磨矿过程物理化学因素对几种碳酸盐矿物浮选的影响
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摘要
碳酸盐矿物是重要的矿物原料,也是提取Fe、Mg、Mn、Pb、Zn、Cu等金属及放射性元素Th、U和稀土元素的重要矿物原料来源。随着硫化矿资源与富矿资源的日趋枯竭,碳酸盐类矿物等氧化矿资源的开发和利用越来越受重视,此外,方解石、白云石等一些碳酸盐矿物常作为脉石矿物与有用矿物共生,许多浮选工艺都涉及到有用矿物与碳酸盐矿物的分离,因此研究碳酸盐的浮选行为,对盐类矿物和非盐类矿物的浮选理论和工业实践均有十分重要的意义。
当前碳酸盐的浮选主要集中在浮选药剂的开发,浮选作用机理的研究和浮选工艺流程的研究上。作为浮选前的必备工序,磨矿作业与碳酸盐矿物浮选间的联系似乎较少有选矿工作者关注。磨矿作业的任务不仅仅是为浮选作业提供粒度合乎要求、充分解离的入选物料,其对矿物的浮选行为也有着重要影响。国内外学者通过大量研究证明,在硫化矿浮选中,磨矿环境对其浮选指标有着重大的影响,在理论研究和生产实践上都取得重要进展。研究磨矿对碳酸盐矿物浮选行为的影响,寻找磨矿过程物理化学因素与碳酸盐矿物浮选行为间的联系及其规律性,有着重要的理论及实践意义。
本文以孔雀石、菱锌矿、菱镁矿、方解石四种碳酸盐矿物和常见硅质脉石石英为研究对象,通过磨矿和浮选试验,结合X射线光电子能谱(XPS)、原子吸收光谱、ζ电位测定等现代表面及溶液分析检测技术,系统研究了磨矿介质、磨矿方式和药剂添加方式(捕收剂、调整剂)变化对五种矿物表面溶液性质及其在油酸钠、十二胺浮选体系中浮选行为的影响,并对其作用机理进行了初步探讨。
研究表明,油酸钠浮选体系中,采用氧化锆球介质磨矿比采用钢球介质磨矿更有利于碳酸盐矿物的浮选,而采用钢球介质磨矿对石英的浮选有明显的活化作用。十二胺浮选体系中,钢球介质磨矿对五种矿物的浮选都产生了抑制作用。这可能归因于钢球介质在磨矿过程中发生的电化学腐蚀。在磨损差异腐蚀原电池和电偶原电池的作用下,发生Fe的氧化和溶解氧的还原,并发生一系列氧化还原反应,通过矿浆(Eh,pH)的测定,根据Fe—H2O体系的Eh—pH图可判断在钢球介质磨矿后的矿浆中Fe元素主要以Fe(OH)3相存在,溶液检测表明,矿浆中同时还有可溶性铁组分存在,根据矿浆溶液的pH值条件、Eh—pH图及Fe2+和Fe3+的浓度对数图判断,溶液中存在的可溶性Fe组分应以Fe2+及其羟基络合物为主。溶液中的Fe2+离子在矿物表面的吸附及Fe(OH)3在矿物表面的吸附改变了矿物的表面电性和表面性质,由此对矿物的浮游性产生影响。
干、湿磨对四种碳酸盐矿物浮游性的影响规律不同,油酸钠浮选体系中,孔雀石氧化锆球介质湿磨的可浮性优于干磨,钢球介质干磨的可浮性优于湿磨。方解石两种介质干磨的可浮性优于湿磨。而菱锌矿和菱镁矿两种介质湿磨的可浮性优于干磨。十二胺浮选体系中,无论采用何种磨矿介质,湿磨孔雀石和方解石的可浮性优于干磨,而干磨菱锌矿和菱镁矿的可浮性优于湿磨。由XPS表面元素分析可知,干磨和湿磨过程使碳酸盐矿物表面阴离子和金属阳离子的分布产生差异,进而影响碳酸盐矿物在油酸钠和十二胺浮选体系中的浮游性。根据对碳酸盐矿物晶体结构差异及其溶解性的分析,作出了“碳酸盐干磨与湿磨浮选差异是溶解初态与溶解平衡态之间的浮选差异”的假设。通过油酸钠浮选体系搅拌时间试验及矿物干、湿磨后ζ电位的测定对该假设进行了初步验证。该假设对菱锌矿和菱镁矿具有较好的适应性,而对孔雀石和方解石的适应性不是很明显。
在单矿物浮选试验的基础上,进行了四种人工混合矿的浮选分离试验。其中孔雀石—石英体系在氧化锆球介质湿磨时获得了较好的浮选分离效果。相同条件下,氧化锆球介质磨矿时的选择性指数略高于钢球介质磨矿时的选择性指数。
Carbonate minerals are very important nonmetal mineral materials, an important mineral source of extracting metal, such as Fe、Mg、Mn、Pb、Zn、Cu and radioactive element and rare earth elements. It is of great economic significance to the world. With sulphide ore and rich ore resources exhausted day by day, the development and utilization of Carbonate minerals draw more and more attention. Calcite and dolomite coexists valuable minerals as gangue minerals usually. Many flotation processes involve the separate of valuable minerals with carbonate minerals. So it is of great significance to the flotation theory and industrial practice of salt minerals to research on the flotation behaviors of carbonate minerals.
The research of carbonate flotation is mainly focus on the develop of flotation reagents, flotation mechanism research and flotation process improvement. But the relationship between grinding and flotation of carbonate minerals is paid little attention by the mineral processing researchers. Grinding is not only substantial to decrease the size and consequently to liberate the valuable minerals from its gangue to allow for their selective recovery during mineral processing processes such as flotation but also to influence the flotation behavior significantly. Many researches and industrial practices showed that the interactions between the ore and the grinding environment affect sulphide both in recovery and selectivity. It has an important theory and practice significance to study the affect of grinding on the flotation behavior of carbonate minerals and to search for the relationship and regularity between physicochemical factors of grinding process and flotation behavior of carbonate minerals.
The study was undertaken using four carbonate minerals, including calcite, malachite, calamine and magnesite and a common gangue mineral, quartz. The influence of different grinding media, different grinding mode and the flotation reagents addition site on the flotation of five minerals using sodium oleate and lauryl amine as collector respectively was investigated using advanced surface and solution test technology such as X-ray photoelectron spectrometric (XPS), atomic absorption spectrometry (AAS) analysis andζpotential measure. And the effecting mechanism of grinding environment on floatability of five minerals was discussed.
It is showed that grinding with zirconia media is beneficial to the flotation of carbonate minerals using sodium oleate as collector than grinding with steel media, but grinding with steel media can activate the flotation of quartz obviously. And grinding with steel media depresses the flotation of all five minerals when using lauryl amine as collector. It may be attributed to the electrochemical corrosion of steel media in grinding. The iron will be oxidized and oxygen in the solution be reduced subjected to the abrasion diversity corrosion and galvanic corrosion. It is showed that the species in slurry after grinding with steel ball are mainly Fe(OH)3 based on the (Eh, pH) value of slurry and the Eh-pH phase digram of Fe-H2O system. And the solution test shows that there is soluble Fe phase in slurry solution, which may be Fe2+ and its hydroxy complexes. The adsorption of Fe(OH)3, Fe2+ and its hydroxy complexes in the minerals surface may change the surface electricity and surface properties, then effect the minerals floatability.
The influence law of wet and dry grinding on the flotation of four carbonate minerals is different. The floatability of malachite using sodium oleate as collector after wet grinding with zirconia media is better than dry grinding, but the floatability of malachite after dry grinding with steel media is better than wet grinding. The floatability of calcite after dry grinding is better than wet grinding, while the floatability of calamine and magnesite after dry grinding is worse than wet grinidng with both kind of grinding media. When using lauryl amine as collector, the floatability of calcite after wet grinding is better than dry grinding, while the floatability of calamine and magnesite after dry grinding is better than wet grinidng with both kind of grinding media.The XPS surface elements test shows that, wet and dry grinding process makes the distribution difference of surface anion and metal cation, then influence the floatability of carbonate minerals using sodium oleate and lauryl amine as collector. An assumption of "the flotation difference of carbonate after wet and dry grinding is the flotation difference between initial state and equilibrium state of carbonate dissolution" was made out according to the analysis of the carbonate crystal structure and solubility properties. And the "Stirring time" test andζpotential measurement were carried out to verify the validity of the assumption. The floatability of calamine and magnesite has good correlation with the assumption but the floatability of malachite and calcite shows a poor correlation.
Flotation separation experiment of four groups of mixed mineral was carried out using sodium oleate as collector. The separation effect of malachite-quartz system wet grinding with zirconia is relatively superior. The selectivity index of grinding with zirconia media is higher than grinding with steel media under the same condition.
当前碳酸盐的浮选主要集中在浮选药剂的开发,浮选作用机理的研究和浮选工艺流程的研究上。作为浮选前的必备工序,磨矿作业与碳酸盐矿物浮选间的联系似乎较少有选矿工作者关注。磨矿作业的任务不仅仅是为浮选作业提供粒度合乎要求、充分解离的入选物料,其对矿物的浮选行为也有着重要影响。国内外学者通过大量研究证明,在硫化矿浮选中,磨矿环境对其浮选指标有着重大的影响,在理论研究和生产实践上都取得重要进展。研究磨矿对碳酸盐矿物浮选行为的影响,寻找磨矿过程物理化学因素与碳酸盐矿物浮选行为间的联系及其规律性,有着重要的理论及实践意义。
本文以孔雀石、菱锌矿、菱镁矿、方解石四种碳酸盐矿物和常见硅质脉石石英为研究对象,通过磨矿和浮选试验,结合X射线光电子能谱(XPS)、原子吸收光谱、ζ电位测定等现代表面及溶液分析检测技术,系统研究了磨矿介质、磨矿方式和药剂添加方式(捕收剂、调整剂)变化对五种矿物表面溶液性质及其在油酸钠、十二胺浮选体系中浮选行为的影响,并对其作用机理进行了初步探讨。
研究表明,油酸钠浮选体系中,采用氧化锆球介质磨矿比采用钢球介质磨矿更有利于碳酸盐矿物的浮选,而采用钢球介质磨矿对石英的浮选有明显的活化作用。十二胺浮选体系中,钢球介质磨矿对五种矿物的浮选都产生了抑制作用。这可能归因于钢球介质在磨矿过程中发生的电化学腐蚀。在磨损差异腐蚀原电池和电偶原电池的作用下,发生Fe的氧化和溶解氧的还原,并发生一系列氧化还原反应,通过矿浆(Eh,pH)的测定,根据Fe—H2O体系的Eh—pH图可判断在钢球介质磨矿后的矿浆中Fe元素主要以Fe(OH)3相存在,溶液检测表明,矿浆中同时还有可溶性铁组分存在,根据矿浆溶液的pH值条件、Eh—pH图及Fe2+和Fe3+的浓度对数图判断,溶液中存在的可溶性Fe组分应以Fe2+及其羟基络合物为主。溶液中的Fe2+离子在矿物表面的吸附及Fe(OH)3在矿物表面的吸附改变了矿物的表面电性和表面性质,由此对矿物的浮游性产生影响。
干、湿磨对四种碳酸盐矿物浮游性的影响规律不同,油酸钠浮选体系中,孔雀石氧化锆球介质湿磨的可浮性优于干磨,钢球介质干磨的可浮性优于湿磨。方解石两种介质干磨的可浮性优于湿磨。而菱锌矿和菱镁矿两种介质湿磨的可浮性优于干磨。十二胺浮选体系中,无论采用何种磨矿介质,湿磨孔雀石和方解石的可浮性优于干磨,而干磨菱锌矿和菱镁矿的可浮性优于湿磨。由XPS表面元素分析可知,干磨和湿磨过程使碳酸盐矿物表面阴离子和金属阳离子的分布产生差异,进而影响碳酸盐矿物在油酸钠和十二胺浮选体系中的浮游性。根据对碳酸盐矿物晶体结构差异及其溶解性的分析,作出了“碳酸盐干磨与湿磨浮选差异是溶解初态与溶解平衡态之间的浮选差异”的假设。通过油酸钠浮选体系搅拌时间试验及矿物干、湿磨后ζ电位的测定对该假设进行了初步验证。该假设对菱锌矿和菱镁矿具有较好的适应性,而对孔雀石和方解石的适应性不是很明显。
在单矿物浮选试验的基础上,进行了四种人工混合矿的浮选分离试验。其中孔雀石—石英体系在氧化锆球介质湿磨时获得了较好的浮选分离效果。相同条件下,氧化锆球介质磨矿时的选择性指数略高于钢球介质磨矿时的选择性指数。
Carbonate minerals are very important nonmetal mineral materials, an important mineral source of extracting metal, such as Fe、Mg、Mn、Pb、Zn、Cu and radioactive element and rare earth elements. It is of great economic significance to the world. With sulphide ore and rich ore resources exhausted day by day, the development and utilization of Carbonate minerals draw more and more attention. Calcite and dolomite coexists valuable minerals as gangue minerals usually. Many flotation processes involve the separate of valuable minerals with carbonate minerals. So it is of great significance to the flotation theory and industrial practice of salt minerals to research on the flotation behaviors of carbonate minerals.
The research of carbonate flotation is mainly focus on the develop of flotation reagents, flotation mechanism research and flotation process improvement. But the relationship between grinding and flotation of carbonate minerals is paid little attention by the mineral processing researchers. Grinding is not only substantial to decrease the size and consequently to liberate the valuable minerals from its gangue to allow for their selective recovery during mineral processing processes such as flotation but also to influence the flotation behavior significantly. Many researches and industrial practices showed that the interactions between the ore and the grinding environment affect sulphide both in recovery and selectivity. It has an important theory and practice significance to study the affect of grinding on the flotation behavior of carbonate minerals and to search for the relationship and regularity between physicochemical factors of grinding process and flotation behavior of carbonate minerals.
The study was undertaken using four carbonate minerals, including calcite, malachite, calamine and magnesite and a common gangue mineral, quartz. The influence of different grinding media, different grinding mode and the flotation reagents addition site on the flotation of five minerals using sodium oleate and lauryl amine as collector respectively was investigated using advanced surface and solution test technology such as X-ray photoelectron spectrometric (XPS), atomic absorption spectrometry (AAS) analysis andζpotential measure. And the effecting mechanism of grinding environment on floatability of five minerals was discussed.
It is showed that grinding with zirconia media is beneficial to the flotation of carbonate minerals using sodium oleate as collector than grinding with steel media, but grinding with steel media can activate the flotation of quartz obviously. And grinding with steel media depresses the flotation of all five minerals when using lauryl amine as collector. It may be attributed to the electrochemical corrosion of steel media in grinding. The iron will be oxidized and oxygen in the solution be reduced subjected to the abrasion diversity corrosion and galvanic corrosion. It is showed that the species in slurry after grinding with steel ball are mainly Fe(OH)3 based on the (Eh, pH) value of slurry and the Eh-pH phase digram of Fe-H2O system. And the solution test shows that there is soluble Fe phase in slurry solution, which may be Fe2+ and its hydroxy complexes. The adsorption of Fe(OH)3, Fe2+ and its hydroxy complexes in the minerals surface may change the surface electricity and surface properties, then effect the minerals floatability.
The influence law of wet and dry grinding on the flotation of four carbonate minerals is different. The floatability of malachite using sodium oleate as collector after wet grinding with zirconia media is better than dry grinding, but the floatability of malachite after dry grinding with steel media is better than wet grinding. The floatability of calcite after dry grinding is better than wet grinding, while the floatability of calamine and magnesite after dry grinding is worse than wet grinidng with both kind of grinding media. When using lauryl amine as collector, the floatability of calcite after wet grinding is better than dry grinding, while the floatability of calamine and magnesite after dry grinding is better than wet grinidng with both kind of grinding media.The XPS surface elements test shows that, wet and dry grinding process makes the distribution difference of surface anion and metal cation, then influence the floatability of carbonate minerals using sodium oleate and lauryl amine as collector. An assumption of "the flotation difference of carbonate after wet and dry grinding is the flotation difference between initial state and equilibrium state of carbonate dissolution" was made out according to the analysis of the carbonate crystal structure and solubility properties. And the "Stirring time" test andζpotential measurement were carried out to verify the validity of the assumption. The floatability of calamine and magnesite has good correlation with the assumption but the floatability of malachite and calcite shows a poor correlation.
Flotation separation experiment of four groups of mixed mineral was carried out using sodium oleate as collector. The separation effect of malachite-quartz system wet grinding with zirconia is relatively superior. The selectivity index of grinding with zirconia media is higher than grinding with steel media under the same condition.
引文
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