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Registered Member #8
Joined: Thu Feb 02 2006, 04:34AM
Location: Harlowton, MT, United States
Posts: 214
Well I've done small scale experiments with the process, now here I go with the real deal. The first step is to sulfate the scrap lead. I do this by setting up a water cooled battery of cells with electrodes made from the scrap lead cast into narrow strips and bent over. Each cell contains more than enough sulfuric acid to react with the part of the electrodes hanging down into the cells. I am applying about 2.5VAC per cell (8 cells in series in this case) and they draw 15-20A. This is roughly equivalent to charging and discharging a lead acid cell 60 times per second, and it rapidly sulfates the alloy.
The insoluble lead sulfate falls off and collects at the bottom of the cell. Tin sulfate is somewhat soluble and remains in solution. When the salts are removed and washed, the precipitate can then be washed with sulfuric acid to remove antimony sulfate as it is insoluble in water but soluble in acids.
The next step is to smelt each of the metal sulfates separately with carbon to obtain the pure metals. Tin sulfate decomposes with the release of sulfur trioxide so sulfuric acid can be regained rather directly from that. The smelting of the lead sulfate evolves CO or CO2 and SO2, for example PbSO4 + 2C --> Pb + 2CO + SO2. The Contact Process can then be applied to this gas mixture, when still hot, catalytically oxidizing it to SO3 to regain the remainder of the sulfuric acid. With an excess of compressed air is added into the gas, I intend to use a steel pipe filled with vanadium pentoxide powder with another tube dipping into it, heated to about 500°C, with the outlet restricted by a needle valve until the reaction pressure reaches about 100psi.
Registered Member #193
Joined: Fri Feb 17 2006, 07:04AM
Location: sheffield
Posts: 1022
I wouldn't bother with that high a pressure. Also the SO2 oxidation works better at lower temperatures and is exothermic. You may need to think about cooling. Also, I'm not sure about V2O5 but lead is often a good catalyst poison
Registered Member #8
Joined: Thu Feb 02 2006, 04:34AM
Location: Harlowton, MT, United States
Posts: 214
Thanks for the info. Any idea what pressure/temperature I could get away with? I doubt cooling will be a issue since I will be adding quite an excess of air for the oxidation. I'm not quite sure how I will balance it with the smelting rate, as I don't really even have a way to measure or guess the gas flow rate from either the smelter or the compressor. That's the part that has me the most bothered.
Lead contamination should not be a problem as I will have extensive piping (maybe a goose-neck trap) between the smelter and the catalyst tube.
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Separating and Refining Scrap Lead
