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黄金科学技术 ›› 2018, Vol. 26 ›› Issue (5): 669-676.doi: 10.11872/j.issn.1005-2518.2018.05.669

• • 上一篇    下一篇

毒砂机械活化性能及其浸出试验研究

刘艳华,陈国宝*,杨洪英,金哲男,王改荣   

  1. 1东北大学冶金学院,辽宁 沈阳 110819
  • 收稿日期:2018-08-01 修回日期:2018-09-07 出版日期:2018-10-20 发布日期:2018-10-31
  • 通讯作者: 陈国宝
  • 基金资助:
    国家自然科学基金重大项目“含砷复杂金矿细菌氧化矿物界面能及其作用机制的基础研究”(编号:U1608254)和中央高校基本科研业务专项资金“超细磨强化难处理金矿浸出的基础研究”(编号:N172504022)联合资助

Research on Mechanical Activation Properties and Leaching Test of Arseno-pyrite

Yanhua LIU,Guobao CHEN*,Hongying YANG,Zhenan JIN,Gairong WANG   

  1. 1School of Metallurgy,Northeastern University,Shenyang 110819,Liaoning,China
  • Received:2018-08-01 Revised:2018-09-07 Online:2018-10-20 Published:2018-10-31
  • Contact: Guobao CHEN

摘要:

研究了一种新的预处理方法即机械活化法对毒砂矿物固态性质及溶解性质的影响。在行星式球磨机中,毒砂分别在不同磨矿速度下机械活化1 h,通过粒度和比表面积分析发现:随着磨矿速度的增加,毒砂颗粒先显著减小而后略有增大,当磨矿速度为300 r/min时,得到毒砂颗粒的最佳粒度分布、最小粒径(中位径为2.36 μm)和最大比表面积(2.667 m2/g)。通过SEM(扫描电子显微镜)对不同磨矿速度下毒砂形貌进行观察发现:随着磨矿速度的增加,毒砂表面形成了微纳米颗粒且表面无定形程度显著增加。XRD(X射线衍射)分析结果表明:随着磨矿速度的增加,没有物相转变发生,但毒砂的无定形度却增加至72%,晶格畸变从0.014%增加至0.097%,晶粒大小由75.6 nm减小至56.0 nm。通过拉曼光谱对毒砂的特征峰217.2 cm-1和273.7 cm-1进行分析,发现在机械力的作用下特征峰273.7 cm-1的振动程度更加明显。最后,对不同磨矿速度下的毒砂进行了硫酸铁酸性浸出试验,结果发现:与未活化的毒砂相比,在最佳磨矿速度为300 r/min的条件下,毒砂中总砷的溶解度增加了一倍,达到48.74%。

关键词: 毒砂, 机械活化, 结构分析, 拉曼光谱, 硫酸铁, 磨矿速度, 无定形度, 浸出试验

Abstract:

The effect of a new pretreatment method i.e. mechanical activation on the solid-state and dissolution properties of arsenopyrite was studied.In a planetary ball mill,arsenopyrite was mechanically activated for 1 h at different grinding speeds.The analysis of particle size and specific surface area indicated that the particle size of arsenopyrite decreased rapidly at first and then increased slightly with increase of milling speed.The optimum particle distribution,minimum particle size value of 2.36 μm and maximum specific surface area of 2.667 m2/g can be observed at milling speed of 300 r/min.The morphology of arsenopyrite at different milling speeds was observed by scanning electron microscopy(SEM),and it was found that the surface of arsenopyrite formed micro-nano particles and amorphization degree significantly increased with the increase of milling speed.XRD(X-ray diffraction)analysis results showed that with the increase of milling speed,no phase transformation occured,but the amorphization degree of arsenopyrite increased to 72%, lattice distortion increased from 0.014% to 0.097%,and crystallite size decreased from 75.6 nm to 56.0 nm.The characteristic peaks of 217.2 cm-1and 273.7 cm-1of arsenopyrite were analyzed by Raman spectroscopy.It was found that the vibration of the characteristic peak located at 273.7 cm-1was more sensitive to the mechanical stress.Finally,the leaching tests of arsenopyrite were carried out by Fe2(SO43solution.The results showed that contrasted with unactivated arsenopyrite,total arsenic extraction from arsenopyrite has doubled to nearly 48.74% under the optimum milling speed of 300 r/min.

Key words: arsenopyrite, mechanical activation, structural analysis, Raman spectroscopy, ferric sulfate, milling speed, amorphousity, leaching test

中图分类号: 

  • TF11

表1

样品XRF分析结果"

成分 含量 成分 含量
As 32.54 Al 0.20
Fe 28.48 Ca 0.07
S 21.90 Zn 0.06
Mg 15.74 Mn 0.03
Si 0.95 K 0.01

表2

样品主要元素定量分析结果"

元素 含量 元素 含量
As 45.60 Si 0.85
Fe 31.20 Mg 0.06
S 20.50

图1

样品XRD图谱"

图2

毒砂的比表面积、中位径与磨矿速度之间的变化关系"

图3

不同转速下毒砂扫描电镜图 (a)未碾磨;(b)磨矿速度为200 r/min;(c)磨矿速度为300 r/min;(d)磨矿速度为580 r/min"

图4

不同磨矿速度下扫描电镜和能谱分析图 (a),(b)未碾磨;(c),(d)磨矿速度为580 r/min"

图5

不同磨矿速度下毒砂的粒度分布 (a)未碾磨;(b)磨矿速度为200 r/min;(c)磨矿速度为300 r/min;(d)磨矿速度为580 r/min"

图6

不同磨矿速度下毒砂的XRD图谱 (a)未碾磨;(b)磨矿速度为200 r/min;(c)磨矿速度为300 r/min;(d)磨矿速度为580 r/min"

图7

毒砂X射线无定形度随磨矿速度的变化"

表3

不同转速下毒砂的晶体学参数"

样品 晶胞体积/(?3) 平均晶粒尺寸/nm 平均最大应变/%
a 175.09 75.6 0.014
b 174.38 72.8 0.017
c 175.19 59.0 0.022
d 175.69 64.5 0.097

图8

不同磨矿速度下毒砂拉曼光谱图谱"

图9

拉曼特征峰随磨矿速度的变化关系"

图10

不同磨矿速度下毒砂中总砷的浸出率与浸出时间的关系"

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