A novel Ce(Ⅳ) ion-selective polyvinyl chloride(PVC) membrane electrode based on HDEHP and HEH/EHP as ionophore was successfully prepared. The factors affecting the response of Ce(Ⅳ) ion were investigated, such as membrane composition, internal solution, concentration of SO_4^(2–), and acidity in test solution. The best performance was obtained using the membrane with PVC:DBP:HDEHP:HEH/EHP:OA mass ratio of 75:175:5:5:5. The proposed electrode exhibited a Nernstian slope of 30.44 mV/decade for Ce(Ⅳ) ion over a linear concentration range of 1×10^(–5)–1×10^(–1) mol/L with the detection limit of 9.0×10^(-6) mol/L. The electrode showed stable response within the SO_4^(2–) concentration range of 0.1–1 mol/L and the acidity range of 0.25–1.2 mol/L H+. The proposed electrode showed high selectivity for Ce(Ⅳ) over a wide variety of interfering ions and a fast response time. It was used as an indicator in the potentiometric titration of Ce(Ⅳ) solution with H_2O_2 solution, and could also be used for the determination of Ce(Ⅳ) in real Ce(Ⅳ)-containing aqueous samples.
Magnetic separation of iron in rare-earth tailings was achieved by magnetizing roast process with coal as reductant. Effects of the temperature, carbon to oxygen ratio, and cooling type on magnetic susceptibility and composition of rare-earth tailings were investigated. The results show that roast conditions with the temperature of 650℃, carbon to oxygen ratio of 3.85, and holding time of 2.5 h are in favor of reduction of Fe_2O_3 to Fe_3O_4 when the roasted rare-earth tailings is cooled along with furnace. Under these roast conditions, magnetic susceptibility of rare-earth tailings is 2.36 that is very close to theoretical value(2.33). However, magnetic separation results of iron in rare-earth tailings cooled along with furnace are not satisfactory. Through comparing magnetic separation results of iron in rare-earth tailings cooled by different ways, it is found that water cooling is more favored of magnetic separation of iron in the roasted rare-earth tailings than furnace cooling and air cooling. Grade and recovery of iron in concentrate from rare-earth tailings cooled by water are 45.00%-49.00% and 65.00%-77.50%, respectively.
探究了稀土精矿和稀土尾矿硫酸铵焙烧水浸稀土工艺。研究发现,氟碳铈矿预活化焙烧处理后与硫酸铵混合焙烧,稀土矿物转变为可溶性硫酸稀土盐,预活化焙烧处理有助于提高硫酸铵焙烧过程中稀土矿物向硫酸盐的转变,进而提高稀土浸出率,稀土浸出率最大达到90%。稀土尾矿煤基还原焙烧-磁选铁富集稀土,该过程不仅得到了铁精矿和富稀土渣,尾矿中氟碳铈矿得到活化分解有利于硫酸铵焙烧过程中的物相转变。针对选铁后的富稀土渣分别考虑了硫酸铵配比、焙烧温度和焙烧时间对稀土浸出率的影响。得出富稀土渣最佳硫酸铵焙烧条件:硫酸铵配比为4∶1,焙烧温度350℃,焙烧时间45 min,80℃热水浴浸出时间2 h,浸出液液固比10 m L·g-1,La、Ce、Nd最高浸出率分别为82.83%,76.53%,77.14%。