Study on impurity removal process of titanium tetrachloride produced by boiling chlorination
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摘要: 沸腾氯化因具有生产效率高、成本低、环境污染小、自动化程度高等优点，已成为四氯化钛生产的主流方式。结合双瑞万基钛业公司研究实际，主要讨论了沸腾氯化生产四氯化钛过程中除铝、除钒以及除去四氯化钛中固体颗粒杂质的工艺及研究进展，认为采用氯化炉多级旋风分离系统、离心分离系统及真空搅拌蒸发系统除去四氯化钛中固体颗粒杂质，有机物除钒，配合精四氯化钛中氧碳杂质在线检测技术精准除铝等多项技术措施并用，可以满足高品质四氯化钛的制备需求。并认为有机物除钒和四氯化钛中固体颗粒物绿色环保回收技术将成为四氯化钛制备的主流工艺。Abstract: Boiling chlorination has become the mainstream production method of tetrachloride production due to its advantages of high production efficiency, low cost, little environmental pollution and high automation. Combined with the research practice in Sunrui Wanji titanium industry company, this paper mainly discussed the process of removing aluminum, vanadium and solid impurities in titanium tetrachloride during the process of boiling chlorination production. By combining the on-line detection technology of oxygen and carbon impurities in refined titanium tetrachloride to accurately remove aluminum, we independently developed and designed a chlorination furnace multi-cyclone separation system, titanium tetrachloride centrifugal separation system and vacuum stirring evaporation system to remove the solid particle impurities in titanium tetrachloride, which can meet the requirements of high-quality titanium tetrachloride preparation. And it is believed that the vanadium removal by organic matter and the environmentally friendly recycling technology of solid particles in titanium tetrachloride will become the mainstream production technologies of titanium tetrachloride industry.
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Key words:
- titanium tetrachloride /
- boiling chloride /
- impurity removal process
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表 1 国内外四氯化钛除AlCl3工艺对比
Table 1. Comparison of AlCl3 removal processes from titanium tetrachloride at home and abroad
序号 除AlCl3技术 优点 缺点 1 在粗四氯化钛中加H2O 成本低 H2O加入量比AlCl3理论所需量高10%以上，导致钛损失 2 粗四氯化钛中加90%H2O和10%NaOH溶液 成本低 需增加设备，并在连续生产中控制加入量，容易造成钛损失 3 在粗四氯化钛中加入NaCl（粒度30～400 μm）和H2O，进行适度搅拌，加热到136 ℃左右，形成不溶性的含铝固体化合物被沉降分离除去 减少Ti损失，保持FeCl3的可利用价值，减少HCl产生量 需增加设备，很难解决根据AlCl3含量等比例加入NaCl和H2O的问题，同时NaCl和H2O相互间的比例也是一个问题，AlCl3与（NaCl+H2O）化合速度比较慢，NaCl质量要求比较高 4 气态粗四氯化钛加入NaCl NaCl与AlCl3和FeCl3都要反应生成固体化合物被收集，同时，过量的石油焦粉尘也可以被分离出来 NaCl消耗量比较大，FeCl3不能作为净水剂利用 5 在氯化炉或第一个收尘器内
加入NaCl固体工艺简单，形成挥发度相对的（NaAlCl4）化合物，很容易通过冷凝收尘器被除去。该种方法在高温下，AlCl3和NaCl化合速度很快 床层温度要求850～1100 ℃，可加重
氯化炉内衬侵蚀，或炉内高温烧结
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