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四氯化钛是生产海绵钛的原料,是钛产业链中的重要中间产品,其中的VOCl3会影响海绵钛O含量和布氏硬度,因此,粗四氯化钛除钒后方可使用。铝粉除钒是主流除钒工艺,除钒物质是TiCl3浆液,其质量对精四氯化钛质量影响较大。我国尚未系统掌握TiCl3浆液制备方法,导致铝粉除钒效果和运行稳定性差。计算了TiCl3浆液制备过程热力学性质;研究了铝粉悬浮液浓度、氯气通入量、最高温度停留时间、冷凝物处理方式和Cl2、N2控制方法等对TiCl3浆液制备过程及质量的影响,得到了较优工艺参数,开展了稳定试验。结果显示:铝粉先与氯气反应,后与四氯化钛反应生成TiCl3·0.33AlCl3;TiCl3浆液制备较优工艺参数为:铝粉悬浮液浓度1.1-1.4%(质量百分含量);氯气加入量按铝粉量控制,Cl2/Al(质量比)为0.7-1.1;最高温度停留时间6-8min;氮气压力170-200kPa,流量为5-7m3/h,氯气压力为120-150kPa,流量为8-10m3/h。采用优化工艺参数制备的TiCl3浆液质量良好,TiCl3含量8.9-10.1%,AlCl3含量3.5%-4.2%,可将粗四氯化钛中VOCl3含量从0.15-0.20%降低至0.0003%。
Titanium tetrachloride is the raw material for the production of titanium sponge and is an important intermediate product in the titanium industry chain. VOCl3 affects the content of O and the Brinell hardness of titanium sponge. Therefore, the crude titanium tetrachloride can be used only after vanadium addition. In addition to vanadium powder is the mainstream of vanadium removal process, in addition to vanadium material is TiCl3 slurry, the quality of the quality of fine titanium tetrachloride greater impact. China has not yet systematically master the preparation of TiCl3 slurry, resulting in vanadium addition to vanadium effect and poor stability. The thermodynamic properties of TiCl3 slurry preparation process were calculated. The effects of aluminum powder suspension concentration, chlorine feed rate, maximum temperature residence time, condensate treatment method and Cl2, N2 control methods on the preparation process and quality of TiCl3 slurry were studied. Better process parameters, to carry out a stable test. The results showed that the reaction between aluminum powder and chlorine gas first reacted with titanium tetrachloride to form TiCl3 · 0.33AlCl3. The optimal technological parameters of preparation of TiCl3 slurry were as follows: aluminum powder suspension concentration 1.1-1.4% (mass percentage); chlorine addition The amount of aluminum powder control, Cl2 / Al (mass ratio) of 0.7-1.1; the maximum temperature residence time of 6-8min; nitrogen pressure 170-200kPa, the flow rate of 5-7m3 / h, chlorine pressure of 120-150kPa, flow rate of 8-10m3 / h. The TiCl3 slurry prepared by optimizing the process parameters has good quality, the content of TiCl3 is 8.9-10.1%, the content of AlCl3 is 3.5% -4.2%, the content of VOCl3 in the crude titanium tetrachloride can be reduced from 0.15-0.20% to 0.0003%.