Pages:
1
2
3 |
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
Picture.
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
...On another note, I've been soaking lead bits in strong HCl for the last week or two, occasionally stirring up the gray/white crud, decanting
and drying it. Well here's an odd one, I seem to have a yellow/green coloration to the solution. PbCl2 doesn't dissolve much, and is white
anyway, doubtful that's the culprit. Besides, after letting the acid sit a while, I get a layer on top of clear white acid! There are also a
few drops of the stuff left in the bucket with the lead, it's almost oily in that it seems to be at least partially seperated and floating.
It could be iron or copper ions (though the latter is unlikely with lead metal in solution, though at this pH that would be an equilibrium of Cu in
solution depsite the Pb, no?), but that wouldn't explain the seperation.
I'll take a photo tomorrow...
Tim
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
Alternate PbO method?
KClO3 has low solubility (and as I recall, tends to plate Pb alone), and as I don't have any NaClO3 or KNO3 on hand, I can't really do much
for electrolytic corrosion of lead. So I was thinking, I have a pretty good amount of CuO on hand, let's react that. Thermite won't have
enough energy from Cu > Pb to sustain, so it'll need cooking, but how much? Enough to melt Pb, okay, but what of the CuO, and PbO and Cu
products?
I'm guessing I should melt the PbO, which unfortunately is a powerful flux (see: lead crystal), and being below iron will oxidize it as well. So
that leaves what, tough alumina-glazed crucibles to try?
Also the problem of getting solid PbO as a result, that might be hard to grind...
Oh, and hrm, I suppose I could try sodium acetate. I guess I'll neutralize some and give it a try...
Tim
P.S. ssssss...GRR! This is the only forum that doesn't have ALT+S = send!
|
|
jpsmith123
National Hazard
Posts: 764
Registered: 24-6-2005
Member Is Offline
Mood: No Mood
|
|
Hello Tim,
I'm not sure I understand what you ultimately want to do. Do you want to make PbO2 powder and do something with that, or are you trying to
"anodize" lead or plate another substrate with PbO2?
Regards,
Joe
|
|
Lambda
National Hazard
Posts: 566
Registered: 15-4-2005
Location: Netherlands
Member Is Offline
Mood: Euforic Online
|
|
MANUFACTURING OF LEAD DIOXIDE COATINGS
Please check this out:
MANUFACTURING OF LEAD DIOXIDE COATINGS:
http://mitglied.lycos.de/echem03/
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
Not PbO2, just PbO. Besides then having fixed lead, I'll have oxide for ceramics projects (why of course I'm going to be trying lead glazes
some day). If I want PbO2 I can always dissolve in vinegar and precipitate with bleach (I believe that's the standard method, no?). So I'm
not too concerned about quality (though in the preceeding method, CuO would be a major impurity and would surely color everything I put it in).
Of course I can also cementate, but how much boiling would be needed to complete CuCl2 > PbCl2? But that also wastes even more chemicals, if cheap
ones (HCl, then NaCO3 to ppt).
Tim
|
|
jpsmith123
National Hazard
Posts: 764
Registered: 24-6-2005
Member Is Offline
Mood: No Mood
|
|
You mean there is some use for lead compounds besides electrodes for chlorate/perchlorate cells?!!!
What happens when you decompose (heat) lead acetate? I think I read somewhere that you get PbO... but I could be mistaken.
Regards,
Joe
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
Most likely (hm... Pb(OOCCH3)2 = Pb + 4CO + 3H2?), but that would be a bad waste of good lead acetate which needs PbO (or CuO) to start with in the
first place anyway.
Anyone know exactly how they made red lead? Yeah, heating in a furnace. How *exactly*?
I've only ever made the green suboxide, stirring around a Pb melt.
Tim
|
|
jpsmith123
National Hazard
Posts: 764
Registered: 24-6-2005
Member Is Offline
Mood: No Mood
|
|
Unfortunately I can't find the information, but supposedly the products are PbO, CO2, and H2O (don't forget, you're heating to >300
degrees C in *air*).
Maybe Pb(CH3COO)2 + 4O2 = PbO + 4CO2 + 3H2O
In any case, I haven't tried it, but supposedly you can make Pb(CH3COO)2 from lead and vinegar; you don't have to use PbO, but I've
heard that adding some H2O2 speeds it up.
I don't know how red lead is made, but supposedly to make litharge from lead you have to melt the lead and spray it into the air through a
nozzle.
Here's a link to an article about making lead acetate from vinegar:
http://www.sas.org/tcs/weeklyIssues_2005/2005-06-17/feature4...
[Edited on 25-7-2005 by jpsmith123]
|
|
tumadre
Hazard to Others
Posts: 172
Registered: 10-5-2005
Member Is Offline
Mood: No Mood
|
|
I melted about a pound of lead in a clay pot and just let it get red for about two hours, after it cooled I had about an ounce of blue, brown and red
material. however the lead was contaminated with antimony and a small amount of zinc/tin from my good supply of car batterys. I am interested knowing
if any specific antimony oxides are blue. also will acetic acid react with pb02? I know it wont with pbso4
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
Was it powdery, flakes or an adherent layer on the metal? Blue sounds like interference to me (that is, the oxide layer is on the order of a half
wavelength of red or so).
I tried burning an antimony alloy as well, it made some yellow oxide, which is perhaps better. The leftover metal is soft and reasonably pure (large
crystals), but also hot short (it broke in two on removing it from the mold just after it solidified). I was going to try dissolving this in HCl to
see if I can get SbCl3 out...
Tim
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
Ah, that reminds me, now that I have some NaClO3 on hand I thought I'd take a stab at electrolytic corrosion again.
200g NaClO3 (finally mostly anhydrous as near as I can tell, stuff loves to cake up!) was added to 500g (..500ml..) H2O. Electrolysis was performed
with a 99%+ pure lead anode and some copper wire cathode. About 4V was applied, giving an estimated current of perhaps 5A. Initially, much Pb(OH)2
was produced, but over time, spongy lead formed on the cathode and the anode was oxidized to PbO2. Oxygen bubbles were noted from the
anode.
(Chemical standard of past tense, but it's still running as I type...)
So, um, I've got some voltage here, the anode seems to be turning to PbO2 and not gaining gross [electrical] resistance, and the chlorate solution is
getting oxygen bubbled through it. Surely I am making perchlorate to some extent here!?
Tim
|
|
Pages:
1
2
3 |