蒸馏水解法制备金红石型高纯TiO_2粉体

Preparation of High-purity Rutile TiO_2 Powders via Distillation and Hydrolysis Two-step Method

以四氯化钛(TiCl_4)为原料,液体石蜡为纯化剂,氨水为形核剂,采用蒸馏与水解两步法制备金红石型高纯TiO_2粉体.通过XRF分析样品中的杂质含量;XRD和SEM表征高纯TiO_2粉体的物相组成及形貌特征.结果表明:在化学法除钒过程中,当液体石蜡加入量与TiCl_4原液质量比为1∶100,加热搅拌1 h,反应温度138℃时,除钒效果最佳;提纯后的TiCl_4经水解,于800℃煅烧2h得到近球形的金红石型TiO_2粉体,粒径约1μm,纯度达到99.994 9%.

The high-purity rutile TiO2 powders were prepared by hydrolysis and distillation two-step method,using TiCl4 as raw materials, liquid paraffin as purifier and NH3·H2O as nucleation agent. The impurity content of the sample was analyzed by XRF; the phase composition and morphology character of the high-purity TiO2 powders were investigated by X-ray diffraction technique and scanning electron microscope technique. The results showed that the processing of vanadium removal was the most effective when heated and stirred for 1 h, the reaction temperature was controlled at 138 ℃,and the quality ratio of the liquid paraffin and TiCl4 was 1∶ 100. Purified by liquid paraffin,TiCl4 was forced to precede a hydrolysis reaction. The powders,which were calcined at 800 ℃ for 2 h,had 99. 9949 % purity,and were approximately1 μm spherical particles with rutile phase.