Separation and recycling of chloride salts from electrolytic titanium powders by vacuum distillation

Separation and recycling of chloride salts from electrolytic titanium powders by vacuum distillation
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真空蒸馏法从电解钛粉中分离回收氯化物

DOI:
10.1016/j.seppur.2019.116282
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发表时间:
2020-04
影响因子:
8.6
通讯作者:
Dachun Liu
Dachun Liu
中科院分区:
工程技术1区
文献类型:
--
作者:
Liang Li;Fuxing Zhu;Pan Deng;Yaoqiang Jia;Lingxin Kong;Bin Deng;Kaihua Li;Dachun Liu

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熔盐电解法是一种重要的低成本钛粉制备方法。电解钛粉中氯盐的分离回收是提高产品质量、降低生产成本的关键。在这项研究中,开发了一种新的方法来去除和回收氯化物盐杂质(例如,NaCl、KCl)在ETP中的溶解度。对ETP中各组分的饱和蒸汽压进行了理论分析,预测了精馏过程中系统的压力和温度条件。结果表明,随着温度的升高,NaCl-KCl混合盐的汽化作用增强。在实验室立式真空蒸馏炉上研究了NaCl-KCl盐的挥发行为以及系统压力、蒸馏温度和保温时间对分离的影响。实验研究表明,提纯后的钛粉中氯杂质含量可保持在0.04wt. %以下。最佳实验条件为:850 °C,3.5 ~ 4 h,0.1 ~ 1 Pa.这些结果表明,通过使用真空蒸馏,可以以环境友好的方式从ETP中有效地分离和回收氯化物盐。工艺对比和评价表明,真空蒸馏后处理是一种不产生废酸和废水的方法,可以生产出含氧杂质较低的钛粉。
Molten salt electrolysis is an important and low-cost method to prepare titanium powders. The separation and recycling of chloride salts from electrolytic titanium powder(ETP) is quite crucial for the purpose of improving the quality and reducing production cost. In this study, a novel process was developed to remove and recycle the chloride salts impurities (e.g., NaCl, KCl) in ETP by using vacuum distillation. The saturated vapor pressures of components in ETP were theoretically analyzed to predict the system pressure and temperature conditions during distillation process. It shows that the vaporization of the mixture of NaCl–KCl salt strengthens upon increasing the temperature. The volatilization behavior of NaCl-KCl salt and the effects of system pressure, distillation temperature and holding time on the separation were investigated using a lab scale vertical vacuum distillation furnace. Experimental studies indicates that the chlorine impurity content in purified titanium powder can be maintained at a percentage of below 0.04 wt. % under the optimal experimental condition of 850 °C, 3.5–4 h, and 0.1–1 Pa. These results demonstrate that the chloride salts can be efficiently separated and recycled from ETP in an environmentally-friendly manner by using vacuum distillation. The process comparison and evaluation show that the vacuum distillation post-treatment is a method without the generation of waste acid and wastewater, and the titanium powder with a low oxygen impurity can be produced.
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