硫化铜镍矿浮选中镁硅酸盐矿物强化分散—同步抑制的理论及技术研究
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摘要
硫化铜镍矿中存在的蛇纹石、滑石等镁硅酸盐矿物,干扰硫化矿的浮选并使精矿中MgO含量升高,影响后续冶炼过程,严重制约着我国铜镍资源的高效利用。本文以层状镁硅酸盐矿物为主要研究对象,采用多种试验方法与分析测试手段,重点针对镁硅酸盐矿物的强化分散与选择性抑制进行了系统深入的研究,形成了硫化铜镍矿浮选体系“固液界面离子选择性迁移-浮选剂分子间组装”调控原理,并以此为基础开发了硫化铜镍矿强化浮选技术原型。论文的主要研究内容和创新成果如下：
(1)层状镁硅酸盐矿物晶体结构、表面性质与可浮性的关系
硫化铜镍矿中层状镁硅酸盐矿物主要包括蛇纹石、滑石和绿泥石,其晶体结构单元层由硅氧四面体与镁氧八面体组成。蛇纹石解离时镁氧八面体层断裂,表面暴露的镁氧键离子性强,水化作用强,天然亲水性好；滑石解离主要沿层间断裂,表面为残余的分子键,水化作用弱,天然疏水性好；绿泥石解离时表面同时暴露出分子键和镁氧键,天然疏水性介于蛇纹石与滑石之间。
在水溶液中蛇纹石表面羟基优先溶解,Mg2+残留在蛇纹石表面使其荷正电,零电点为10.0；滑石与绿泥石解离表面优先吸附溶液中的OH-,矿物表面荷负电,零电点分别为3.0和4.4。当pH<10时蛇纹石易与表面荷负电的镍黄铁矿等硫化矿物通过静电作用发生异相凝聚,影响硫化铜镍矿的浮选。(2)颗粒间异相凝聚对矿物浮选行为的影响
蛇纹石与硫化矿颗粒间的异相凝聚,导致硫化矿对捕收剂的吸附能力降低,从而降低硫化矿的可浮性；蛇纹石与滑石矿物间的异相凝聚,一方面使滑石的可浮性降低,另一方面导致滑石对抑制剂的吸附能力降低,从而使滑石不能被完全抑制。聚合磷酸盐和水玻璃能较好的分散蛇纹石与硫化矿、蛇纹石与滑石,减弱甚至消除矿物颗粒间的异相凝聚。(3)蛇纹石表面电性的强化调控机制
降低蛇纹石表面电位是消除矿物间异相凝聚的有效途径,而蛇纹石表面电性调控的关键在于蛇纹石表面镁向液相的迁移行为,即控制蛇纹石表面镁向液相迁移,减少双电层中定位离子的正电荷密度,从而降低蛇纹石表面电位。
链状聚合磷酸盐能有效降低蛇纹石表面电位,其作用机制主要包括三个方面：1)促进蛇纹石表面的镁迁移到液相,降低蛇纹石的表面电位；2)与液相中的Mg2+作用生成为稳定的可溶性络合物,阻止Mg2+向蛇纹石表面反吸附,保持蛇纹石表面的负电性；3)通过吸附在蛇纹石表面,进一步降低其表面电位。
通过对蛇纹石表面电性的强化调控,消除了异相凝聚对硫化矿可浮性的影响,并实现了滑石的完全抑制。
(4)固液界面浮选剂的分子间组装
有机高分子聚合物古尔胶和CMC是滑石的有效抑制剂,但同时也抑制硫化矿的浮选；而巯基捕收剂黄药只与硫化矿作用,并不在滑石表面吸附。优先添加捕收剂可以减弱抑制剂在硫化矿表面的吸附,增强浮选剂作用的选择性。因此改变药剂添加顺序,调整捕收剂与抑制剂在矿物表面的组装过程,能够增大硫化矿与滑石表面润湿性差异,有利于二者浮选分离。
(5)硫化铜镍矿强化浮选技术
基于多矿相镁硅酸盐矿物“强化分散-同步抑制”调控原理,形成了硫化铜镍矿强化浮选技术,并在新疆哈密天隆镍矿进行了工业试验。针对原矿品位Ni0.53%、Cu0.27%的低品位硫化铜镍矿,获得Ni5.68%、Cu3.14%的铜镍混合浮选精矿,Ni、Cu回收率分别达到80.23%和88.05%。采用硫化铜镍矿强化浮选技术,在精矿镍、铜品位相近的情况下,镍回收率提高3.04个百分点,铜回收率提高9.92个百分点。
High content of magnesium-silicate minerals like serpentine and talc not only obstructs the flotation separation of copper-nickel sulfide ores but also makes a undesirable high content of MgO in concentrate to impede the subsequent smelting process, which restricts the efficient utilization of copper and nickel resources in China. Basing on the layered magnesium-silicate minerals, this thesis firstly investigated the enhanced dispersion and selective depression of magnesium-silicate minerals by various experimental methods and analysis technologies. Then, the regulation principle of "selective migration of ion in solid/liquid interface-molecular assembly of flotation agent" in the floatation system of copper-nickel sulphide ores was established. Last but not least, the technical prototype of strengthening flotation of copper-nickel sulphide ores was proposed. Main conclusions and innovations of this thesis are listed as follows:
1. Relevance among crystal structure, surface property and floatability of layered magnesium-silicate minerals
Layered magnesium-silicate minerals associated with copper-nickel sulfide ores include serpentine, talc and chlorite. All of them are characterized with uniform crystal structures consisting of silicon-oxygen tetrahedron and magnesium-oxygen octahedron. The magnesium-oxygen octahedron layers are broken during the liberation of serpentine to expose the magnesium-oxygen bonds with strong ionicity and hydration, which results in natural hydrophilicity of serpentine. For talc, characterized as good natural hydrophobicity, the liberation comes from the interlaminar fracture to remain molecular bonds on surface with weak hydration. Meanwhile, both molecular bonds and magnesium-oxygen bonds are exposed on chlorite surface when liberation occurs, resulting in moderate natural hydrophobicity between serpentine and talc.
In water, the hydroxyl on serpentine surface ruptures and dissolves into the aqueous phase while the Mg2+remains, resulting in surface positive charge with pHPZC of10.0. On the other hand, the preferential adsorption of OH-on liberated talc and chlorite make surface negatively charges the minerals' surfaces with pHPZC of3.0and4.4, respectively. Hetercoagulation is easy to occur between serpentine and negatively charged sulfide ores due to the electrostatic interaction when pH<10, which hinders the flotation of copper-nickel sulfide ores.
2. Influence of hetercoagulation among mineral particles on mineral flotation separation
Firstly hetercoagulation between serpentine and sulfide ore particles reduces the adsorption capacity of collector on sulfides surface and leads to lower floatability of sulfide ores. Secondly hetercoagluation between serpentine and talc not only decreases the floatability of talc, but also weakens the adsorption capacity of talc to depressant, which hinders talc to be totally depressed. Polyphosphate and sodium silicate can effectively disperse serpentine and sulfide, as well as talc, and can weaken, even eliminate the hetercoagulation among mineral particles.
3. Strengthening regulation mechanism of serpentine surface electrical property
Key to eliminate hetercoagulation among minerals is to reduce the surface electrical potential of serpentine, and key to regulate surface electrical potential of serpentine is to control the migration behaviour of Mg2+on serpentine surface from solid particles to aqueous solution. Namely, increase of migration of Mg2+from particles to solution will decrease the positive charge density of positioning ion Mg2+in electric double layer and then reduce the surface potential of serpentine.
The reduction of surface potential of serpentine by chained polyphosphate is determined by three factors. First, chained polyphosphate can promote the migration of Mg2+from particles to solution to lower the surface potential of serpentine. Second, stable soluble complex can be formed by combining Mg2+with chained polyphosphate, which hinders the readsorption of Mg2+onto serpentine surface and maintains the negative potential of serpentine surface. Third, the surface potential of serpentine can be further reduced by the specific adsorption of chained polyphosphate onto the serpentine surface.
Through the strengthening regulation of serpentine surface electrical property, the influence of hetercoagulation on floatability of sulfide ores has been edulcorated, and the talc has been totally depressed.
4. Molecular assembly of flotation agents on solid-liquid interface
Organic polymer guar gum and CMC are efficient depressant for talc and also have certain depression for sulfide floatability. Meanwhile the thiol collector xanthate only reacts with sulfide ores and has nothing to do with talc. Preferential addition of collector can prevent the adsorption of depressant onto sulfide surface. Therefore the selective interaction between flotation agents and different minerals is achieved. Thus, through changing the addition sequence of flotation agents and adjusting the assembly process of collectors and depressants onto mineral surface, the surface wettability difference between sulfide and talc can be enlarged enough to benefit the flotation separation.
5. Strengthening flotation technique for copper-nickel sulfide ore
Basing on the control principle of strengthening dispersion synchronous depression for kinds of magnesium-silicate minerals, the strengthening flotation technique has been proposed and experimented industrially by using Kami low grade copper-nickel sulfide ore (Ni of0.53%and Cu of0.27%) as raw material. The high grade mixed concentrate of copper-nickel (Ni of5.68%and Cu of3.14%) have been obtained with the nickel and copper recovery of80.23%and88.05%, respectively. In the case of similar concentrate grade, the recovery of nickel and copper has been increased by3.04%and9.92%, respectively, though applying the strengthening flotation technique.
(1)层状镁硅酸盐矿物晶体结构、表面性质与可浮性的关系
硫化铜镍矿中层状镁硅酸盐矿物主要包括蛇纹石、滑石和绿泥石,其晶体结构单元层由硅氧四面体与镁氧八面体组成。蛇纹石解离时镁氧八面体层断裂,表面暴露的镁氧键离子性强,水化作用强,天然亲水性好；滑石解离主要沿层间断裂,表面为残余的分子键,水化作用弱,天然疏水性好；绿泥石解离时表面同时暴露出分子键和镁氧键,天然疏水性介于蛇纹石与滑石之间。
在水溶液中蛇纹石表面羟基优先溶解,Mg2+残留在蛇纹石表面使其荷正电,零电点为10.0；滑石与绿泥石解离表面优先吸附溶液中的OH-,矿物表面荷负电,零电点分别为3.0和4.4。当pH<10时蛇纹石易与表面荷负电的镍黄铁矿等硫化矿物通过静电作用发生异相凝聚,影响硫化铜镍矿的浮选。(2)颗粒间异相凝聚对矿物浮选行为的影响
蛇纹石与硫化矿颗粒间的异相凝聚,导致硫化矿对捕收剂的吸附能力降低,从而降低硫化矿的可浮性；蛇纹石与滑石矿物间的异相凝聚,一方面使滑石的可浮性降低,另一方面导致滑石对抑制剂的吸附能力降低,从而使滑石不能被完全抑制。聚合磷酸盐和水玻璃能较好的分散蛇纹石与硫化矿、蛇纹石与滑石,减弱甚至消除矿物颗粒间的异相凝聚。(3)蛇纹石表面电性的强化调控机制
降低蛇纹石表面电位是消除矿物间异相凝聚的有效途径,而蛇纹石表面电性调控的关键在于蛇纹石表面镁向液相的迁移行为,即控制蛇纹石表面镁向液相迁移,减少双电层中定位离子的正电荷密度,从而降低蛇纹石表面电位。
链状聚合磷酸盐能有效降低蛇纹石表面电位,其作用机制主要包括三个方面：1)促进蛇纹石表面的镁迁移到液相,降低蛇纹石的表面电位；2)与液相中的Mg2+作用生成为稳定的可溶性络合物,阻止Mg2+向蛇纹石表面反吸附,保持蛇纹石表面的负电性；3)通过吸附在蛇纹石表面,进一步降低其表面电位。
通过对蛇纹石表面电性的强化调控,消除了异相凝聚对硫化矿可浮性的影响,并实现了滑石的完全抑制。
(4)固液界面浮选剂的分子间组装
有机高分子聚合物古尔胶和CMC是滑石的有效抑制剂,但同时也抑制硫化矿的浮选；而巯基捕收剂黄药只与硫化矿作用,并不在滑石表面吸附。优先添加捕收剂可以减弱抑制剂在硫化矿表面的吸附,增强浮选剂作用的选择性。因此改变药剂添加顺序,调整捕收剂与抑制剂在矿物表面的组装过程,能够增大硫化矿与滑石表面润湿性差异,有利于二者浮选分离。
(5)硫化铜镍矿强化浮选技术
基于多矿相镁硅酸盐矿物“强化分散-同步抑制”调控原理,形成了硫化铜镍矿强化浮选技术,并在新疆哈密天隆镍矿进行了工业试验。针对原矿品位Ni0.53%、Cu0.27%的低品位硫化铜镍矿,获得Ni5.68%、Cu3.14%的铜镍混合浮选精矿,Ni、Cu回收率分别达到80.23%和88.05%。采用硫化铜镍矿强化浮选技术,在精矿镍、铜品位相近的情况下,镍回收率提高3.04个百分点,铜回收率提高9.92个百分点。
High content of magnesium-silicate minerals like serpentine and talc not only obstructs the flotation separation of copper-nickel sulfide ores but also makes a undesirable high content of MgO in concentrate to impede the subsequent smelting process, which restricts the efficient utilization of copper and nickel resources in China. Basing on the layered magnesium-silicate minerals, this thesis firstly investigated the enhanced dispersion and selective depression of magnesium-silicate minerals by various experimental methods and analysis technologies. Then, the regulation principle of "selective migration of ion in solid/liquid interface-molecular assembly of flotation agent" in the floatation system of copper-nickel sulphide ores was established. Last but not least, the technical prototype of strengthening flotation of copper-nickel sulphide ores was proposed. Main conclusions and innovations of this thesis are listed as follows:
1. Relevance among crystal structure, surface property and floatability of layered magnesium-silicate minerals
Layered magnesium-silicate minerals associated with copper-nickel sulfide ores include serpentine, talc and chlorite. All of them are characterized with uniform crystal structures consisting of silicon-oxygen tetrahedron and magnesium-oxygen octahedron. The magnesium-oxygen octahedron layers are broken during the liberation of serpentine to expose the magnesium-oxygen bonds with strong ionicity and hydration, which results in natural hydrophilicity of serpentine. For talc, characterized as good natural hydrophobicity, the liberation comes from the interlaminar fracture to remain molecular bonds on surface with weak hydration. Meanwhile, both molecular bonds and magnesium-oxygen bonds are exposed on chlorite surface when liberation occurs, resulting in moderate natural hydrophobicity between serpentine and talc.
In water, the hydroxyl on serpentine surface ruptures and dissolves into the aqueous phase while the Mg2+remains, resulting in surface positive charge with pHPZC of10.0. On the other hand, the preferential adsorption of OH-on liberated talc and chlorite make surface negatively charges the minerals' surfaces with pHPZC of3.0and4.4, respectively. Hetercoagulation is easy to occur between serpentine and negatively charged sulfide ores due to the electrostatic interaction when pH<10, which hinders the flotation of copper-nickel sulfide ores.
2. Influence of hetercoagulation among mineral particles on mineral flotation separation
Firstly hetercoagulation between serpentine and sulfide ore particles reduces the adsorption capacity of collector on sulfides surface and leads to lower floatability of sulfide ores. Secondly hetercoagluation between serpentine and talc not only decreases the floatability of talc, but also weakens the adsorption capacity of talc to depressant, which hinders talc to be totally depressed. Polyphosphate and sodium silicate can effectively disperse serpentine and sulfide, as well as talc, and can weaken, even eliminate the hetercoagulation among mineral particles.
3. Strengthening regulation mechanism of serpentine surface electrical property
Key to eliminate hetercoagulation among minerals is to reduce the surface electrical potential of serpentine, and key to regulate surface electrical potential of serpentine is to control the migration behaviour of Mg2+on serpentine surface from solid particles to aqueous solution. Namely, increase of migration of Mg2+from particles to solution will decrease the positive charge density of positioning ion Mg2+in electric double layer and then reduce the surface potential of serpentine.
The reduction of surface potential of serpentine by chained polyphosphate is determined by three factors. First, chained polyphosphate can promote the migration of Mg2+from particles to solution to lower the surface potential of serpentine. Second, stable soluble complex can be formed by combining Mg2+with chained polyphosphate, which hinders the readsorption of Mg2+onto serpentine surface and maintains the negative potential of serpentine surface. Third, the surface potential of serpentine can be further reduced by the specific adsorption of chained polyphosphate onto the serpentine surface.
Through the strengthening regulation of serpentine surface electrical property, the influence of hetercoagulation on floatability of sulfide ores has been edulcorated, and the talc has been totally depressed.
4. Molecular assembly of flotation agents on solid-liquid interface
Organic polymer guar gum and CMC are efficient depressant for talc and also have certain depression for sulfide floatability. Meanwhile the thiol collector xanthate only reacts with sulfide ores and has nothing to do with talc. Preferential addition of collector can prevent the adsorption of depressant onto sulfide surface. Therefore the selective interaction between flotation agents and different minerals is achieved. Thus, through changing the addition sequence of flotation agents and adjusting the assembly process of collectors and depressants onto mineral surface, the surface wettability difference between sulfide and talc can be enlarged enough to benefit the flotation separation.
5. Strengthening flotation technique for copper-nickel sulfide ore
Basing on the control principle of strengthening dispersion synchronous depression for kinds of magnesium-silicate minerals, the strengthening flotation technique has been proposed and experimented industrially by using Kami low grade copper-nickel sulfide ore (Ni of0.53%and Cu of0.27%) as raw material. The high grade mixed concentrate of copper-nickel (Ni of5.68%and Cu of3.14%) have been obtained with the nickel and copper recovery of80.23%and88.05%, respectively. In the case of similar concentrate grade, the recovery of nickel and copper has been increased by3.04%and9.92%, respectively, though applying the strengthening flotation technique.
引文
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