采用真空熔炼—真空蒸馏的方法处理焊锡电解阳极泥,在还原真空度20~30 Pa,还原温度为1273 K,还原剂为30%,还原时间1.5 h,蒸馏温度1573 K,蒸馏真空度10^-2~0 Pa,蒸馏时间30 min下,得到了纯度为98.13%的粗锡,粗锡中锑、铋、银的含量降低至0.19%,0.85%,0.82%,大部分的锑、铋进入冷凝物中,实现了锡与锑等有价金属一定程度的分离。真空处理后得到的粗锡可返回锡电解系统生产精锡,得到的冷凝物可作为锑冶炼原料进行利用。
The soldering tin electrolytic anode slime was recycled by carbo-thermal reduction and thermal distillation in low vacuum. The influence of the recycling conditions,including but not limited to the reduction/distillation temperatures and times,reductant content(coke powder) and pressure,on the contents of Sn,Sb,Bi and Ag in the crude Sn ingot and condensates,was theoretically analyzed and experimentally investigated with X-ray diffraction. The results show that the novel technique does a good job in recycling the Sn anode slime. To be specific,reduced at 1273 K for 1. 5 h in 20 ~30 Pa and with a 30%(wt) of coke powder; and distilled at 1573 K for 30 min in 10^-2~0. 0 Pa,the crude Sn ingot contains 98. 13% Sn,and the Sb,Bi and Ag impurity contents decreased to0. 19%,0. 85%,0. 82% of those in the anode slime,respectively. We suggest that the distilled crude tin be a good raw material for Sn-electrolysis and further Sb-extraction.