Study on the impurities removal process of calcified vanadium liquid by extraction process
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摘要: 以攀钢西昌钒厂的酸性钙化钒液为研究对象,针对其低酸高钒、除杂困难的特点,采用萃取除杂工艺针对性地去除Mn2+、Ca2+、Fe3+阳离子,考察了萃取过程的主要影响因素。确定的最佳萃取参数为:有机相配比20% P204+80% 260#溶剂油,氨水皂化,皂化率100%,萃取剂相比为O/A=2:1,单级萃取时间为5 min,钒液初始pH值为2.9,Mn、Ca的单级萃取率可达到98%以上,萃取后钒液中Mn的含量为0.05 g/L,Ca、Fe、Al的浓度均小于0.1 g/L。Abstract: The acidic calcified vanadium solution from Pangang Xichang Vanadium Plant was the research object in this study. In response to its characteristics of low acidity, high vanadium content, and difficulty in impurities removal, an extraction process was adopted to specifically remove Mn2+, Ca2+ and Fe3+ cations. The main influencing factors of the extraction process were investigated. And the optimal extraction parameters were determined. The organic phase ratio was 20% P204+80% 260# solvent oil with a saponification rate of 100% using ammonium hydroxide. The extractant ratio was O/A=2:1 at the initial pH of vanadium solution of 2.9 for 5 minutes. Under the above conditions, the single stage extraction rate of Mn and Ca reach over 98%. After extraction, the Mn content drops to around 0.05 g/L, Ca, Fe and Al leves are below 0.1 g/L in acidic vanadium solution.
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表 1 酸性钒液主要元素含量
Table 1. Main element content of acid vanadium solution
g/L V Fe Mn Si P Al Cr Ca SO42− NH4+ K Na Mg 23.82 0.03 9.05 0.61 0.03 0.035 0.059 0.903 26.54 2.76 0.165 1.36 1.34 表 2 初始pH为2.9的平衡水相中元素含量
Table 2. Element content in equilibrium aqueous phase with an initial pH of 2.9
g/L 萃取级数 V Fe Ca Mn Al NH4+ Mg Si 一级 22.51 0.022 0.228 6.51 < 0.01 6.34 1.78 0.356 二级 22.25 0.021 0.035 1.57 < 0.01 9.04 1.64 0.347 表 3 萃余液水相静置产生沉淀元素分析
Table 3. Analysis of precipitation elements produced by static settlement of extraction raffinate
% V Fe Si Mn 41.13 < 0.01 < 0.01 0.017 表 4 两级萃取后的钒液中主要杂质含量
Table 4. Element content in equilibrium aqueous phase with 5min extraction
g/L 萃取级数 V Fe Ca Mn Al NH4+ 一级 21.88 0.02 0.05 1.68 0.01 6.68 二级 18.83 <0.01 <0.01 0.05 <0.01 9.27 表 5 萃取剂饱和容量试验
Table 5. Extraction agent saturation capacity test
水相
数量平衡水相/(g·L−1) 水相
pH平衡有机相/(g·L−1) 萃取率/% V Fe Ca Mn V Fe Ca Mn V Fe Ca Mn 1# 23.36 0.01 0.23 5.40 3.61 0.45 0.04 1.34 7.08 1.93 66.67 74.75 40.33 2# 23.62 0.01 0.50 9.89 3.48 0.38 0.08 2.12 5.01 0.84 66.67 44.30 -9.28 3# 22.54 0.02 0.56 11.00 3.32 2.49 0.10 2.78 0.67 5.37 40.00 37.87 -21.55 表 6 反萃液成分分析
Table 6. Composition analysis of backextract solution
g/L V Fe Ca Mn Al 7.28 < 0.01 0.259 58.46 0.172 -
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