四氯化钛精制除钒试剂的制备及应用研究  

Preparation and Application of Vanadium Removing Reagent in Refining Crude TiCl_4

作　　者：李亮[1] 李开华[1] 苗庆东[1] 程晓哲[1] 何安西[1] 孙朝晖[1] 

机构地区：[1]攀钢集团研究院有限公司钒钛资源综合利用国家重点实验室,四川攀枝花617000

出　　处：《稀有金属》2015年第7期666-672,共7页Chinese Journal of Rare Metals

基　　金：国家科技部重点基础研究发展计划(973计划)项目(2013CB632606)资助

摘　　要：TiCl4是海绵钛与氯化法钛白的生产原料,粗TiCl4精制除钒是确保TiCl4质量的重要环节。为稳定制备粗钛除钒试剂质量及优化粗钛除钒效果,结合我国攀西地区高钙镁钛渣氯化所得粗TiCl4的原料特点,对粗TiCl4铝粉除钒试剂的制备原理进行了热力学分析,并考察了铝粉含量、氯气浓度、停止通氯温度、反应最高温度持续时间对除钒试剂制备过程的影响,获得了除钒试剂稳定制备的优化工艺参数;同时开展了工艺优化验证实验与除钒应用实验研究。热力学分析结果表明：温度为25~140℃时,Al粉与精TiCl4能够在通氯条件下反应生成低价钛除钒试剂,控制温度为90~150℃时,能使溶于粗TiCl4中的VOCl3转变为不溶于TiCl4的VOCl2沉淀除去。实验研究表明：当铝粉悬浮液中铝含量为30~35 g·L-1,Cl2浓度为85%~90%、停止通氯温度为105℃、反应器内最高温度持续时间为8~10 min时,能稳定制备质量较佳除钒试剂,在最优工艺条件下制备所得除钒试剂中TiCl3含量为8.24%~9.24%,Al Cl3含量为2.67%~3.68%,质量稳定且除钒效果好,该除钒试剂能将粗TiCl4中VOCl3含量由0.0963%~0.1116%降低至0.0003%。Pure TiCl4 is raw material for titanium sponge and pigment grade TiO2 production. Removing vanadium from crude TiCl4 is an important process to ensure the quality of TiCl4. According to the characteristic of crude TiCl4 which was produced from titanium slag with high calcium and magnesium in Panxi region of China,preparation principle of vanadium removing reagent was analyzed from the perspective of thermodynamics to optimize vanadium impurities removal from crude TiCl4 and stablize the quality of vanadium removing reagent. Influences of Al powder content,concentration of chlorine gas,stop temperature of Cl2 and maximum temperature duration preparation process were investigated to obtain the optimal and stable preparation process parameters of vanadium removing reagent. Process optimization and application experiments of vanadium removing reagent were also carried out. Thermodynamic analysis results showed that low valence titanium slurry could be produced when Al powder and Cl2 were added in pure TiCl4 at 25 ~ 140 ℃.VOCl3 dissolved in crude TiCl4 could transform into VOCl2 precipitation which was insoluble to TiCl4 at 90 ~ 150 ℃,and thus VOCl3 was removed from crude TiCl4. Experimental research showed that high quality and stable vanadium removing reagent could be obtained when Al powder content in suspension liquid was 30 ~ 35 g·L- 1,Cl2 concentration was 85% ~ 90%,stop temperature of Cl2 was 105℃,and maximum temperature duration time was 8 ~ 10 min. TiCl3 and Al Cl3 contents in low valence titanium slurry which was produced under optimal conditions were 8. 24% ~ 9. 24% and 2. 67% ~ 3. 68%,respectively. VOCl3 content in crude TiCl4 could be reduced from 0. 0963% ~ 0. 1116% to 0. 0003% after vanadium removing operation.

关 键 词：四氯化钛精制 铝粉除钒 三氯化钛 稳定制备 

分 类 号：TF823[冶金工程—有色金属冶金]