织金新华磷矿稀土赋存状态及其在浮选、酸解过程中的行为研究
摘要
织金新华磷矿位于贵州省织金县,是一个超大型伴生稀土的中低品位磷矿床,P205品位平均为17.51%, IREO品位为0.05%-0.13%,已探明磷矿石储量13.34亿t,占贵州省磷矿储量的一半,稀土氧化物储量144.6万t,其中重稀土氧化钇占32.18%,在全国磷资源和稀土资源中均占有重要的地位。织金新华磷矿稀土储量大,但由于稀土品位低,且稀土以类质同象形式赋存于胶磷矿中,使在开发利用磷资源时,为稀土的有效回收造成了很大困难。本文所研究的织金新华磷矿,是按照工业大规模开采的方式进行取样的,具有很好的代表性。针对所取矿样,从磷矿稀土的赋存状态、浮选过程稀土的富集行为和酸解过程稀土的酸解行为等进行了系统的研究,并对磷矿酸解过程稀土的反应机理进行了深入分析,为该矿的综合开发利用提供理论依据。
通过织金新华磷矿稀土的赋存状态研究表明,矿石中稀土主要以钇(Y2O3)、镧(La2O3)、钕(Nd2O3)、铈(CeO2)四种元素为主,占稀土总量的81.20%。轻稀土含量稍微高于重稀土含量,占稀土总量分别为55.90%和42.15%；其中稀土钇(Y2O3)占稀土总量的32.18%,占重稀土总量的76.29%。并且矿石中稀土与磷成正相关关系,稀土总量与磷含量的相关系数为0.98191。胶磷矿单体矿物中除存在稀土的独立矿物独居石外,还新发现了稀土的独立矿物方铈石,但稀土的独立矿物数量极微,没有发现稀土钇的独立矿物,稀土元素主要以类质同象形式赋存于胶磷矿中。这种结构导致稀土极不易从磷矿中单独选取。
通过织金新华磷矿浮选过程稀土的行为研究表明,稀土主要富集在磷精矿中,并且WF-01是织金新华磷矿反浮选工艺中白云石矿物的有效捕收剂,采用磷酸作为抑制剂和矿浆pH值调整剂,在控制适宜的浮选条件下,磷精矿中∑REO的回收率达到90%,富集比达到1.50。本文利用一级浮选速率模型ε=ε∞(1-e-kt)推导出了反浮选速率模型ε=ε∞+(100-ε∞)e-k(t+θ),该模型可以很好地描述织金新华磷矿反浮选过程中浮选槽内产品含稀土磷矿物(以∑REO表示)和脉石矿物(以MgO表示)回收率随时间的变化规律,并以修正的浮选速率常数kmod和选择性指数SI来衡量含稀土磷矿物和脉石矿物分选效果的好坏。通过浮选正交动力学实验研究,捕收剂WF-01用量是影响∑REO修正速率常数kmod最主要的因素,而抑制剂H3P04用量是影响选择性指数SI最主要的因素。采用三维表面图和等高线线图对两种药剂组合方式下∑REO的浮选动力学参数变化进行表征时表明,磷矿反浮选时,如捕收剂WF-01用量为0.8 kg/t,为获得较好的含稀土磷矿物与白云石矿物的分选效果,可适当增加抑制剂H3P04用量。
通过织金新华磷矿酸解过程稀土的行为研究表明,溶液的酸度是影响稀土分布规律的主要因素。增加溶液中硫酸浓度或磷酸浓度均可使磷矿中∑REO进入溶液中的分布比例降到5%以下。织金新华磷矿中∑REO的酸解动力学可以用包含了自阻化因素的德罗兹多夫方程来很好的描述,拟合曲线的相关系数均在0.99以上。根据Arrenius方程对织金新华磷矿酸解过程P2O5的反应表观活化能计算,表明硫酸分解织金新华磷矿的主要反应为固态膜扩散控制过程,而对于磷矿中稀土的反应,也属于固态膜扩散控制过程。织金新华磷矿酸解过程稀土的反应机理研究表明,稀土与酸的反应包括四个主要过程：一是反应体系的氢离子(H+)、阴离子(SO42-、PO43-、H2PO4等)以及分子(H2SO4或H3PO4)等反应物向颗粒界面扩散的过程；二是磷矿颗粒界面稀土元素与反应物发生化学反应过程,反应物S042-或H2SO4浓度高,生成RE2(SO4)3的几率增加,PO43-、H2PO4或H3P04浓度高,生成REPO4或REH2PO42+的几率增加；三是生成物向反应主体系的扩散过程,生成的不溶性的REPO4沉积在颗粒表面硫酸钙结晶物形成的固体膜层中,生成的可溶性RE2(SO4)3、或REH2PO42+等通过扩散层扩散进入反应主体系。RE2(SO4)3的溶解度随温度的升高而显著下降,过饱和的RE2(SO4)3将生成结晶物沉积在固体膜层中；四是稀土被硫酸钙晶体包裹现象,磷矿颗粒界面硫酸钙的核晶速度很快,颗粒内部反应的稀土来不及通过扩散层,便被包裹进了硫酸钙晶体中,这也是造成稀土在磷石膏中的分布比例大于磷酸中分布比例的主要原因。
通过本文的研究,织金新华磷矿用于生产湿法磷酸,可以在磷矿酸解过程中采取增加溶液酸度的方法,能够使矿石中90%以上的稀土元素进入磷石膏,然后探寻从磷石膏中回收稀土的经济、合理有效的方法。
Xinhua phosphorite in Zhijin County of Guizhou is one of the super large-scale REE-bearing medium-low grade phosphorite deposits in Southwest of China. The proved up reserve of phosphorite ores was 13.34×108t, which accounts for about 50% of total phosphorite reserve of Guizhou Province. Previous investigations have revealed that the total reserve of REE oxide comes up to 140×104t, among which yttrium oxide accounts for 32.18% of the total REE oxide. The average contents of P2O5 in phosphorite was 17.51%, and the contents of EREO (which stands for the total REE oxides) ranges from 0.05% to 0.13%. This phosphorite is noted for its greatly abundant reserve of REE but considerably low contents of REE. Moreover, it is very difficult to recovery REE from ores due to the isomorphous substitution of REE for the lattices of calcium ion in collophanite. Nevertherless, the studying on recovering REE is still necessary at present. In this paper, the samples derived from mined ores in the big scale of industrial explotation. Hence, the samples were better representative for the studing on Zhijin Xinhua phosphorite ores. Based on the samples, the existing state of REE in ores, the enrichment rule of REE by flotation, the behavior and reacting mechaniism of REE disoluted by acid were systematiclly and deeply investigated in this paper. This research will provide the valuable reference for the development and utilization of Zhijin REE-bearing phosphorite deposits.
The exiting state of REE in Zhijin Xinhua phosphorite ores were investigated systematically. The results showed that Y2O3, La2O3, Nd2O3 and CeO2 were main four rare earth elements in ore, which accounted for 81.20%of∑REO. The contents of∑LREO (which stands for the total light rare earth oxides) were slishtly higher than those of∑HREO (which stands for the total heavy rare earth oxides), accounting for 55.90%and 42.15%of∑REO, respectively. Among∑REO, Y2O3 was most abundant, accounting for 32.18%of∑REO and 76.29%of∑HREO. Remarkably, there existed good positive correlationship between REE and phosphorus, and the correlation coefficient was 0.98191. There existed independent minerals of REE in single collophanite mineral, such as cerianite and monazite, moreove, cerianite was found first time, but the amount of them was extremely little. No independent mineral of yttrium has been found in this investigation. Therefore, REE were mainly present in the form of ions in the lattices of collophanite, which leaded to it extremely difficult to extract REE from phosphorites.
The enrichment rule of REE by flotation was investigated for Zhijin Xinhua phosphorite ores. The results indicated that REE can be.mainly enriched in concentrate by reverse flotation technology. Moreover, it has been found that a high flotation efficiency and excellent selectivity could be achieved when collector WF-01 was used to effectively collect dolomite minerals and other gangue minerals and phosphoric acid was used as phosphate minerals depressant and pH adjustment of pulp. The∑REO recovery rate of flotation concentrates came up to 90% and the enrichment ratio of∑REO in concentrates was up to 1.50. In addition, based on the classical first-order rate model ofε=ε∞(1-e-kt), the reverse flotation rate model ofε=ε∞+(100-ε∞)e-k(t+θ) was obtained, which could fit the data very well to describe the effect of flotation time on recovery rate of EREO and MgO in concentrate. Furthermore, a modified flotation rate constant kmod defined as theproduct ofε∞and k, i.e., kmod=ε∞·k and selectivity index SI defined as the ratio of the modifiedrate constant of valuables to the modified rate constant of gangue, i.e., SI=kmod1/kmod2, were also used to better measure the separability between bearing-REE phosphoric mineral and gangue mineral. The kinetics based on flotation Orthogonal experiment showed that the collector WF-01 dose was the most significant variable affecting kmod for∑REO, while depressant H3PO4 dosage affected the SI significantly. In order to further analyzed the effect of compounding reagents with WF-01 and H3PO4 on parameters kmod and SI, the response surface graphs and the contour graphs were drawn for kmod of∑REO, kmod of MgO and SI. The result indicated that the excellent separation between∑REO and MgO could be obtained by increasing depressant H3PO4 dosage in the condition of collector WF-01 dosage of 0.8 kg/t when reverse flotation were carried out for Zhijin Xinhua phosphorite ores.
The behaviors and reacting mechanisms of REE dissoluted by acid were studied deeply for Zhijin Xinhua phosphorite ores. It was found that the acidic value of solution was the main effect factor on the distribution of REE in products. The distribution proportions of∑REO in phosphoric acid solution could be decreased to lower than 5% by increasing sulphuric acid or phosphoric acid concentration in reacting solution. The kinetics of ores dissoluted by acid showed that the Drozdov equation , which taked into account the self-impeding effect, could describe the dissolution progress of∑REO of ore quite well. The correlation coefficient fitting experimental data was more than 0.99.The reaction apparent activation energy of P2O5 calculated by Arrenius equation indicated that the main reaction of Zhijin Xinhua phosphorite ores dissoluted by sulphuric acid was a diffusion control process, as well as for REE. In addition, the studing on the reacting mechanisms of REE dissoluted by acid showed that the reactions included four main processes. One was the reactants, such as ions of H+、SO42-、PO43- or H2PO4-, and molecule of H2SO4 or H3PO4, diffusing toward the particle interface of ore. Another was REE reacting with reactants in particle interface. RE2(SO4)3 would be obtained when there were high SO42- ion or H2SO4 molecule concentration, while REPO4 or REH2PO42+ would be obtained when there were high PO43-, H2PO4- or H3PO4 concentration. The third was the resultants diffusing toward the solution main system, in which the insoluble REPO4 or part of RE2(SO4)3 would be precipitated in the solid film formed by calcium sulphate crystal, while the soluble RE2(SO4)3 or REH2PO42+ diffusing toward the solution main system through diffusion layer. In addition, the phenomenon of REE being enwraped by calcium sulphate crystal was happened due to the fact that the speed of calcium sulphate crystalizing was faster than that of REE diffusing through solid film, which was the main reason that the distribution proportions of∑REO in phosphogypsum was more than that in phosphoric acid.
Based on the studying in this paper, The distribution proportions of IREO in phosphogypsum could come up to 90% by increasing solution acidic value in wet-phosphoric acid process. Then, economical and reasonable method will be seeked to recovery REE from phosphogypsum.
通过织金新华磷矿稀土的赋存状态研究表明,矿石中稀土主要以钇(Y2O3)、镧(La2O3)、钕(Nd2O3)、铈(CeO2)四种元素为主,占稀土总量的81.20%。轻稀土含量稍微高于重稀土含量,占稀土总量分别为55.90%和42.15%；其中稀土钇(Y2O3)占稀土总量的32.18%,占重稀土总量的76.29%。并且矿石中稀土与磷成正相关关系,稀土总量与磷含量的相关系数为0.98191。胶磷矿单体矿物中除存在稀土的独立矿物独居石外,还新发现了稀土的独立矿物方铈石,但稀土的独立矿物数量极微,没有发现稀土钇的独立矿物,稀土元素主要以类质同象形式赋存于胶磷矿中。这种结构导致稀土极不易从磷矿中单独选取。
通过织金新华磷矿浮选过程稀土的行为研究表明,稀土主要富集在磷精矿中,并且WF-01是织金新华磷矿反浮选工艺中白云石矿物的有效捕收剂,采用磷酸作为抑制剂和矿浆pH值调整剂,在控制适宜的浮选条件下,磷精矿中∑REO的回收率达到90%,富集比达到1.50。本文利用一级浮选速率模型ε=ε∞(1-e-kt)推导出了反浮选速率模型ε=ε∞+(100-ε∞)e-k(t+θ),该模型可以很好地描述织金新华磷矿反浮选过程中浮选槽内产品含稀土磷矿物(以∑REO表示)和脉石矿物(以MgO表示)回收率随时间的变化规律,并以修正的浮选速率常数kmod和选择性指数SI来衡量含稀土磷矿物和脉石矿物分选效果的好坏。通过浮选正交动力学实验研究,捕收剂WF-01用量是影响∑REO修正速率常数kmod最主要的因素,而抑制剂H3P04用量是影响选择性指数SI最主要的因素。采用三维表面图和等高线线图对两种药剂组合方式下∑REO的浮选动力学参数变化进行表征时表明,磷矿反浮选时,如捕收剂WF-01用量为0.8 kg/t,为获得较好的含稀土磷矿物与白云石矿物的分选效果,可适当增加抑制剂H3P04用量。
通过织金新华磷矿酸解过程稀土的行为研究表明,溶液的酸度是影响稀土分布规律的主要因素。增加溶液中硫酸浓度或磷酸浓度均可使磷矿中∑REO进入溶液中的分布比例降到5%以下。织金新华磷矿中∑REO的酸解动力学可以用包含了自阻化因素的德罗兹多夫方程来很好的描述,拟合曲线的相关系数均在0.99以上。根据Arrenius方程对织金新华磷矿酸解过程P2O5的反应表观活化能计算,表明硫酸分解织金新华磷矿的主要反应为固态膜扩散控制过程,而对于磷矿中稀土的反应,也属于固态膜扩散控制过程。织金新华磷矿酸解过程稀土的反应机理研究表明,稀土与酸的反应包括四个主要过程：一是反应体系的氢离子(H+)、阴离子(SO42-、PO43-、H2PO4等)以及分子(H2SO4或H3PO4)等反应物向颗粒界面扩散的过程；二是磷矿颗粒界面稀土元素与反应物发生化学反应过程,反应物S042-或H2SO4浓度高,生成RE2(SO4)3的几率增加,PO43-、H2PO4或H3P04浓度高,生成REPO4或REH2PO42+的几率增加；三是生成物向反应主体系的扩散过程,生成的不溶性的REPO4沉积在颗粒表面硫酸钙结晶物形成的固体膜层中,生成的可溶性RE2(SO4)3、或REH2PO42+等通过扩散层扩散进入反应主体系。RE2(SO4)3的溶解度随温度的升高而显著下降,过饱和的RE2(SO4)3将生成结晶物沉积在固体膜层中；四是稀土被硫酸钙晶体包裹现象,磷矿颗粒界面硫酸钙的核晶速度很快,颗粒内部反应的稀土来不及通过扩散层,便被包裹进了硫酸钙晶体中,这也是造成稀土在磷石膏中的分布比例大于磷酸中分布比例的主要原因。
通过本文的研究,织金新华磷矿用于生产湿法磷酸,可以在磷矿酸解过程中采取增加溶液酸度的方法,能够使矿石中90%以上的稀土元素进入磷石膏,然后探寻从磷石膏中回收稀土的经济、合理有效的方法。
Xinhua phosphorite in Zhijin County of Guizhou is one of the super large-scale REE-bearing medium-low grade phosphorite deposits in Southwest of China. The proved up reserve of phosphorite ores was 13.34×108t, which accounts for about 50% of total phosphorite reserve of Guizhou Province. Previous investigations have revealed that the total reserve of REE oxide comes up to 140×104t, among which yttrium oxide accounts for 32.18% of the total REE oxide. The average contents of P2O5 in phosphorite was 17.51%, and the contents of EREO (which stands for the total REE oxides) ranges from 0.05% to 0.13%. This phosphorite is noted for its greatly abundant reserve of REE but considerably low contents of REE. Moreover, it is very difficult to recovery REE from ores due to the isomorphous substitution of REE for the lattices of calcium ion in collophanite. Nevertherless, the studying on recovering REE is still necessary at present. In this paper, the samples derived from mined ores in the big scale of industrial explotation. Hence, the samples were better representative for the studing on Zhijin Xinhua phosphorite ores. Based on the samples, the existing state of REE in ores, the enrichment rule of REE by flotation, the behavior and reacting mechaniism of REE disoluted by acid were systematiclly and deeply investigated in this paper. This research will provide the valuable reference for the development and utilization of Zhijin REE-bearing phosphorite deposits.
The exiting state of REE in Zhijin Xinhua phosphorite ores were investigated systematically. The results showed that Y2O3, La2O3, Nd2O3 and CeO2 were main four rare earth elements in ore, which accounted for 81.20%of∑REO. The contents of∑LREO (which stands for the total light rare earth oxides) were slishtly higher than those of∑HREO (which stands for the total heavy rare earth oxides), accounting for 55.90%and 42.15%of∑REO, respectively. Among∑REO, Y2O3 was most abundant, accounting for 32.18%of∑REO and 76.29%of∑HREO. Remarkably, there existed good positive correlationship between REE and phosphorus, and the correlation coefficient was 0.98191. There existed independent minerals of REE in single collophanite mineral, such as cerianite and monazite, moreove, cerianite was found first time, but the amount of them was extremely little. No independent mineral of yttrium has been found in this investigation. Therefore, REE were mainly present in the form of ions in the lattices of collophanite, which leaded to it extremely difficult to extract REE from phosphorites.
The enrichment rule of REE by flotation was investigated for Zhijin Xinhua phosphorite ores. The results indicated that REE can be.mainly enriched in concentrate by reverse flotation technology. Moreover, it has been found that a high flotation efficiency and excellent selectivity could be achieved when collector WF-01 was used to effectively collect dolomite minerals and other gangue minerals and phosphoric acid was used as phosphate minerals depressant and pH adjustment of pulp. The∑REO recovery rate of flotation concentrates came up to 90% and the enrichment ratio of∑REO in concentrates was up to 1.50. In addition, based on the classical first-order rate model ofε=ε∞(1-e-kt), the reverse flotation rate model ofε=ε∞+(100-ε∞)e-k(t+θ) was obtained, which could fit the data very well to describe the effect of flotation time on recovery rate of EREO and MgO in concentrate. Furthermore, a modified flotation rate constant kmod defined as theproduct ofε∞and k, i.e., kmod=ε∞·k and selectivity index SI defined as the ratio of the modifiedrate constant of valuables to the modified rate constant of gangue, i.e., SI=kmod1/kmod2, were also used to better measure the separability between bearing-REE phosphoric mineral and gangue mineral. The kinetics based on flotation Orthogonal experiment showed that the collector WF-01 dose was the most significant variable affecting kmod for∑REO, while depressant H3PO4 dosage affected the SI significantly. In order to further analyzed the effect of compounding reagents with WF-01 and H3PO4 on parameters kmod and SI, the response surface graphs and the contour graphs were drawn for kmod of∑REO, kmod of MgO and SI. The result indicated that the excellent separation between∑REO and MgO could be obtained by increasing depressant H3PO4 dosage in the condition of collector WF-01 dosage of 0.8 kg/t when reverse flotation were carried out for Zhijin Xinhua phosphorite ores.
The behaviors and reacting mechanisms of REE dissoluted by acid were studied deeply for Zhijin Xinhua phosphorite ores. It was found that the acidic value of solution was the main effect factor on the distribution of REE in products. The distribution proportions of∑REO in phosphoric acid solution could be decreased to lower than 5% by increasing sulphuric acid or phosphoric acid concentration in reacting solution. The kinetics of ores dissoluted by acid showed that the Drozdov equation , which taked into account the self-impeding effect, could describe the dissolution progress of∑REO of ore quite well. The correlation coefficient fitting experimental data was more than 0.99.The reaction apparent activation energy of P2O5 calculated by Arrenius equation indicated that the main reaction of Zhijin Xinhua phosphorite ores dissoluted by sulphuric acid was a diffusion control process, as well as for REE. In addition, the studing on the reacting mechanisms of REE dissoluted by acid showed that the reactions included four main processes. One was the reactants, such as ions of H+、SO42-、PO43- or H2PO4-, and molecule of H2SO4 or H3PO4, diffusing toward the particle interface of ore. Another was REE reacting with reactants in particle interface. RE2(SO4)3 would be obtained when there were high SO42- ion or H2SO4 molecule concentration, while REPO4 or REH2PO42+ would be obtained when there were high PO43-, H2PO4- or H3PO4 concentration. The third was the resultants diffusing toward the solution main system, in which the insoluble REPO4 or part of RE2(SO4)3 would be precipitated in the solid film formed by calcium sulphate crystal, while the soluble RE2(SO4)3 or REH2PO42+ diffusing toward the solution main system through diffusion layer. In addition, the phenomenon of REE being enwraped by calcium sulphate crystal was happened due to the fact that the speed of calcium sulphate crystalizing was faster than that of REE diffusing through solid film, which was the main reason that the distribution proportions of∑REO in phosphogypsum was more than that in phosphoric acid.
Based on the studying in this paper, The distribution proportions of IREO in phosphogypsum could come up to 90% by increasing solution acidic value in wet-phosphoric acid process. Then, economical and reasonable method will be seeked to recovery REE from phosphogypsum.
引文
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