Effect of sodium chlorite on surface modification and flotation behavior of ilmenite
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摘要: 采用亚氯酸钠对钛铁矿进行表面改性以增强捕收剂的吸附效果。首先从微浮选试验与Zeta电位角度研究了亚氯酸钠改性钛铁矿的机理，结果表明，在油酸钠体系下，经过亚氯酸钠改性后，钛铁矿的回收率有大幅度提升，并在油酸钠浓度1.54×10−4 mol/L、亚氯酸钠浓度80 mg/L、pH=8时达到最佳值，为80.67%。在pH 5～10时，在亚氯酸钠和油酸钠同时作用下，钛铁矿Zeta电位比仅添加油酸钠时更趋向于负值，表明油酸钠在钛铁矿表面吸附量增加。然后以TiO2品位为5.83%的钛铁矿实际矿石为研究对象，通过响应曲面法分析了水玻璃、油酸钠、亚氯酸钠之间的交互作用对钛铁矿浮选过程的影响，并优化了药剂制度，在药剂用量为水玻璃160 g/t、油酸钠110 g/t、亚氯酸钠220 g/t的条件下进行验证试验，可得钛精矿中TiO2品位和回收率为33.92%和86.30%，所得结果与模拟的预测结果接近，表明响应模型具有较高的可靠性。最后通过闭路试验得到钛精矿品位为48.24%，回收率为62.55%的良好指标。Abstract: The surface modification of ilmenite with sodium chlorite was carried out to enhance the adsorption effect of collector. The mechanism of sodium chlorite modification was investigated by microflotation test and zeta potential. The results of microflotation test showed that the recovery of ilmenite in sodium oleate system was greatly improved after sodium chlorite modification, and the optimal conditions were sodium oleate concentration of 1.54×10−4 mol/L, sodium chlorite concentration of 80 mg/L and pH=8. When pH was 5-10, under the simultaneous action of sodium chlorite and sodium oleate, the zeta potential of ilmenite tended to be more negative than that of sodium oleate-treated ilmenite, demonstrating that the adsorption of sodium oleate on the surface of ilmenite was increased. The effects of interaction between inhibitor sodium silicate, collector sodium oleate and oxidant sodium chlorite on TiO2 grade and recovery in titanium concentrate were analyzed by response surface method, and then the reagent system was optimized. Under the conditions of 160 g/t water glass, 110 g/t sodium oleate and 220 g/t sodium chlorite, the actual grade and recovery of TiO2 in titanium concentrate were 33.92% and 86.30%, which were close to the predicted results, indicating that the response model has high reliability. Finally, through the closed-circuit test on this basis, good indexes of titanium concentrate grade 48.24% and recovery 62.55% were obtained.
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Key words:
- ilmenite /
- sodium chlorite /
- surface modification /
- response surface /
- recovery rate
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图 1 不同pH条件下有无亚氯酸钠对钛铁矿回收率的影响
Figure 1. Effect of with sodium chlorite or not on recovery of ilmenite at different pH
图 2 亚氯酸钠浓度对钛铁矿回收率的影响
Figure 2. Effect of sodium chlorite concentration on recovery of ilmenite
图 3 钛铁矿的Zeta电位和pH值之间的关系
Figure 3. Relationship between pH and zeta potential of ilmenite
图 4 TiO2品位与回收率模型预测值与试验值对比
Figure 4. Comparison of model predicted and actually measured TiO2 grade and recovery
图 5 各因素交互作用对TiO2品位影响的响应曲面
Figure 5. Response surface diagram of the influence of interaction of various factors on TiO2 grade
图 6 各因素交互作用对TiO2回收率影响的响应曲面
Figure 6. Response surface diagram of the influence of interaction of various factors on TiO2 recovery
表 1 原矿化学多元素分析结果
Table 1. Results of chemical multielement analysis of raw ore
% TiO2 Fe Al2O3 S MgO CaO SiO2 K Na V2O5 P As 5.83 14.00 20.66 0.02 1.22 0.46 37.86 0.38 0.55 0.09 0.15 <0.1 
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表 2 响应曲面中心组合设计(药剂用量）
Table 2. Response surface center combination design factors and level code
g/t 因素 编码 水平 −1 0 1 水玻璃 A 100 200 300 油酸钠 B 50 90 130 亚氯酸钠 C 0 200 400
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表 3 试验设计与结果
Table 3. Test design and results
试验编号 因素 响应值 A: 水玻璃用量/（g·t−1） B:油酸钠用量/（g·t−1） C: 亚氯酸钠用量/（g·t−1） TiO2品位/ % TiO2回收率/ % 1 300 130 200 32.67 82.69 2 300 90 0 30.75 80.52 3 300 50 200 31.18 80.83 4 100 90 400 33.07 84.48 5 200 90 200 33.78 85.84 6 100 90 0 31.81 83.17 7 100 50 200 32.85 83.47 8 200 50 0 30.52 80.38 9 200 90 200 33.82 86.04 10 200 90 200 33.81 86.24 11 300 90 400 32.87 83.06 12 200 50 400 32.12 83.12 13 200 90 200 33.80 85.96 14 200 130 0 31.42 81.66 15 200 90 200 32.98 85.14 16 200 130 400 33.76 85.28 17 100 130 200 33.57 85.07
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表 4 TiO2品位模型回归方差分析
Table 4. Regression analysis of variance for TiO2 grade
来源 平方和 自由度 均方差 F值 P值 模型 19.76 9 2.20 18.99 0.0004 显著 A 1.83 1 1.83 15.86 0.0053 B 2.82 1 2.82 24.39 0.0017 C 6.70 1 6.70 57.92 0.0001 AB 0.15 1 0.15 1.28 0.2948 AC 0.18 1 0.18 1.60 0.2465 BC 0.14 1 0.14 1.18 0.3126 A2 0.85 1 0.85 7.38 0.0299 B2 1.62 1 1.62 14.01 0.0072 C2 4.76 1 4.76 41.13 0.0004 残差 0.81 7 0.12 失拟项 0.27 3 0.09 0.66 0.6195 不显著 绝对误差 0.54 4 0.14 总和 20.57 16 标准差 0.34 拟合优度 0.9607 平均值 32.63 调整拟合优度 0.9101 变异系数(C.V.%) 1.04 预测拟合优度 0.7509 信噪比 12.0111
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表 5 TiO2回收率模型回归方差分析
Table 5. Regression analysis of variance for TiO2 recovery
来源 平方和 自由度 均方差 F值 P值 模型 68.54 9 7.61 43.36 <0.0001 显著 A 3.24 1 3.24 19.74 0.0030 B 1.25 1 1.25 7.61 0.0282 C 24.40 1 24.40 148.69 <0.0001 AB 1.48 1 1.48 9.00 0.0200 AC 1.69 1 1.69 10.30 0.0149 BC 0.93 1 0.93 5.68 0.0487 A2 14.36 1 14.36 87.50 <0.0001 B2 14.55 1 14.55 88.69 <0.0001 C2 3.23 1 3.23 19.72 0.0030 残差 1.15 7 0.16 失拟项 0.39 3 0.13 0.68 0.6079 不显著 绝对误差 0.76 4 0.19 总和 69.60 16 标准差 0.41 拟合优度 0.9835 平均值 83.89 调整拟合优度 0.9623 变异系数(C.V.%) 0.48 预测拟合优度 0.8936 信噪比 18.1992
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表 6 预测最优试验和实际试验对比
Table 6. Comparison of predicted optimal test and actual test
试验方案 药剂用量/（g·t−1） TiO2品位/% TiO2回收率/% 水玻璃 油酸钠 亚氯酸钠 预测 162.59 108.67 220.96 33.95 86.26 实际 160.00 110.00 220.00 33.92 86.30
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表 7 闭路试验结果
Table 7. Results of the flotation closed circuit test
产品 产率/% TiO2品位/% TiO2回收率/% 精矿 21.20 48.24 62.55 尾矿 78.80 7.77 37.45 钛粗精矿(浮选给矿) 100.00 16.35 100.00
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