Development and application instances of vacuum stirring evaporation technology of titanium tetrachloride slurry
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摘要: 为实现泥浆中四氯化钛及有价金属的高效回收利用，进行了四氯化钛泥浆真空旋转蒸发试验，并设计了真空搅拌蒸发系统。利用余热蒸汽加热四氯化钛，螺杆真空泵组提供较高真空度，搅拌桨叶对泥浆进行搅拌，所得四氯化钛干粉含湿率低于1%，四氯化钛回收率达99%，有效解决了四氯化钛泥浆难处理及泥浆中有价金属难回收的问题。且该系统运行对环境友好，设备运行效率高，自动化程度高，适用于大规模的四氯化钛生产。Abstract: In order to realize the efficient recovery and utilization of titanium tetrachloride and valuable metals in the slurry, a vacuum rotary evaporation experiment and vacuum stirring evaporation system for titanium tetrachloride slurry were designed. This paper, used the waste heat steam to heat the titanium tetrachloride, the screw vacuum pump set provided a higher vacuum degree, and the stirring blade stirred the slurry. The moisture content of the obtained dry titanium tetrachloride powder was less than 1%, and the recovery rate of titanium tetrachloride was 99%, effectively solving the complex treatment problems of titanium tetrachloride slurry and difficult recovery of valuable metals in the slurry. The system was environmentally friendly, with high operation efficiency and automation, and was suitable for large-scale titanium tetrachloride production.
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Key words:
- titanium tetrachloride /
- slurry /
- vacuum evaporation /
- airtight stirring /
- waste heat steam
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图 2 四氯化钛沸点与蒸气压的关系
Figure 2. Relationship between the boiling point of titanium tetrachloride and the vapor pressure
图 3 四氯化钛回收率与油浴温度的关系
Figure 3. Relationship between the recovery rate of titanium tetrachloride and the temperature of the oil bath
图 4 真空蒸发试验清液分离效果
Figure 4. The separation effect of clear liquid in the vacuum evaporation experiment
图 5 真空蒸发试验固体颗粒物分离效果
Figure 5. The separation effect of solid particles in the vacuum evaporation experiment
图 6 四氯化钛泥浆真空搅拌蒸发技术方案
Figure 6. Technical scheme of titanium tetrachloride slurry vacuum stirring and evaporation
图 7 四氯化钛泥浆蒸发得到固体粉末样品
Figure 7. Titanium tetrachloride slurry evaporates to produce a sample of solid powder
图 8 泥浆蒸发回收得到四氯化钛样品
Figure 8. The mud evaporates and is recovered to produce a titanium tetrachloride sample
图 9 泥浆真空蒸发试验固体颗粒物粒度分析
Figure 9. The particle size analysis of solid particles in the mud vacuum evaporation experiment
表 1 真空蒸发时间对四氯化钛回收率和固体含湿率的影响
Table 1. The effect of vacuum evaporation time on the recovery rate of titanium tetrachloride and solid moisture content
蒸发时间/
minTiCl4
回收率/%固体含
湿率/%蒸发时间/
minTiCl4
回收率/%固体
含湿率/%0 0 73 50 99 2.9 10 65 48 60 99.2 2 20 90 21 90 99.3 1.1 30 96 11.1 120 99.5 1 40 98 6.2 
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表 2 四氯化钛泥浆蒸发后固体颗粒物含量
Table 2. Solid particles content after evaporation of titanium tetrachloride slurry
% 试样 TiO2 Al2O3 TFe SiO2 V2O5 ZrO2 Nb2O5 冷凝泥浆 3.1 15.1 10 8.84 0.7 36.94 8.9 精制泥浆 5.4 17.1 16.6 12 5.3 21.8 1.6
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