Sciencemadness Discussion Board - Any lead sulfate reactions?

Any lead sulfate reactions?

acetone - 5-6-2014 at 03:28

Hi,

I'm looking for some reactions involving lead sulfate PbSo4 as one of the reactants. I want to recover lead from its sulfate. Internet is not being helpful with this one. Lead sulfate was salvaged from malfunctioned Sealed Lead acid batteries. Can you help?

Bert - 5-6-2014 at 04:01

Be aware that the battery Lead probably has some Antimony, Strontium and Arsenic additives-

There have been a couple of threads quite recently in beginnings/reagent acquisition about this subject, try using Google to search instead of the site search function?

Searching this string:

sciencemadness.org battery lead sulfate reactions

Gives me this...

https://www.google.com/search?q=sciencemadness.org+battery+l...

[Edited on 5-6-2014 by Bert]

acetone - 5-6-2014 at 05:35

I searched the site but there is no info on how to extract Pb from PbSo4. Perhaps I should try reacting it with NaOH?

acetone - 5-6-2014 at 08:09

I wonder whether trying to displace lead from a water soluble lead salt(like lead nitrate) would work? Perhaps reacting lead nitrate with iron fillings?

CHRIS25 - 5-6-2014 at 08:31

Tin is right above lead in the reactivity series, Tin + Lead sulphate perhaps? Or, maybe try adding more H⁺ ions via another acid such as HCl + Lead sulphate forcing the sulphate and Hydrogen bond?
PbSO₄ + 2HCl = Pb + H2SO₄ + 2Cl

No doubt I might be corrected, welcomed, but this is my best working to the solution if it was me.

It's funny I actually want to make lead sulphate (have tons of lead ingots that I melted) lead crystals are very beautiful.

[Edited on 5-6-2014 by CHRIS25]

UnintentionalChaos - 5-6-2014 at 08:48

As near as I can tell, you have two options.

Aluminothermic reduction of PbSO4 to PbS, which on treatment with something like HNO3 would give Lead nitrate solution.

Now, PbSO4 is highly insoluble, but solubility is always relative. Lead sulfate has a Ksp of 2.53×10^(-8) but PbCO3 is 7.40×10^(-14). This means that Lead (II) sulfate is 342,000 times more soluble than the carbonate. Prolonged boiling of the sulfate with sodium carbonate solution would convert (eventually) all of it to the carbonate. Filter off and react to a soluble lead salt.

A fully charged lead acid battery has plates of lead metal and PbO2, which would be much easier to deal with...

blogfast25 - 5-6-2014 at 12:25

Quote: Originally posted by UnintentionalChaos

As near as I can tell, you have two options.

Aluminothermic reduction of PbSO4 to PbS, which on treatment with something like HNO3 would give Lead nitrate solution.

Highly exothermic as such a reaction would be, its a recipe for blowing Pb compounds into your environment. DON'T DO IT!

Conversion to lead carbonate (or a basic lead carbonate) is much simpler and safer. Then convert to nitrate or acetate.

Lead will be displaced from its solutions by electropositive metals: Zn, Al, Mg, Fe etc.

[Edited on 5-6-2014 by blogfast25]

DraconicAcid - 5-6-2014 at 12:28

Quote: Originally posted by blogfast25

Lead will be displaced from its solutions by electropositive metals: Zn, Al, Mg, Fe etc.

It you want to get it into solution, the merck Index says that it's soluble in sodium hydroxide solution, ammonium acetate solution, ammonium tartrate solution, or concentrated hydroiodic acid. If you dissolve it in NaOH, you should be able to displace it fairly easily with aluminum or zinc.

blogfast25 - 5-6-2014 at 12:34

Quote: Originally posted by DraconicAcid

[It you want to get it into solution, the merck Index says that it's soluble in sodium hydroxide solution, ammonium acetate solution, ammonium tartrate solution, or concentrated hydroiodic acid. If you dissolve it in NaOH, you should be able to displace it fairly easily with aluminum or zinc.

Lead is amphoteric both as plumbous (II) or plumbic (IV), so treating PbSO4 with NaOH should get you sodium plumbite, Na2Pb(OH)4. That should be reducible with Al or Zn. Neutralisation of sodium plumbite with HNO3 or glacial acetic acid should yield lead (II) nitrate ot acetate respectively.

[Edited on 5-6-2014 by blogfast25]

DraconicAcid - 5-6-2014 at 12:41

Quote: Originally posted by blogfast25

If you dissolve lead(II) sulphate in sodium hydroxide, and then neutralize with acid, there will still be sulphate ions present, and your lead(II) sulphate will simply reprecipitate.

blogfast25 - 5-6-2014 at 13:00

Oooops. Haste makes waste.

bismuthate - 5-6-2014 at 13:30

How about using sodium aluminate to neutralize it. I don't believe that the solution would be basic enough to redissolve and lead hydroxide.
Although that may just yield other things that I didn't anticipate such as Al(OH)3.
[Edited on 5-6-2014 by bismuthate]

[Edited on 5-6-2014 by bismuthate]

DraconicAcid - 5-6-2014 at 13:41

Quote: Originally posted by bismuthate

How about using sodium aluminate to neutralize it. I don't believe that the solution would be basic enough to redissolve and lead hydroxide.
Although that may just yield other things that I didn't anticipate such as Al(OH)3.

You want to neutralize the sodium plumbite by adding a weak base?

bismuthate - 5-6-2014 at 13:52

No the PbSO4.
EDIT Also I believe that blogfast's idea would work in the presence of Ba+2.

[Edited on 5-6-2014 by bismuthate]

jock88 - 5-6-2014 at 14:20

"
Now, PbSO4 is highly insoluble, but solubility is always relative. Lead sulfate has a Ksp of 2.53×10^(-8) but PbCO3 is 7.40×10^(-14). This means that Lead (II) sulfate is 342,000 times more soluble than the carbonate. Prolonged boiling of the sulfate with sodium carbonate solution would convert (eventually) all of it to the carbonate. Filter off and react to a soluble lead salt. "

How long would you need to boil. Days perhaps?

DraconicAcid - 5-6-2014 at 14:38

Quote: Originally posted by jock88

"
Now, PbSO4 is highly insoluble, but solubility is always relative. Lead sulfate has a Ksp of 2.53×10^(-8) but PbCO3 is 7.40×10^(-14). This means that Lead (II) sulfate is 342,000 times more soluble than the carbonate. Prolonged boiling of the sulfate with sodium carbonate solution would convert (eventually) all of it to the carbonate. Filter off and react to a soluble lead salt. "

How long would you need to boil. Days perhaps?

Who knows? The rate at which the stuffs dissolves will depend on the size of the lead sulphate particles, how dry they were to begin with, etc. it might be faster to dissolve it in sodium hydroxide, then neutralize the base with sodium bicarbonate.

[Edited on 5-6-2014 by DraconicAcid]

acetone - 5-6-2014 at 21:21

What is likely to be present in a sealed lead acid battery which has been lying discharged for a long time - PbSO4 or PbO2? I salvaged whatever lead I could find from the heap by heating and pouring down the metal. Now I have some black greyish stuff which if heated strongly becomes orange. I suppose thats PbO2?

blogfast25 - 6-6-2014 at 03:38

The discharge reaction for a lead/acid battery is:

Pb(s) + PbO2(s) + 2H2SO4(aq) → 2PbSO4(s) + 2H2O(l)

jock88 - 6-6-2014 at 05:09

Leas salts thread:

http://www.sciencemadness.org/talk/viewthread.php?tid=5490

violet sin - 6-6-2014 at 06:21

electrowinning with sulfamic acid would do well to recover your lead. there is a fair amount of papers on it, but here is one. "Method of extracting metals from spent electric storage batteries": http://www.google.com/patents/US3985630 sulfamic acid can be found as a tile de-hazing etchant, alternative to the volatile HCl. a little tub is like 6$ at the hardware store if they carry it.

http://www.homedepot.com/p/Custom-Building-Products-TileLab-...

Zyklon-A - 6-6-2014 at 11:45

Lead carbonate from lead sulfate:

Attachment: US2152242 Basic Lead Carbonate from Lead Sulfate (1).pdf (274kB)
This file has been downloaded 397 times

chloric1 - 22-12-2024 at 07:08

Quote: Originally posted by Zyklon-A

Lead carbonate from lead sulfate:

That does seem viable. I’m surprised nobody mentioned making sodium plumbite and adding excess 12% sodium
hypochlorite and boil. You will get lead dioxide which might be contaminated with red led and sodium salts. Mix this with 25-30% nitric acid and pure lead dioxide should be left behind. Use directly as a strong oxidizer or simply mix with acetic, nitric, perchloric, or sulfamic acid and reduce with hydrogen peroxide to reduce it to soluble Pb(II).

RU_KLO - 22-12-2024 at 15:25

I transformed some insolubles sulfates to "more insoluble" carbonates.
Barium was the last one (BaSO4 -> BaCO3)

It was done by boiling a solution of the sulfate(with reflux to avoid loosing water - or you can add lost water) with sodium carbonate.

best ratio: 3.5:1 CO3:SO4 (mol) , at least half hour, better 1 hour. (boiling)

in your case: 1 mol PbSO4 to 3.5 mol Na2CO3.

At the end, after filtering and washing the salt 2 or 3 times, you could take a sample (10 mg) of your carbonate and add nitric or acetic acid of any concentration until there is no more bubbling. (Bubbling -> carbonate)
(H2SO4 or HCl does not work because of insoluble lead salts)

As lead nitrate and lead acetate are soluble and you get a transparent solution, any salt left, is not converted sulfate, so you can check how good the convertion was...