微细粒钛铁矿浮选理论与技术研究
摘要
我国90%以上的钛资源蕴藏于钒钛磁铁矿中。该类型矿石中微细粒钛铁矿的回收一直是矿物加工领域公认的难题,但总体来看,长期存在着资源利用率偏低和浮选基础理论研究薄弱等问题。本文采用多种现代测试技术,结合理论分析和试验研究,对该体系中矿物表面组分与性质、浮选剂分子间的界面组装及矿物颗粒间的界面作用等内容进行了细致系统的研究,形成了钛铁矿浮选体系“固液界面离子选择性迁移-表面组分可控组装”的浮选分离调控机制,并以此为基础开发了攀枝花微细粒钛铁矿浮选新技术原型。主要研究内容和创新如下：
(1)固液界面离子的选择性迁移与捕收剂定向吸附
采用XPS、红外光谱和动电位等表面分析方法,发现了钛铁矿浮选体系固液界面离子迁移选择性、捕收剂吸附定位的差异性及二者之间的关联,深入揭示了钛铁矿浮选体系的内在机制。
攀枝花钛铁矿与脉石矿物钛辉石表面均含有Ti、Fe、Ca、Mg等元素,两种矿物表面Ca、Mg的溶解行为显著强于Ti和Fe。弱酸性矿浆环境中,固液界面发生离子选择性迁移与捕收剂定向吸附两个过程。对于钛铁矿,表面溶解过程中Fe2+被大量氧化为Fe3+,后者与油酸钠作用能力更强,进而有利于油酸钠的吸附；对于钛辉石,在表面溶解过程中Ca2+、Mg2+大量迁移至矿浆中,而Ca2+、Mg2+是钛辉石与油酸钠作用的主要活性质点,导致油酸钠的吸附减弱。在弱碱性矿浆环境中,两种矿物表面离子迁移行为较弱,而且均以钙镁为主要活性质点与油酸钠作用。
基于以上结果,提出了低pH环境强化溶解与弱酸性环境中超声助溶两种矿物界面性质强化调控措施,以增大二者的可浮性差异。
(2)固液界面多组分浮选剂分子间组装机制
通过对组合药剂的表面活性、吸附机制以及矿物可浮性的研究,探讨了矿物表面捕收剂分子间组装的协同作用与调整剂分子间组装的竞争吸附,为浮选药剂制度的制定提供依据。
螯合剂、阴离子表面活性剂以及非离子型表面活性剂三类浮选剂与油酸钠组合使用可以增强对钛铁矿的捕收性能。苯甲羟肟酸与油酸钠的组合使药剂降低表面张力的能力减弱,但二者均可在钛铁矿表面发生化学作用,使组合药剂吸附更牢固；十二烷基硫酸钠使药剂降低表面张力的能力略有增强,可以依靠静电作用与油酸钠共同吸附于钛铁矿表面；TX-100自身难以在钛铁矿表面吸附,但可以提高药剂降低表面张力的效率,在与油酸钠共同作用时在钛铁矿表面发生共吸附。
一定条件下,调整剂水玻璃、CMC与捕收剂油酸钠在两种矿物表面发生竞争吸附。在钛铁矿表面三种药剂的吸附能力强弱顺序为油酸钠>CMC>水玻璃；而在钛辉石表面则是水玻璃>CMC>油酸钠。
(3)同异相矿物颗粒间的界面交互作用与调控
利用浮选与沉降试验、粒度分析和扫描电镜等方法,结合颗粒间相互作用能理论计算,考查了矿物颗粒间的异相凝聚、选择性絮凝与载体作用等界面作用,及其与强化微细粒矿物回收的关系。
细粒钛辉石可与钛铁矿发生异相凝聚而严重影响钛铁矿的可浮性,水玻璃对二者的异相凝聚具有良好的分散作用；水玻璃与CMC共同作用可以实现微细粒钛铁矿的选择性絮凝,形成的钛铁矿絮团可与捕收剂作用进行絮团浮选；油酸钠可以使矿物颗粒产生疏水聚团,钛铁矿粗细粒共存体系存在白载体作用,控制载体比例,进行载体／聚团浮选可显著提高细粒钛铁矿的回收率。
DLVO和EDLVO理论计算表明,钛铁矿与钛辉石颗粒间异相凝聚的产生及分散的本质在于矿物表面电性的调控,钛铁矿自载体作用产生的前提是调控矿物表面润湿性,使颗粒间产生疏水作用能。
(4)攀枝花钛铁矿浮选技术研究
开发了两种钛铁矿浮选新技术,为攀枝花钛铁矿资源的高效利用提供了技术支撑。
针对原矿品位9.00%左右的攀枝花钛铁矿,采用“全粒级絮团浮选”新技术进行直接浮选,开路试验得到Ti02品位47.90%,回收率35.07%的钛精矿,尾矿Ti02品位降低到2.07%；采用“分级磁选-载体／聚团浮选"新技术,闭路试验Ti02品位47.93%,回收率高达52.11%。
In china, more than90percent titanium resources are reserved in vanadic titano-magnetite deposit. The flotation treatment of ilmenite in this type of ore has always been the world-class problem and research emphasis in mineral processing field. In general, there are still some deficiencies needed to be improved, such as the low efficiency of resource utilization and weak theoretical research. Using various modern analysis technologies and combining theoretical investigation with experimental study, this dissertation has done detailed and systematical researches in ilmenite flotation system, including the interfacial composition and properties, the interfacial assembly of the flotation reagents and the interface interaction between particles, etc.. Basing on above-mentioned researches, this dissertation resultantly has established a novel separation principle of "ion selective migration and components controllable assembly on solid-liquid interface", and proposed innovative technical prototypes to process Panzhihua ilmenite. Main conclusions and innovations of this dissertation are listed as follows:
1. Ion selective migration and collector directional adsorption on solid-liquid interface
Adopting the surface analysis methods such as X-ray photoelectron spectroscopy(XPS), infrared spectroscopic(FTIR) and zeta potential, this dissertation has discovered the selectivity of ion migration behavior, the difference of collector adsorption location, and the connection between these two processes, well revealing the internal mechanism of the collector adsorption process in ilmenite flotation.
Same elements such as Ti、Fe、Ca、Mg exist on the surface of both ilmenite and titanaugite (the gangue mineral), and the dissolution behavior of the Ca、 Mg is much more remarkable than that of Ti and Fe. In a weak acid environment, ion migration and collector adsorption on solid-liquid interface would take place. On the surface of ilmenite, surface dissolution is beneficial to the oxidation from Fe2+to Fe3+which has a much stronger reaction with oleat, therefore the adsorption is strengthened. As for titanaugite, Ca2+and Mg2+substantially transform into the pulp during surface dissolution process, while Ca2+and Mg2+are the main active points reacting with sodium oleate, so the absorption would be weakened. In a weak alkalic pulp environment, the ion migration trend becomes weakly, and Ca and Mg play a leading role in the adsorption of the both minerals.
Based on the above results, to enlarge the floatability difference between these two minerals, pre-treatment methods of strengthening dissolution in lower pH environment and assistant dissolution by ultrasonic were proposed.
2. Assembly mechanism of multicomponent flotation reagents on the surface of minerals
By studying the surface activity, adsorption mechanism, and flotation performance of combined reagents, the synergistic effect of collectors and competitive adsorption of regulators were discussed, providing a basis for establishing flotation reagent system.
Combining sodium oleate with some flotation reagents could enhance their collection property on ilmenite, such as chelating agent, anionic surfactant and nonionic surfactant. Although the combination of benzyl hydroxamic acid and sodium oleate would weaken the ability for reducing the surface tension, both of them could form chemical absorption on the mineral surface, which could fasten the absorption. Sodium dodecyl sulfate could slightly enhance the ability for reducing the surface tension, and it can be absorbed on the mineral surface together with sodium oleate by electrostatic interaction. TX-100can't be adsorbed on the surface of ilmenite by itself, but coadsorption could occur when it is combined with sodium oleate, and TX-100could significantly improve the efficiency for reducing the surface tension.
Under certain condition, competitive absorption would take place on the two mineral surfaces when waterglass, CMC and sodium oleate are in coexistence. The intensity sequence of absorption ability on surface of ilmenite is:sodium oleate>CMC>waterglass; while for titanaugite, the sequence would be:waterglass> CMC> sodium oleate.
3. Interface interaction and regulation between homophase/ heterogeneous particles
By flotation and sedimentation test, particle size analysis and scanning electron microscope (SEM) combining the interaction energy calculation, heterocoagulation, selective flocculation and carrier effect were studied, and the relationship with the enhancement of fine particles flotation was also analysed.
Heterocoagulation between fine titanaugite particles and ilmenite particles, having an adverse impact on the floatability of ilmenite, could be dispersed by waterglass. Selective flocculation flotation could be realized by the combination of water glass and CMC. Hydrophobic agglomeration would be observed when sodium oleate is added, as for ilmenite, it is found that autogenous-carrier effect exerts between fine and coarse particles, and the floatability of fine particles could be increased significantly when carrier proportion is well controlled.
The calculations from DLVO and EDLVO theory show that, the essence of generation and dispersion of heterocoagulation is the regulation of surface electricity, and the precondition of autogenous-carrier effect is the regulation of surface wettability, which brings about the hydrophobic property among particles.
4. Flotation technology of Panzhihua ilmenite
Two novel flotation technologies developed for Panzhihua ilmenite ore, greatly enhance the resource utilization of Panzhihua ilmenite.
The Panzhihua ilmenite with TiO2grade about9.00%is used as raw material for flotation tests. By open circuit test of "Whole size fraction flocculation flotation" technology process, the grade and recovery of obtained concentrate (calculated by TiO2) are47.90%and35.07%, respectively, the grade of TiO2in tailing as low as2.07%. By close circuit test of "coarse and fine particles classification, respective magnetic separation, and mixed flotation" technology process, the grade and recovery of obtained concentrate (calculated by TiO2) are47.93%and52.11%, respectively.
(1)固液界面离子的选择性迁移与捕收剂定向吸附
采用XPS、红外光谱和动电位等表面分析方法,发现了钛铁矿浮选体系固液界面离子迁移选择性、捕收剂吸附定位的差异性及二者之间的关联,深入揭示了钛铁矿浮选体系的内在机制。
攀枝花钛铁矿与脉石矿物钛辉石表面均含有Ti、Fe、Ca、Mg等元素,两种矿物表面Ca、Mg的溶解行为显著强于Ti和Fe。弱酸性矿浆环境中,固液界面发生离子选择性迁移与捕收剂定向吸附两个过程。对于钛铁矿,表面溶解过程中Fe2+被大量氧化为Fe3+,后者与油酸钠作用能力更强,进而有利于油酸钠的吸附；对于钛辉石,在表面溶解过程中Ca2+、Mg2+大量迁移至矿浆中,而Ca2+、Mg2+是钛辉石与油酸钠作用的主要活性质点,导致油酸钠的吸附减弱。在弱碱性矿浆环境中,两种矿物表面离子迁移行为较弱,而且均以钙镁为主要活性质点与油酸钠作用。
基于以上结果,提出了低pH环境强化溶解与弱酸性环境中超声助溶两种矿物界面性质强化调控措施,以增大二者的可浮性差异。
(2)固液界面多组分浮选剂分子间组装机制
通过对组合药剂的表面活性、吸附机制以及矿物可浮性的研究,探讨了矿物表面捕收剂分子间组装的协同作用与调整剂分子间组装的竞争吸附,为浮选药剂制度的制定提供依据。
螯合剂、阴离子表面活性剂以及非离子型表面活性剂三类浮选剂与油酸钠组合使用可以增强对钛铁矿的捕收性能。苯甲羟肟酸与油酸钠的组合使药剂降低表面张力的能力减弱,但二者均可在钛铁矿表面发生化学作用,使组合药剂吸附更牢固；十二烷基硫酸钠使药剂降低表面张力的能力略有增强,可以依靠静电作用与油酸钠共同吸附于钛铁矿表面；TX-100自身难以在钛铁矿表面吸附,但可以提高药剂降低表面张力的效率,在与油酸钠共同作用时在钛铁矿表面发生共吸附。
一定条件下,调整剂水玻璃、CMC与捕收剂油酸钠在两种矿物表面发生竞争吸附。在钛铁矿表面三种药剂的吸附能力强弱顺序为油酸钠>CMC>水玻璃；而在钛辉石表面则是水玻璃>CMC>油酸钠。
(3)同异相矿物颗粒间的界面交互作用与调控
利用浮选与沉降试验、粒度分析和扫描电镜等方法,结合颗粒间相互作用能理论计算,考查了矿物颗粒间的异相凝聚、选择性絮凝与载体作用等界面作用,及其与强化微细粒矿物回收的关系。
细粒钛辉石可与钛铁矿发生异相凝聚而严重影响钛铁矿的可浮性,水玻璃对二者的异相凝聚具有良好的分散作用；水玻璃与CMC共同作用可以实现微细粒钛铁矿的选择性絮凝,形成的钛铁矿絮团可与捕收剂作用进行絮团浮选；油酸钠可以使矿物颗粒产生疏水聚团,钛铁矿粗细粒共存体系存在白载体作用,控制载体比例,进行载体／聚团浮选可显著提高细粒钛铁矿的回收率。
DLVO和EDLVO理论计算表明,钛铁矿与钛辉石颗粒间异相凝聚的产生及分散的本质在于矿物表面电性的调控,钛铁矿自载体作用产生的前提是调控矿物表面润湿性,使颗粒间产生疏水作用能。
(4)攀枝花钛铁矿浮选技术研究
开发了两种钛铁矿浮选新技术,为攀枝花钛铁矿资源的高效利用提供了技术支撑。
针对原矿品位9.00%左右的攀枝花钛铁矿,采用“全粒级絮团浮选”新技术进行直接浮选,开路试验得到Ti02品位47.90%,回收率35.07%的钛精矿,尾矿Ti02品位降低到2.07%；采用“分级磁选-载体／聚团浮选"新技术,闭路试验Ti02品位47.93%,回收率高达52.11%。
In china, more than90percent titanium resources are reserved in vanadic titano-magnetite deposit. The flotation treatment of ilmenite in this type of ore has always been the world-class problem and research emphasis in mineral processing field. In general, there are still some deficiencies needed to be improved, such as the low efficiency of resource utilization and weak theoretical research. Using various modern analysis technologies and combining theoretical investigation with experimental study, this dissertation has done detailed and systematical researches in ilmenite flotation system, including the interfacial composition and properties, the interfacial assembly of the flotation reagents and the interface interaction between particles, etc.. Basing on above-mentioned researches, this dissertation resultantly has established a novel separation principle of "ion selective migration and components controllable assembly on solid-liquid interface", and proposed innovative technical prototypes to process Panzhihua ilmenite. Main conclusions and innovations of this dissertation are listed as follows:
1. Ion selective migration and collector directional adsorption on solid-liquid interface
Adopting the surface analysis methods such as X-ray photoelectron spectroscopy(XPS), infrared spectroscopic(FTIR) and zeta potential, this dissertation has discovered the selectivity of ion migration behavior, the difference of collector adsorption location, and the connection between these two processes, well revealing the internal mechanism of the collector adsorption process in ilmenite flotation.
Same elements such as Ti、Fe、Ca、Mg exist on the surface of both ilmenite and titanaugite (the gangue mineral), and the dissolution behavior of the Ca、 Mg is much more remarkable than that of Ti and Fe. In a weak acid environment, ion migration and collector adsorption on solid-liquid interface would take place. On the surface of ilmenite, surface dissolution is beneficial to the oxidation from Fe2+to Fe3+which has a much stronger reaction with oleat, therefore the adsorption is strengthened. As for titanaugite, Ca2+and Mg2+substantially transform into the pulp during surface dissolution process, while Ca2+and Mg2+are the main active points reacting with sodium oleate, so the absorption would be weakened. In a weak alkalic pulp environment, the ion migration trend becomes weakly, and Ca and Mg play a leading role in the adsorption of the both minerals.
Based on the above results, to enlarge the floatability difference between these two minerals, pre-treatment methods of strengthening dissolution in lower pH environment and assistant dissolution by ultrasonic were proposed.
2. Assembly mechanism of multicomponent flotation reagents on the surface of minerals
By studying the surface activity, adsorption mechanism, and flotation performance of combined reagents, the synergistic effect of collectors and competitive adsorption of regulators were discussed, providing a basis for establishing flotation reagent system.
Combining sodium oleate with some flotation reagents could enhance their collection property on ilmenite, such as chelating agent, anionic surfactant and nonionic surfactant. Although the combination of benzyl hydroxamic acid and sodium oleate would weaken the ability for reducing the surface tension, both of them could form chemical absorption on the mineral surface, which could fasten the absorption. Sodium dodecyl sulfate could slightly enhance the ability for reducing the surface tension, and it can be absorbed on the mineral surface together with sodium oleate by electrostatic interaction. TX-100can't be adsorbed on the surface of ilmenite by itself, but coadsorption could occur when it is combined with sodium oleate, and TX-100could significantly improve the efficiency for reducing the surface tension.
Under certain condition, competitive absorption would take place on the two mineral surfaces when waterglass, CMC and sodium oleate are in coexistence. The intensity sequence of absorption ability on surface of ilmenite is:sodium oleate>CMC>waterglass; while for titanaugite, the sequence would be:waterglass> CMC> sodium oleate.
3. Interface interaction and regulation between homophase/ heterogeneous particles
By flotation and sedimentation test, particle size analysis and scanning electron microscope (SEM) combining the interaction energy calculation, heterocoagulation, selective flocculation and carrier effect were studied, and the relationship with the enhancement of fine particles flotation was also analysed.
Heterocoagulation between fine titanaugite particles and ilmenite particles, having an adverse impact on the floatability of ilmenite, could be dispersed by waterglass. Selective flocculation flotation could be realized by the combination of water glass and CMC. Hydrophobic agglomeration would be observed when sodium oleate is added, as for ilmenite, it is found that autogenous-carrier effect exerts between fine and coarse particles, and the floatability of fine particles could be increased significantly when carrier proportion is well controlled.
The calculations from DLVO and EDLVO theory show that, the essence of generation and dispersion of heterocoagulation is the regulation of surface electricity, and the precondition of autogenous-carrier effect is the regulation of surface wettability, which brings about the hydrophobic property among particles.
4. Flotation technology of Panzhihua ilmenite
Two novel flotation technologies developed for Panzhihua ilmenite ore, greatly enhance the resource utilization of Panzhihua ilmenite.
The Panzhihua ilmenite with TiO2grade about9.00%is used as raw material for flotation tests. By open circuit test of "Whole size fraction flocculation flotation" technology process, the grade and recovery of obtained concentrate (calculated by TiO2) are47.90%and35.07%, respectively, the grade of TiO2in tailing as low as2.07%. By close circuit test of "coarse and fine particles classification, respective magnetic separation, and mixed flotation" technology process, the grade and recovery of obtained concentrate (calculated by TiO2) are47.93%and52.11%, respectively.
引文
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