Research progress and prospect of comprehensive utilization technology of vanadium extraction tailings from vanadium-titanium magnetite
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摘要: 钒钛磁铁矿提钒尾渣是转炉钒渣提钒的副产品，因含有多种有价元素而极具回收价值。但因目前缺乏有效的利用工艺而大量填埋或堆积，造成资源浪费和环境污染。根据钒渣提钒工艺和化学成分对钒钛磁铁矿提钒尾渣进行了分类，阐述了采用氧化法（包括氧化焙烧、电场耦合H2O2+CaF2浸出法）、直接浸出法（包括酸浸和亚熔盐法）、还原法（包括熔融还原和直接还原）对提钒尾渣中有价元素提取的原理和优缺点，以及作为功能材料用于制备蓄热材料的研究现状。认为酸浸工艺是当前研究的热点，但熔融还原能够同时回收铁、钒、铬、钛，具有综合回收率高、工艺流程短的特点，应用前景较广。指出了当前综合利用工艺存在的问题，提出了火法冶金+湿法冶金+物理分离的耦合技术以及作为热能蓄热材料使用的研究方向，并应加强终渣、废液排放的监管力度和毒性检测的研究，为钒钛磁铁矿提钒尾渣的高值化、无害化综合利用提供参考。Abstract: Vanadium extraction tailings of vanadium-titanium magnetite, as a by-product of vanadium extraction from converter vanadium slag, have great recovery value because of containing many valuable elements. However, due to the lack of effective utilization technology, they are currently being landfilled or stockpiled in large quantities, leading to resource waste and environmental pollution, resulting in waste of resources and environmental pollution. In this paper vanadium extraction tailings of vanadium-titanium magnetite had been classified based on vanadium extraction technology from vanadium slag and their chemical composition. The principle, advantages and disadvantages of extracting valuable elements from vanadium extraction tailings by oxidation method (including oxidation roasting, electric field coupled leaching of H2O2 + CaF2), direct leaching (including acid leaching and submolten salt process) and reduction method (including melting reduction and direct reduction) were described. The current research status of using them as functional materials for preparing thermal storage materials had been discussed. Acid leaching process is considered to be a hot topic of current research. However, smelting reduction can simultaneously recover iron, vanadium, chromium and titanium, featuring a high comprehensive recovery rate and short process, and therefore has a broader application prospect. Then he problems existing in the current comprehensive utilization process were pointed out. And the coupling technology of pyrometallurgy + hydrometallurgy + physical separation was proposed, as well as research directions for their use as solar thermal storage materials. In addition, the supervision of final residue and waste liquid discharge and the research on toxicity detection should be strengthened. It is hoped these introductions can provide reference for the development direction of high value and harmless comprehensive utilization of vanadium extraction tailings from vanadium titanium magnetite.
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图 1 氧化焙烧+酸浸法提取提钒尾渣中的有价元素工艺流程
Figure 1. Process flow for extracting valuable elements from vanadium extraction tailings by oxidation roasting + acid leaching method
表 1 钒钛磁铁矿提钒尾渣主要化学成分及分类
Table 1. Main chemical compositions and classification of vanadium extraction tailings from vanadium titanium-magnetite
% 分类1 Fe2O3 TiO2 V2O5 SiO2 Al2O3 CaO Na2O Cr2O3 MgO MnO 分类2 参考文献 钠化
提钒
尾渣54.90 17.40 0.28 2.71 2.86 0.57 4.23 0.33 0.53 普通型 [1] 35.10 10.62 3.60 15.06 1.95 1.96 7.68 6.60 7.86 高铬型 [12] 47.14 11.95 1.75 20.41 2.18 1.94 6.87 4.32 2.63 4.87 高铬型 [13] 钙化
提钒
尾渣33.24 7.08 1.20 10.97 1.54 15.91 4.70 2.33 6.45 高铬型 [13] 45.50 14.89 2.65 14.51 3.36 6.74 1.53 2.57 4.88 普通型 [3] 73.78 12.39 0.47 1.58 3.76 1.26 0.01 0.73 0.25 普通型 [14] 31.08 11.00 0.66 16.95 2.17 5.66 7.60 2.79 4.75 高铬型 [15] 
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表 2 采用直接浸出工艺对提钒尾渣再提钒的研究对比
Table 2. Comparison of processes for vanadium re-extraction from vanadium extraction tailings by direct leaching process
工艺 钒提取率/% 优点 缺点 常压酸浸 <60 设备简单，处理能力大 钒浸出率较低，酸用量多，腐蚀设备，污染环境 加压酸浸 可达80 工艺流程短，钒浸出率高 对设备要求高，处理能力小 亚熔盐法 可达85 提钒效率高，可以实现钒、铬共同提取 设备投资大，工艺复杂，对环境造成潜在影响
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表 3 还原法回收提钒尾渣中有价元素的研究对比
Table 3. Comparison of processes on recovery of valuable elements in vanadium extraction tailings by reduction method
工艺名称 工艺参数 Fe回收率/% 其它有价金属的处置 V、Cr回收率/% 参考文献 熔融还原 ① >90 V、Cr被还原进入铁水 >90 [33] 提钒尾渣与铬铁矿协同还原熔分 ② 93.49 Cr被还原进入铁水 95.18 [15] 高温直接还原+磁选 ③ 99 V、Cr被还原进入铁水 V：90 Cr：95 [3] CaCO3还原焙烧+磁选 ④ 91.05 TiO2含量为41.75%的含钛渣 [14] 注：①采用电弧炉熔融还原，配碳量为12%～14%，碱度为1.0～1.1；②铬铁矿与提钒尾渣配比为5∶1、SiO2添加量为5.08%、配碳量为20.54%、还原熔分时间为35 min；③ 1400 ℃焙烧+磁选；④还原温度1250 ℃、还原时间2 h、还原剂用量为尾渣质量的20%、CaCO3加入量为5% 。
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表 4 钒钛磁铁矿提钒尾渣制备显热蓄热材料的性能研究
Table 4. Study on properties of sensible heat storage materials prepared from vanadium extraction tailings of vanadium titanium-magnetite
密度/(g·cm−3) 导热系数/[W·(m·K)−1] 比热容/[J·(kg·K)−1] 蓄热密度/(kJ·kg−1) 蓄热量/(kWh·kg−1) 1000 kWh所需质量/kg提钒尾渣蓄热材料 2.27～2.551 0.848～1.54 133～7 064 207～255 0.058～0.071 14100 ～17300 常用显热蓄热材料① 1.8～3.0 1.1～7.0 850～ 1400 135～298 0.038～0.083 12100 ～20300 注：①指高温混凝土、镁耐火砖、硅耐火砖、固体氯化钠、砂石。
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表 5 添加钒钛磁铁矿提钒尾渣对相变蓄热材料性能的影响研究
Table 5. Study on the effect of vanadium extraction tailings from vanadium titanium magnetite on the properties of phase-change thermal storage materials
原料 制备工艺 性能 参数及效果 VT+CF+PA+SA+PW 恒温浸渍法和浇注法 蓄热性 ① VT+EG+PW 熔融共混法 稳定性 ② 导电性 ③ ④ 导热性 ⑤ 注：①在三种复合材料CF+PW、CF+PA和CF+SA中分别添加2%、1.6%和0.8%的微米级VT后，材料蓄-放热时间缩短，中心处温度和最高温度的差值分别提高2.7～3.8 ℃、6.4～7.8 ℃和5～11.9 ℃；②进行60次热循环，添加VT前后，复合材料EG+PW的质量损失率由小于0.03％升高到0.08％，添加VT对材料热稳定性影响较小；③成型压力为2～8 MPa时，添加粒度小于45 µm的VT后的材料电阻率均比未添加的小，电阻率随VT添加量增加而减小，说明添加VT可以增强材料的导电性能；④成型压力从2 MPa增加到8 MPa时，电阻率下降率在49％以下，添加VT后复合材料电阻率下降率变大，添加VT可以使复合材料电阻率的压敏性提高；⑤添加1%～3%的微米级VT之后，在4 MPa下压制成型，进行60次热循环，复合材料在不同温度下热导率多数变大，添加微米级VT可以增强复合材料的导热性能。
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