Recovery of Rubidium from a Tungsten Tailings Containing High Calcite by Reverse−positive Flotation Process
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摘要:
某钨尾矿含铷0.098%，脉石矿物主要为石英、石榴石、萤石、方解石，铷主要赋存在白云母、黑云母及钾长石中，其与脉石矿物嵌布关系极为复杂，属伴生高钙低品位铷矿。为确定铷回收工艺，采用反浮选脱钙—铷正浮选原则流程，详细开展了反浮选脱钙粗选捕收剂、抑制剂和铷浮选粗选活化剂、矿浆pH、十二胺用量、精选抑制剂六偏磷酸钠用量等条件实验。结果表明，反浮选脱钙采用捕收剂CYP+抑制剂SN−1，铷正浮选采用硫酸+十二胺，最终通过反浮选脱钙（两粗三精）—无氟少酸铷正浮选（一粗一扫一精）闭路流程，获得了铷精矿Rb2O品位0.214%、Rb2O回收率71.04%的指标，较好地实现了铷资源的回收。
Abstract:A tungsten tailings contains 0.098% rubidium, and the gangue minerals are mainly quartz, garnet, fluorite, and calcite. Rubidium is mainly present in muscovite, biotite, and potassium feldspar, and its distribution relationship with the gangue minerals is extremely complex, belonging to the associated high calcium low grade rubidium ore. In order to determine the rubidium recovery process, a reverse flotation decalcification rubidium flotation principle process was adopted. Detailed experiments were conducted on the collector, inhibitor, and selection process of reverse flotation decalcification coarse selection, as well as conditions such as rubidium flotation coarse selection activator, pulp pH, dodecylamine, and selected sodium hexametaphosphate. The results determined that a collector CYP+inhibitor SN−1 reagent system was used for reverse flotation decalcification, and a sulfuric acid+dodecylamine reagent system was used for rubidium positive flotation. Finally, through the closed circuit process of reverse flotation decalcification (two coarse and three fine) − fluorine−free low acid rubidium flotation (one coarse and one sweep and one fine), the Rb2O grade of rubidium concentrate was 0.214%, and the Rb2O recovery rate was 71.04%, effectively achieving the recovery of rubidium resources
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Key words:
- rubidium ore /
- mica /
- feldspar /
- reverse flotation /
- decalcification /
- hydrofluoric acid−free and less sulfuric acid
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表 1 矿石化学多元素分析结果
Table 1. Chemical multi−element analysis results of ore
/% 组 分 Rb2O Li2O Cs2O Na2O K2O SiO2 Al2O3 CaO 含 量 0.098 0.02 0.0039 0.65 1.37 33.27 10.16 26.69 组 分 TFe FeO Fe2O3 F TiO2 MgO MnO 烧失 含 量 7.99 4.69 6.22 7.10 0.18 1.45 0.80 6.37 
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表 2 矿石的矿物组成
Table 2. Mineral composition of the raw ore
/% 矿物 白云母 黑云母 钠长石 钾长石 石 英 石榴石 萤 石 方解石 含量 7.55 3.09 8.89 3.31 11.49 32.44 14.40 5.59 矿物 辉石 绿泥石
黝帘石磁铁矿 黄铁矿 磁黄
铁矿菱铁矿 褐铁矿 其 他 含量 3.21 2.18 2.26 1.91 0.40 0.99 0.23 2.06
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表 3 铷在各矿物中的赋存分布
Table 3. Occurrence and distribution of rubidium in various minerals
/% 矿 物 含 量 Rb2O品位 Rb2O分布率 白云母 7.55 0.58 46.68 黑云母 3.09 0.88 29.24 钾长石 3.31 0.57 20.11 钠长石 8.89 0.04 3.92 其 他 77.16 微量 0.05 合 计 100.00 0.093 100.00
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表 4 反浮选粗选捕收剂种类实验结果
Table 4. Test results of types of collectors in reverse rough flotation
/% 捕收剂种类 产品名称 产率 品位 回收率 Rb2O CaCO3 Rb2O CaCO3 731 尾矿 48.74 0.073 8.540 38.67 84.09 粗精矿 51.26 0.110 1.536 61.33 15.91 给矿 100.00 0.092 4.950 100.00 100.00 CYP−1 尾矿 49.19 0.067 8.540 35.06 88.44 粗精矿 50.81 0.120 1.081 64.94 11.56 给矿 100.00 0.094 4.750 100.00 100.00 油酸 尾矿 54.47 0.077 8.040 45.10 90.67 粗精矿 45.53 0.112 0.990 54.90 9.33 给矿 100.00 0.093 4.830 100.00 100.00
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表 5 反浮选粗选抑制剂种类实验结果
Table 5. Test results of inhibitors type for reverse rough flotation
抑制剂种类及用量 产品名称 产率/% 品位/% 回收率/% Rb2O CaCO3 Rb2O CaCO3 水玻璃
（625 g/t）尾矿 49.19 0.067 8.540 35.06 88.44 粗精矿 50.81 0.120 1.081 64.94 11.56 给矿 100.00 0.094 4.750 100.00 100.00 SN−1抑制剂
（1200 g/t）尾矿 43.89 0.057 9.120 26.61 83.39 粗精矿 56.11 0.123 1.421 73.39 16.61 给矿 100.00 0.094 4.800 100.00 100.00 六偏磷酸钠
（200 g/t）尾矿 34.78 0.074 8.540 27.67 60.74 粗精矿 65.22 0.103 2.944 72.33 39.26 给矿 100.00 0.093 4.890 100.00 100.00
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表 6 反浮选脱钙全流程实验结果
Table 6. Test results of the whole flowsheet of reverse flotation decalcification
/% 产品名称 产率 品位 回收率 Rb2O CaCO3 Rb2O CaCO3 尾矿 21.46 0.021 15.740 4.65 68.79 中矿3 3.21 0.078 5.130 2.58 3.35 中矿2 9.80 0.100 2.510 10.10 5.01 中矿1 24.62 0.120 1.540 30.46 7.72 反浮选精矿 40.91 0.124 1.815 52.21 15.13 给矿 100.00 0.097 4.910 100.00 100.00
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表 7 反浮选脱钙闭路实验结果
Table 7. Closed circuit test results of reverse flotation decalcification
/% 产品名称 产率 品位 回收率 Rb2O CaCO3 Rb2O CaCO3 尾矿 24.91 0.024 15.390 6.23 77.92 反浮选精矿
（选铷给矿）75.09 0.120 1.447 93.77 22.08 给矿 100.00 0.096 4.920 100.00 100.00
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表 8 活化剂对比实验结果
Table 8. Comparison test results of activators
活化剂 产品名称 作业产率
/%Rb2O品位
/%Rb2O作业
回收率/%硫酸：10 kg/t；
pH值4铷粗精矿 53.43 0.159 70.21 尾矿 46.57 0.077 29.79 选铷给矿 100 0.121 100 氢氟酸：40 kg/t；
pH值4铷粗精矿 52.32 0.162 70.63 尾矿 47.68 0.074 29.37 选铷给矿 100 0.12 100
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表 9 反浮选脱钙—无氟少酸铷全流程闭路浮选实验结果
Table 9. Results of closed circuit flotation test for the whole process of decalcification by reverse flotation − fluorine free rubidium acid
/% 产品名称 产率 Rb2O品位 Rb2O回收率 铷精矿 31.87 0.214 71.04 尾矿 68.13 0.0408 28.96 给矿 100.00 0.096 100.00
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