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Author: Subject: The lead salts preparation thread!
S.C. Wack
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[*] posted on 3-11-2011 at 15:23


I'd imagine that chlorine hydrate can be made to react with anything.



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blogfast25
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[*] posted on 5-11-2011 at 03:56


Is 'anything' not a bit too broad? Certain metals will not be attacked appreciably, others so slowly it isn't a practical method.



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[*] posted on 5-11-2011 at 04:00


Has anyone tried to make very pure lead from the salts obtained? For example, a nice lead plate using electrolysis, for element collection.



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[*] posted on 5-11-2011 at 06:49


Quote: Originally posted by Endimion17  
Has anyone tried to make very pure lead from the salts obtained? For example, a nice lead plate using electrolysis, for element collection.


I made lead by electrolysing molten PbCl2 with copper electrodes when I was about 16 but I've no idea how pure it was.




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[*] posted on 5-11-2011 at 11:49


Quote: Originally posted by blogfast25  
Is 'anything' not a bit too broad? Certain metals will not be attacked appreciably, others so slowly it isn't a practical method.


Obviously "made to react" is a small, off-topic comment, (I could have added that I also found PbSO4 in quite small crystals covering the electrodes of a very much dying battery, but this was already pointed out) which does not exactly mean adding water to chlorine hydrate, nor was I speaking of some practical amazing all-inclusive method for dissolving every substance known despite the use of anything. It was an attempt to point out that chlorine and water can be concentrated.

It is already known that no one appreciates brevity and hidden layers of meaning.




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[*] posted on 5-11-2011 at 13:52


You're just to clever by half... ;)



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[*] posted on 6-11-2011 at 07:26


Quote: Originally posted by Endimion17  
Has anyone tried to make very pure lead from the salts obtained? For example, a nice lead plate using electrolysis, for element collection.


For most of my purposes, I don't really need purity, however if I do, I will get Lead dissolved in solution and add a sulfate to the solution to precip. PbSO4. Hot solutions speed this up a lot and produce larger particles. There are very few insoluble sulfate salts, so you should have rather pure PbSO4 after thorough washing. I do believe that BaSO4 is used in small quantities in batteries for seed crystal sites and so that would be the main contaminate. Do note that if sodium is present in moderate or high concentration, this will not work as PbSO4 is soluble in said solutions. From PbSO4 use Sodium Carbonate or Bicarbonate to convert it to PbCO3. From there you can turn it into the product of your choice.

As for plating out Lead, I've done that but I don't know of its purity and it also forms as a loose sponge mass/dendrites that is probably >90% electrolyte. Takes a while to flush out all the electrolyte and dry it before melting. I'm not aware of any method that produces compact deposits outside of a Fluroborate electrolyte. I'd definitely like to know if anyone has gotten a compact deposit besides the use of a Fluroborate electrolyte.
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[*] posted on 6-11-2011 at 13:53


Quote: Originally posted by sxl168  
........... Do note that if sodium is present in moderate or high concentration, this will not work as PbSO4 is soluble in said solutions. From PbSO4 use Sodium Carbonate or Bicarbonate to convert it to PbCO3. ....................


Are you saying that Lead Sulphate is soluble in a solution of Sodium Sulphate?

That does not make sense to me.

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[*] posted on 7-11-2011 at 08:58


My bad for not proofreading before posting. Meant Sodium Chloride there.
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[*] posted on 31-5-2012 at 06:32



Interesting method using sugar to dissolve Lead Acid battery parts here:

http://www.sciencemadness.org/talk/viewthread.php?tid=20175


Lead Nitrate can be prepared with Ammonium Nitrate + Litharge (PbO). The PbO is added to a solution of AN and boiled whereby the Ammonia goes away and Lead Nitrate is left.
This was suggested by Plante1999.
PbO can be obtained from battery PbO2 by calcining (heating strongly) (Plante1999)

Dann2



[Edited on 31-5-2012 by dann2]
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[*] posted on 31-5-2012 at 06:44


Quote: Originally posted by dann2  

Interesting method using sugar to dissolve Lead Acid battery parts here:

http://www.sciencemadness.org/talk/viewthread.php?tid=20175


Lead Nitrate can be prepared with Ammonium Nitrate + Litharge (PbO). The PbO is added to a solution of AN and boiled whereby the Ammonia goes away and Lead Nitrate is left.

Dann2


Thanks. I've been meaning to try that!




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[*] posted on 31-5-2012 at 08:45


Quote: Originally posted by dann2  


Lead Nitrate can be prepared with Ammonium Nitrate + Litharge (PbO). The PbO is added to a solution of AN and boiled whereby the Ammonia goes away and Lead Nitrate is left.

Dann2


I just make this process yesterday, and posted it in PbO2 anode thread this morning, few hour later the process is already in lead salt thread... Please give your reference next time (the reference is me).




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[*] posted on 31-5-2012 at 11:32


Quote: Originally posted by garage chemist  


PbO2, lead dioxide, is very easily made by electrolyzing 20% H2SO4 with two lead electrodes. At the cathode hydrogen is evolved, at the anode PbO2 is formed as a dark brown powder.
The electrolysis can be continued until the entire anode is converted into PbO2. The PbO2 is isolated by filtering the solution, washing and drying the PbO2.

PbO2 is a powerful oxidiser, capable of forming very energetic pyrotechnic mixes, especially with powdered metals.



Excellent method ...Ill need to try this one........I did have some nice chocolate brown Lead (IV) Oxide from and old accumulator, but this sounds a nice reaction.


Ammonium Chloro Plumbate (NH4)2.PbCl6
Adding PbO2 to ICE COOLED concentrated about (30% ish) HCl, PBO2 dissolves without oxidising the HCl to , to form a lead tetra chloride ligand. PbCL4 -2.

If I remember, the solution turns a yellow colour, but if the temp rises the PbCl2 will crystallize, and the unstable-ish ligand releases chlorine....

I think I remember reading that addition of ammonia/ammonium chloride to the ice cooled, Pb Cl4 complex should precipitate out ammonium chloro Plumbate.

PbO2 + 4HCL ----> PbCl4 + H20

PbCL4 + 2Cl- ------> PbCl6 -2

then

2NH4+ ----> PbCl6 -2 -------> (NH4)2.PbCl6

Says if this is added to ice cool H2SO4 then PbCL4 as a heavy yellow oil, hydrolysed with H2O......
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[*] posted on 31-5-2012 at 12:04


Your method is correct, MR A. The PbO2 must be freshly prepared though. (NH4)2PbCl6 is yellow. (NH4)2SnCl6 also exists.



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MR AZIDE
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[*] posted on 31-5-2012 at 12:12



The PBO2 I used was from the mesh on an old accumulator, which may have been contaminated with sulphates.

Ive found a big lump of lead sheet I found years ago, ( about 3mm thick and about 40 by 30 cm.
I going to try electrolysing the H2SO4 with Pb electrodes, to see how much PbO2 I can get........


Dont know what fun can be had with the ammonium chloro plumbate yet.
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[*] posted on 31-5-2012 at 13:15


Quote: Originally posted by MR AZIDE  


Dont know what fun can be had with the ammonium chloro plumbate yet.


Not much. As you wrote, with cold (IIRW), dry, concentrated sulphuric a dark oil of PbCl4 separates out.




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[*] posted on 31-5-2012 at 15:21



I HAVE just electrolyzed a strong NaCl solution with 2 lead electrodes, in a 100 ml beaker.

Using a MOT Tx in reverse, so the supply is 24 V.

Now, PbOH is supposed to be produced which is white, but at first, chlorine gas was being emmited, and the solution quickly has turned orange, then a dark brown precipitate has formed, which is settling at bottom of cell.

IS this precipitate likely to be Lead(IV) Oxide, or is it possible that it is a Lead Chlorate, is the Cl gas was mixing with the solution.? What colour are the LEad chlorate's,? Im assuming they are insoluble.


The elecrolysis, has now after a few mins, stopped producing any Cl gas, the Cathode still fizzing away.., and Now white PbOH is being formed at anode, with no gas evolution.
The current is falling due to the inhibition of the insolubility of the coating of Pb(OH)2,
IF the anode is wiped clean, the current is aver 2 Amp but drops to aony about 40mA.

Question is, why is the brown precip, now not happening, and its Pb(OH)2 .??


Its now disconnected, I think Ill repeat this tommorrow in a U-tube to keep the elecrtodes separate, and see what happens.
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[*] posted on 1-6-2012 at 05:54


Quote: Originally posted by MR AZIDE  

I HAVE just electrolyzed a strong NaCl solution with 2 lead electrodes, in a 100 ml beaker.

Using a MOT Tx in reverse, so the supply is 24 V.

Now, PbOH is supposed to be produced which is white, but at first, chlorine gas was being emmited, and the solution quickly has turned orange, then a dark brown precipitate has formed, which is settling at bottom of cell.

IS this precipitate likely to be Lead(IV) Oxide, or is it possible that it is a Lead Chlorate, is the Cl gas was mixing with the solution.? What colour are the LEad chlorate's,? Im assuming they are insoluble.


The elecrolysis, has now after a few mins, stopped producing any Cl gas, the Cathode still fizzing away.., and Now white PbOH is being formed at anode, with no gas evolution.
The current is falling due to the inhibition of the insolubility of the coating of Pb(OH)2,
IF the anode is wiped clean, the current is aver 2 Amp but drops to aony about 40mA.

Question is, why is the brown precip, now not happening, and its Pb(OH)2 .??


Its now disconnected, I think Ill repeat this tommorrow in a U-tube to keep the elecrtodes separate, and see what happens.


Did you mean Pb(OH)2? The precipitate is PbO2. Lead chlorate would be white, I'm quite sure of it.




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[*] posted on 1-6-2012 at 10:10


had a bit of difficulty in looking up lead chlorates/ perchlorates, but they are freely soluble in water.

I think what happened is the NACL was concentrated enough, that Pb(OH)2 was formed, and immediately reacted with the Cl gas, maybe changing the Pb(OH)2 to PBO2 .
I ve thrown it away now anyway.

I had much more interesting results electrolysing some HCL with Pb electrodes today, which I may post in the technochemistry bit.

here www.sciencemadness.org/talk/viewthread.php?tid=20284

[Edited on 1-6-2012 by MR AZIDE]
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[*] posted on 1-6-2012 at 12:58


Quote: Originally posted by MR AZIDE  

I think what happened is the NACL was concentrated enough, that Pb(OH)2 was formed, and immediately reacted with the Cl gas, maybe changing the Pb(OH)2 to PBO2 .
I ve thrown it away now anyway.


[Edited on 1-6-2012 by MR AZIDE]


Check the half-potentials to see if:

Pb2+ + Cl2 === > Pb4+ + 2 Cl-

... is possible. Dunno off the top of my head, TBH...

Edit: I checked. This oxidation appears not to be thermodynamically favourable, chlorine isn't strong enough. But hypochlorite is and some of that may have formed with your electrolysis.

[Edited on 1-6-2012 by blogfast25]




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[*] posted on 2-6-2012 at 10:21


as long as the Cl2 gas was liberated , the probable Pbo2 was produced, as definately hypochlorite will be being produced.......this oxidised the lead to from +2 to +4, .......

PbO2, Ive just read can be produced by shaking a solution of a hypochlorite with a suspension of Pb(OH)2 in water.
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[*] posted on 2-6-2012 at 10:29


Quote: Originally posted by blogfast25  


Check the half-potentials to see if:

Pb2+ + Cl2 === > Pb4+ + 2 Cl-

... is possible. Dunno off the top of my head, TBH...

Edit: I checked. This oxidation appears not to be thermodynamically favourable, chlorine isn't strong enough. But hypochlorite is and some of that may have formed with your electrolysis.

I had a paper on producing Pb(AcO)4 from Pb3O4, acetic acid and acetic anhydride. The yield could be maximized by oxidizing the remaining Pb2+ with chlorine gas IIRC.




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[*] posted on 2-6-2012 at 10:46


Quote: Originally posted by MR AZIDE  


PbO2, Ive just read can be produced by shaking a solution of a hypochlorite with a suspension of Pb(OH)2 in water.


No need for shaking ;), see the other thread on battery lead and my results. Hypochlorite easily oxidises Pb(OH)2 to PbO2.

[Edited on 2-6-2012 by blogfast25]




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[*] posted on 2-6-2012 at 11:24


I see your source of NAOCl, was bleach.......is this like the cheap stuff you can buy in supermarkets.?

Ive seen like the cheap own brand stuff in the supermarket, and I read the labels just says '' contains sodium hypochlorite'', but it never says what concentration the sodium hypochlorite is.
Ive never got round to buying any to play with.

are most of these thick /thin bleaches( as they call it,) basically NaOCl in plain water?,,,, are there many additives........is the solution colorless of slightly yellow?

If so Id like to try at some point making KClO3 via nurdrage's method........

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[*] posted on 2-6-2012 at 12:10


Quote: Originally posted by MR AZIDE  
I see your source of NAOCl, was bleach.......is this like the cheap stuff you can buy in supermarkets.?

Ive seen like the cheap own brand stuff in the supermarket, and I read the labels just says '' contains sodium hypochlorite'', but it never says what concentration the sodium hypochlorite is.
Ive never got round to buying any to play with.

are most of these thick /thin bleaches( as they call it,) basically NaOCl in plain water?,,,, are there many additives........is the solution colorless of slightly yellow?

If so Id like to try at some point making KClO3 via nurdrage's method........



Get 'no frills' thin bleach: 4 - 5 % NaClO (sodium hypochlorite). Weak concentration, strong oxidiser. Ca(ClO)2 ('pool shock') is 100 % (solid) but harder to get.

Thick = thin + glycerine. Avoid!




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