen), and is lighter than the oxygen in the air, so a small leak will allow oxygen to seep into your container. Helium
as an inert gas is pretty much useless - it escapes rapidly through the tiniest spaces.
|
|
Chemistry Alchemist
Hazard to Others
Posts: 403
Registered: 2-8-2011
Location: Australia
Member Is Offline
Mood: No Mood
|
|
alot of the K would of burned up in the flash when the reaction proceeded, there was a noticeable colour change when in the presents of Potassium...
is there a way to hold it? and then once the reaction is done, let the pressure out and then open it up? im guessing that then the reaction goes off
it releases some gas... so you could see if the reaction proceeded when then pressure in the vessel increased... or wouldn't this work well? just a
guess
|
|
quicksilver
International Hazard
Posts: 1820
Registered: 7-9-2005
Location: Inches from the keyboard....
Member Is Offline
Mood: ~-=SWINGS=-~
|
|
This thread doesn't belong in the Energetic Materials section of the Forum; therefore moved to General Chemistry.
|
|
quicksilver
|
Thread Moved 12-10-2011 at 06:14 |
blogfast25
International Hazard
Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline
Mood: No Mood
|
|
This method is like flogging a dead horse. Why make tiny amounts of basically irrecoverable potassium, good only for showing that there is some, when
you can make appreciable quantities of neat, clean metal with a small conical flask, a primitive cooler (reflux), a sand bath and some (mostly) OTC
chemicals? See the relevant potassium ‘synthesis’ thread…
But if you do want to improve things, try recovering the slag/metal mix and treat it with kerosene (or any inert hydrocarbon solvent). Some hours of
jiggling the suspension at 100 C or more may yield some actual K nuggets. Recovering these you can merge them into larger ones, once you’ve
separated them from the MgO.
|
|
blogfast25
International Hazard
Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by Chemistry Alchemist | alot of the K would of burned up in the flash when the reaction proceeded, there was a noticeable colour change when in the presents of Potassium...
is there a way to hold it? and then once the reaction is done, let the pressure out and then open it up? im guessing that then the reaction goes off
it releases some gas... so you could see if the reaction proceeded when then pressure in the vessel increased... or wouldn't this work well? just a
guess |
KOH + Mg === > K + MgO + 1/2 H2
For each mol of K formed, 1/2 mol of H2 is formed. In standard conditions that's about 11 L of H2 (per mol of K), at higher temperatures, apply the
Ideal Gas Laws. Hard to keep a lid on, except with a proper bomb (pressure resistant) reactor. Don't try this at home!
Containing the reaction products in a bomb type reactor would almost certainly lead to potassium hydride (KH) being formed: K +1/2 H2 === > KH
|
|
metalresearcher
National Hazard
Posts: 758
Registered: 7-9-2010
Member Is Offline
Mood: Reactive
|
|
On a German forum I posted the result as well and some advised me to 'moderate' the reaction by mixing it with MgO. I don't have MgO but I have silica sand normally
used for a bird's cage (from a pet supply shop) which I can mix with the KOH + Mg. This mixture I will fill into the retort and heat to red hot and
capture the K vapor to condense / freeze into lamp oil.
@cyanureeves : Thank you ! My first attempts a year ago with the 1200oC furnace were unsuccesful just because of the fact that the mild steel retorts
burned out and the Na vapor leaked out.
The Mg methos requires a lot lower temps which do not damage the retort.
[Edited on 2011-10-12 by metalresearcher]
|
|
phlogiston
International Hazard
Posts: 1379
Registered: 26-4-2008
Location: Neon Thorium Erbium Lanthanum Neodymium Sulphur
Member Is Offline
Mood: pyrophoric
|
|
Heating Mg + SiO2 will give you magnesium silicide. An often performed demonstation experiment is to prepare this compound and drop chunks of it in
hydrochloric acid, will will yield silane gas. Bubbles of this explode with audible pops when they come into contact with air.
I can tell you are Dutch. I don't have MgO, but I have a few kg of ZnO pigment that I was planning to discard anyway, if you think it could be of use
to you, let me know. I am not sure if ZnO may perform a thermite-like reaction with Mg metal, though, and any K formed would probably react with the
ZnO to Zn metal, so I suspect it is not a good choice for this purpose.
[Edited on 13-10-2011 by phlogiston]
[Edited on 13-10-2011 by phlogiston]
-----
"If a rocket goes up, who cares where it comes down, that's not my concern said Wernher von Braun" - Tom Lehrer
|
|
blogfast25
International Hazard
Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by metalresearcher | On a German forum I posted the result as well and some advised me to 'moderate' the reaction by mixing it with MgO. I don't have MgO but I have silica sand normally
used for a bird's cage (from a pet supply shop) which I can mix with the KOH + Mg. This mixture I will fill into the retort and heat to red hot and
capture the K vapor to condense / freeze into lamp oil.
[Edited on 2011-10-12 by metalresearcher] |
Phlogiston is entirely right: silica won’t do at all here, it’s simply not inert enough.
The only chemicals that realistically can be used here to temper the reaction are fluorite (CaF2) and cryolite (Na3AlF6). These are commonly used,
especially CaF2, as adjuvants in commercial thermite reactions because they are totally inert in the conditions of the reaction: Mg cannot reduce
either CaF2 or Na3AlF6.
[Edited on 13-10-2011 by blogfast25]
|
|