采用熔盐蒸馏法,以氯化物熔盐为加热介质,利用四氯化钛沉淀泥浆中TiCl4与其他氯化物的沸点差异,通过蒸发回收沉淀泥浆中的TiCl4并通过蒸馏试验,考察了氯化物熔盐种类、蒸馏温度、蒸馏时间及沉淀泥浆与熔盐比例对泥浆中Ti,Nb和A1蒸发率的影响,并对熔盐蒸馏残渣进行了分析和表征。实验结果表明:NaCl-AlCl3络合物熔盐是最佳的蒸馏介质,其不仅可有效提高蒸馏过程的传热和传质,还可与沉淀泥浆中的AlCl3反应而减少Al的蒸发;试验得到最佳的蒸馏温度和蒸馏时间分别为180℃和40min;蒸馏过程中泥浆与熔盐比例不宜超过2。在最佳工艺条件下,Ti的蒸发率为99.6%,Nb和A1的蒸发率分别为2.3%和1.5%,试验结果表明采用NaCl-AlCl3络合氯化物熔盐为蒸馏介质,通过蒸馏可有效回收粗四氯化钛沉淀泥浆中的TiCl4。蒸馏得到的残渣主要成分为Na,Al,C1和O,可采用真空蒸馏的方法回收其中的氯化物,实现熔盐的循环利用。
TiCl4 was recovered from the slurry formed in raw titanium tetrachloride by molten salt distillation due to the distinct differ- ence of boiling point. Factors affecting the evaporation of Ti, Nb and Al including species of molten salt, distillation temperature, dis- tillation time and slurry to molten salt ratio in distillation experiments were studied at different conditions, meanwhile, the distillation residues were detected. The results showed that NaCl-AlCl3 was the optimum distillation media for the evaporation of TiCl4 from the slurry; the molten chlorides not only raised the heat and mass transfer efficiency in the distillation, but also reacted with the slurry which reduced the evaporation of Al in the slurry ; the best distillation temperature and time were 180 ~C and 40 min, respectively. The results also indicated that the slurry to molten salt ratio should not exceed 2 in the process of distillation. Under optimal conditions, the evaporation ratio of Ti, Nb and Al were 99.6% , 2.3% and 1.5% , respectively, which indicated that TiCl4 in the slurry could be recovered effectively by molten salt distillation. The main constituents of the residue obtained after distillation were Na, Al, Cl and O, which could be recovered by vacuum distillation and returned to distillation process.