Application of a SEM-EDS-Based Automated Process Mineralogy Analyzing System on the Occurrence State of Silver in Copper Ore Flotation Tailings
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摘要:
元素赋存状态及工艺矿物学特征是决定其选矿工艺及回收指标的关键因素，对指导矿产资源高效综合回收利用有重要意义。由于银矿物种类繁多且含量低、粒度细小不易识别，传统人为鉴别目标矿物并统计工艺矿物学参数的方法在银的赋存特征研究方面存在局限性，制约了资源高效综合利用。本文利用基于扫描电子显微镜(SEM)和X射线能谱仪(EDS)的工艺矿物学参数自动分析系统(BPMA)对某铜矿浮选尾矿样品(Ag 41.96µg/g，Cu 0.44%)进行矿物学分析，展示其在尾矿样品中铜和银的赋存状态及工艺矿物学特征研究中的具体应用。结果表明：样品中铜矿物主要为辉铜矿和斑铜矿；铜硫化物及其集合体的嵌布粒度细微且解离程度低，是影响铜回收的主要矿物学因素。样品中银主要以独立矿物的形式存在，(含)银矿物有自然银、辉银矿/螺状硫银矿、硒银矿、硒铜银矿、硫铜银矿和含银辉铜矿，银在各(含)银矿物中的分布率分别为95.62%、2.07%、1.33%、0.15%、0.80%和0.03%；银矿物嵌布粒度不均匀，粗粒(＞74µm)、中粒(74～37µm)、细粒(37～10µm)、微粒(＜10µm)银矿物的占有率分别为32.25%、30.35%、21.44%和15.95%；银矿物的解离程度较高，单体含量高达88.28%，可采用浮选法与铜硫化物一起回收。该研究为提高资源的选矿回收率提供了矿物学依据，同时采用的BPMA & SEM-EDS分析方法为矿物种类复杂、含量低、粒度细小的稀贵金属元素赋存状态及工艺矿物学研究提供了一种技术借鉴。
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关键词:
- 银；赋存状态 /
- 工艺矿物学 /
- 矿物粒度 /
- 矿物解离度 /
- 工艺矿物学参数自动分析系统
Abstract:The silver occurrence state and process mineralogical characteristics are critical to its beneficiation process and recovery indicators, which can be used for assisting in process development, plant design, and improvement of silver recovery. In order to define the occurrence state of silver in copper ore flotation tailings with low-grade Ag 41.96g/g & Cu 0.44%, BGRIMM process mineralogy analyzing system (BPMA) with version 2.0 BPMA software, scanning electron microscopy (SEM) and energy dispersive X-ray spectrometer (EDS) were applied to investigate the copper mineralogical characteristics and silver occurrence state of the flotation tailings. The copper minerals in the tailings are mainly fine-grained and poorly liberated copper sulfide minerals; the silver mainly occurs as independent silver minerals, with high liberation and non-uniform grain size. The analytical results show that the BPMA & SEM-EDS in situ analysis method can serve as a technical reference for the study of the occurrence state and process mineralogy of rare precious metal elements. The BRIEF REPORT is available for this paper at
http://www.ykcs.ac.cn/en/article/doi/10.15898/j.ykcs.202310250165 . -
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表 1 尾矿试样粒度筛析结果
Table 1. Particle size sieving analysis results of the tailing samples
粒级
(mm)质量
(g)产率
(%)元素品位 分布率 Cu(%) Ag(µg/g) Cu（%） Ag（%） +0.074 30.5 31.57 0.41 29.4 29.26 22.12 −0.074至+0.038 20.8 21.53 0.22 69.2 10.71 35.51 −0.038至+0.023 13.0 13.46 0.21 24.3 6.39 7.79 −0.023 32.3 33.44 0.71 43.4 53.65 34.58 合计 96.6 100.00 0.44 41.96 100.00 100.00 
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表 2 BPMA系统预设测量参数
Table 2. Operation conditions of the BPMA system
仪器工作参数 设定条件 全颗粒测量 选择颗粒测量 加速电压 20keV 20keV 工作距离 15mm 15mm 束流强度 3nA 3nA 放大倍率 400 1000 视场宽度 692.02µm 276.77µm 图像分辨率 1024×768pixel 1024×768pixel 像素尺寸 0.67µm 0.27µm 最大可测量帧数 1320 8426 背底阈值 30 100 最小颗粒面积 50pixel 1pixel 最大颗粒面积 − − 亮相灰度 100 100 亮相最小打点相面积 4pixel 1pixel 暗相最小打点相面积 4pixel 1pixel 分相精度 3 5 能谱采谱时间 60ms 60ms 测量终止条件 颗粒数: 105000 帧数: 8426 指定目标灰度 / 100～255 指定目标元素 / Ag
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表 3 尾矿试样的矿物组成分析结果
Table 3. Analytical results of mineral composition for the tailing samples
序号 矿物名称 分子式 矿物
颗粒数矿物含量
(wt.%)序号 矿物名称 分子式 矿物
颗粒数矿物含量
(wt.%)1 自然银 Ag 50 0.004 17 方解石 Ca[CO3] 5498 5.55 2 辉银矿/螺状硫银矿 Ag2S 21 0.0001 18 白云石 CaMg[CO3]2 4596 4.77 3 硒银矿 Ag2Se 55 ＜0.0001 19 绢云母 K{Al2[AlSi3O10](OH，F)2} 10001 4.74 4 硒铜银矿 CuAgSe 13 Trace 20 斜长石 (Na，Ca)[(Si，Al)4O8] 7100 1.66 5 硫铜银矿 AgCuS 13 Trace 21 辉石 (Ca，Mg，FeⅡ，FeⅢ，Al)(Si，Al)2O6 4373 1.51 6 辉铜矿 Cu2S 454 0.45 22 黑云母 K{Mg，Fe)3[AlSi3O10](OH)2 4893 1.23 7 斑铜矿 Cu5FeS4 182 0.09 23 绿泥石 {(Mg，Fe，Al)3[(Si，Al)4O10](OH)2}·(Mg，Fe，Al)3(OH)6 844 0.38 8 黄铜矿 CuFeS2 10 ＜0.01 24 金红石 TiO2 397 0.26 9 黄铁矿 FeS2 16 ＜0.01 25 重晶石 Ba[SO4] 255 0.20 10 方铅矿 PbS 20 ＜0.01 26 磷灰石 Ca5[(PO4)3]F 263 0.20 11 闪锌矿 ZnS 8 ＜0.01 27 高岭石 Al4[Si4O10](OH)8 276 0.09 12 磁铁矿 FeⅡFeⅢ2O4 560 0.59 28 锆石 Zr[SiO4] 68 0.03 13 钛铁矿 FeTiO3 104 0.01 29 独居石 Ce[PO4] 22 0.03 14 石英 SiO2 28976 54.21 30 其他 / 961 0.21 15 钾长石 K[AlSi3O8] 23726 13.10 合计 / 105386 100.00 16 钠长石 Na[AlSi3O8] 11627 10.66
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表 4 尾矿中主要铜矿物嵌布粒度分布
Table 4. Grain size distribution of main copper minerals in tailing samples
粒级(mm) 辉铜矿 斑铜矿 铜硫化物集合体 含量(%) 累积(%) 含量(%) 累积(%) 含量(%) 累积(%) +0.038 — — — — — — −0.038至+0.020 7.81 7.81 — — 8.55 8.55 −0.020至+0.015 9.04 16.85 — — 12.45 21.00 −0.015至+0.010 23.65 40.50 23.54 23.54 18.94 39.94 −0.010至+0.005 31.25 71.75 33.16 56.70 32.64 72.58 −0.005 28.25 100.00 43.31 100.01 27.42 100.00 注：铜硫化物集合体是将样品中辉铜矿、斑铜矿、黄铜矿等铜硫化物作为一个整体进行统计计算，下同。
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表 5 尾矿中主要铜矿物解离度分析结果
Table 5. Mineral liberation degree analysis results of main copper minerals in tailing samples
矿物名称 目标矿物占比(%) 合计
(%)0＜x≤25 25＜x≤50 50＜x≤75 75＜x＜100 100 辉铜矿 70.12 8.25 4.52 1.56 15.55 100.00 斑铜矿 67.28 7.82 4.06 1.63 19.22 100.00 铜硫化物集合体 64.60 12.94 3.36 1.67 17.43 100.00 注：“x”为复合颗粒中目标矿物的质量百分比。
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表 6 尾矿中主要铜矿物连生关系分析结果
Table 6. The interlocking relationships of main copper minerals in tailing samples
矿物名称 矿物单体含量
(%)连生体含量(%) 合计
(%)与其他铜硫化物连生 与石英连生 与长石连生 与方解石、白云石连生 与云母连生 与其他矿物连生 辉铜矿 15.55 6.73 40.90 21.77 7.50 5.56 1.99 100.00 斑铜矿 19.22 17.60 21.16 15.92 12.61 4.18 9.31 100.00 铜硫化物集合体 17.43 / 38.17 24.05 9.57 5.39 5.39 100.00
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表 7 尾矿中银矿物的种类及相对含量
Table 7. Mineral composition and relative content of silver-bearing minerals in tailing samples
银矿物种类 银矿物含量 矿物中银元素的
平均含量(%)银的分布率
(%)银矿物颗粒数 相对质量百分比(%) 自然银(Ag) 50 93.55 99.09 95.62 辉银矿/螺状硫银矿(Ag2S) 21 2.30 87.11 2.07 硒银矿(Ag2Se) 55 1.84 70.33 1.33 硒铜银矿(CuAgSe) 13 0.41 35.43 0.15 硫铜银矿(AgCuS) 13 1.51 51.15 0.80 含银辉铜矿[(Ag，Cu)2S] 4 0.39 6.88 0.03 合计 156 100.00 / 100.00
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表 8 尾矿中银矿物的嵌布特征及占有率统计结果
Table 8. Occurrence characteristics and distribution ratio of silver-bearing minerals in tailing samples
银矿物种类 银矿物赋存形式 嵌布特征 颗粒数 相对质量百分比
(%)合计
(%)自然银 单体 单体解离 39 84.13 84.13 连生 与石英连生 4 7.40 8.92 与方解石连生 2 1.38 与钠长石连生 2 0.14 包裹 被石英包裹 2 0.47 0.49 被方解石包裹 1 0.02 辉银矿/螺状硫银矿 单体 单体解离 17 2.01 2.01 连生 与钠长石连生 1 0.07 0.07 包裹 被石英包裹 3 0.22 0.22 硒银矿 单体 单体解离 4 0.42 0.42 连生 与方解石连生 6 0.54 0.57 与钠长石连生 2 0.03 裂隙 嵌布于方解石裂隙中 16 0.25 0.34 嵌布于石英裂隙中 3 0.09 包裹 被方解石包裹 23 0.48 0.50 被石英包裹 1 0.02 硒铜银矿 单体 单体解离 1 0.16 0.16 裂隙 嵌布于方解石裂隙中 12 0.26 0.26 硫铜银矿 单体 单体解离 9 1.24 1.24 连生 与白云石连生 1 0.15 0.19 与石英连生 1 0.03 包裹 被石英包裹 2 0.09 0.09 含银辉铜矿 单体 单体解离 3 0.32 0.32 连生 与钾长石连生 1 0.07 0.07 合计 156 100.00 100.00 注: “连生”是指银矿物与其他矿物共伴生但其表面裸露的嵌布形式，下同。
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表 9 尾矿中银矿物粒度分布
Table 9. Size distribution of silver-bearing minerals in tailing samples
粒级
(µm)银矿物* 自然银 辉银矿/螺状硫银矿 硒银矿 颗粒数 质量百分比
(%)累积
(%)颗粒数 质量百分比
(%)累积
(%)颗粒数 质量百分比
(%)累积
(%)颗粒数 质量百分比
(%)累积
(%)+74 1 32.25 32.25 1 34.47 34.47 — — — — — — −74+37 1 30.35 62.60 1 32.44 66.91 — — — — — — −37+20 2 14.99 77.59 2 16.03 82.94 — — — — — — −20+10 4 6.45 84.04 4 6.90 89.84 — — — — — — −10+5 20 8.69 92.73 13 6.77 96.61 3 50.75 50.75 1 15.29 15.29 −5+4 14 2.39 95.12 4 1.02 97.63 2 11.33 62.09 3 26.43 41.71 −4+3 23 2.61 97.73 12 1.79 99.42 5 21.08 83.17 3 13.20 54.91 −3+2 30 1.49 99.22 5 0.34 99.77 7 13.22 96.38 8 22.58 77.49 −2+1 29 0.65 99.88 8 0.23 100.00 3 3.49 99.87 16 17.56 95.05 −1 32 0.12 100.00 0 0.00 100.00 1 0.13 100.00 24 4.95 100.00 注： “银矿物粒度”是指将试样中自然银、辉银矿/螺状硫银矿、硒银矿、硒铜银矿、硫铜银矿等所有的银矿物作为整体统计其粒度。
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