Source analysis and control technology of impurity Al in titanium sponge
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摘要: 对克劳尔法生产过程海绵钛中Al杂质的来源进行了分析，主要为原料四氯化钛以及原料镁所引入。随后主要对四氯化钛的Al杂质元素的来源进行分析，采取在氯化工序中通水蒸气的措施进行除铝，当通水量在10 kg/h时，就能达到84.22%的除铝效果；同时对原料镁中带入的Al的来源进行分析，并通过加入精炼剂来进行除杂，当精炼剂加入量达到20 kg/t时，除杂效果优异。又因为海绵钛钛坨在生成期间，受反应过程影响，杂质元素Al在海绵钛中分布并不均匀，因此要生产高质量海绵钛，需要从源头进行Al元素的除杂。Abstract: The sources of impurity Al in titanium sponge produced by the Kroll process were analyzed. The impurity Al is mainly derived from titanium tetrachloride and magnesium. Based on the source analysis of Al in titanium tetrachloride, water vapor was introduced for Al removal from titanium tetrachloride during the chlorination process, where 84.22% of Al removal ratio can be obtained at 10 kg/h of water dosage. At the same time, Al in magnesium was removed by adding refining agent, and a favorable effect can be obtained at 20 kg/t of refining agent amount. Influenced by the reaction process for titanium sponge formation, Al is not evenly distributed in titanium sponge. Therefore, it is necessary to carry out Al removal measures from the source materials to produce high-quality titanium sponge.
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Key words:
- titanium sponge /
- aluminum /
- titanium tetrachloride /
- coarse magnesium /
- refining
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图 1 精镁中杂质Al含量随精炼剂加入量变化
Figure 1. Variation of Al content in crude magnesium with the addition of refining agent
表 1 不同通水量对四氯化钛中Al含量的影响
Table 1. Effect of water dosage on Al content in titanium tetrachloride
通水量/ (kg·h−1) 粗四氯化钛罐杂质元素含量/% Al Zr Nb 4 0.003823 0.00064 0.00299 8 0.001557 0.00021 0.00153 10 0.000603 0.00003 0.00080 12 0.000435 0.00001 0.00074 15 0.000366 0.00002 0.00065 
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表 2 常用的精炼剂（钙溶剂）成分
Table 2. Chemical compositions of the refining agent
％ MgCl2 KCl NaCl CaCl2 BaCl2 MgO 38±3 37±3 8±3 8±3 9±3 ≤2
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表 3 加入精炼剂前后精镁中其他杂质元素含量的变化
Table 3. Content of other impurities in crude magnesium before and after adding refining agent
％ Fe Si V Ni Na Cr Sn 添加精炼剂前 0.00987 0.00368 0.00020 0.00174 0.000462 0.00102 0.000116 添加精炼剂后 0.00720 0.00238 0.00021 0.00147 0.000205 0.00104 0.000114
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表 4 海绵钛坨不同位置Al含量
Table 4. Al content in different positions of titanium sponge
取样位置 Al含量/% 1#样 2#样 3#样 平均值 0.0093 0.0158 0.0122 PBT ① 0.0056 0.0114 0.0134 PBT ② 0.0054 0.0130 0.0318 顶部 0.0045 0.0238 0.0193 上左 0.0051 0.0143 0.0164 上中 0.0037 0.0069 0.0055 上右 0.0035 0.0158 0.0101 上部均值 0.0041 0.0123 0.0107 中左 0.0035 0.0071 0.0126 中中 0.0015 0.0055 0.0097 中右 0.0056 0.0063 0.0124 中部均值 0.0035 0.0063 0.0116 下左 0.0057 0.1787 0.0065 下中 0.0063 0.028 0.0108 下右 0.0226 0.037 0.0203 下部均值 0.0115 0.0812 0.0125 底部1 0.011 0.0836 0.0615 底部2 0.0086 0.2412 0.0596 注：PBT表示爬壁钛。
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