Recovery of copper, antimony and lead tin from crude tin electrolysis anode slime
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 Rough tin electrolytic anode mud treatment process
(1) in the anode mud after drying reverberatory furnace, oxidizing roasting, copper → CuO, tin → SnO 2 at a temperature of 700 ~ 750 ℃, and volatile part of arsenic, antimony.
(2) baking for 40 to 60 mesh sand, 5% to 7% dilute sulfuric acid leaching of copper, the liquid: solid = 2: 1, stirred for 2h, the leaching temperature is 80 ~ 90 ℃. Copper enters the solution as CuSO 4 . After leaching, the liquid contains copper 4.5 to 6
(3) replacing the copper-containing solution to obtain an iron powder with copper powder.
Recycling bismuth:
(1) a dilute sulfuric acid leach residue after the copper, with 8% to 10% diluted hydrochloric acid leaching liquid: solid = 2: 1, the leaching temperature is 90 ~ 95 ℃, stirred for 2 ~ 3H, bismuth into solution was BiCl 3 , the leachate contains 铋 40 ~
( 2 ) The hydrazine-containing solution is hydrolyzed to obtain a BiOCl precipitate. The volume ratio of the water added to the hydrazine solution is 8 to 10 : 1 . The mixture was hydrolyzed and stirred, and allowed to stand for 24 hours after hydrolysis . The obtained BiOCl precipitate contains 65% to 72% Bi , which can be used as a raw material for producing electrolytic ruthenium.
( 3 ) The steps and technical conditions for producing electrolytic ruthenium from BiOCl :
The BiOCl precipitate is slowly added to 10 % to 12 % hydrochloric acid to dissolve into BiCl 3 : liquid: solid = 3 : 1 , and stirred at room temperature, a small amount of potassium chlorate may be added to ensure complete dissolution of the hydrazine. Adding glue at the end of dissolution
The crude BiCl 3 solution is replaced with an iron plate to obtain a sponge crucible; an iron plate can also be used as a cathode and an anode to control current density.
The sponge crucible is melt cast into a rough anode. The sponge is covered with caustic soda or caustic potash at 35 0 ~
Rough electrolytic refining: using HCl-BiC1 3 electrolyte (hydrochloric acid 16 0 ~
( 4 ) The direct yield of the whole process is 78 % to 81 %.
Recycling lead and tin:
(1) hydrochloric acid residue of the secondary component (%) after leaching bismuth: 4 0 ~ 48Sn, 22 ~ 28Pb, 1 ~ 2Bi. Reverberatory furnace smelting reduction with tin, lead, bismuth, reduced to metal. The ratio of smelting ingredients is: secondary filter residue
( 2 ) Rough solder electrolytic refining. Silicon hydrofluoric acid electrolyte, the component (g · L -1) was: total acid 16 0 ~ 180, Sn 2+ 15 , Pb 2+ 10, HBF 4 12 ~ 15, gelatin 0.15, β - naphthol 0.15. The conditions controlled during electrolysis are: current density 6 5 to 70 A · m -2 , electrolyte temperature 3 2 ~
Impurities such as antimony and arsenic remain in the anode slime. This anode mud is the raw material for the tadpole.