用全浮选法从攀枝花钒钛磁铁矿中回收钛的工艺及理论研究
摘要
攀枝花的钒钛磁铁矿是我国最重要的钛资源之一,矿石中主要的含钛工业矿物是钛铁矿。但由于该矿石成分复杂,钛含量较低,其回收是一大难题。多年以来有许多学者和科研人员对攀枝花的钒钛磁铁矿进行了大量深入而细致的研究工作,对矿石的综合利用提出过许多方案。
中国是世界上第一个实现了在工业规模上从复杂钒钛磁铁矿矿石中综合提取铁、钒、钛的国家,取得这样的成绩极为不易。攀枝花钒钛磁铁矿矿石中含铁和含钛的工业矿物分别是(钛)磁铁矿和钛铁矿。综合利用总的技术路线是首先选铁,由于钒主要赋存于(钛)磁铁矿中,因此选铁的同时钒进入铁精矿,在冶炼过程中进行回收。选铁的尾矿进行选钛。相比于选铁而言,钛铁矿的回收难度要大得多。为了更好地回收钛,相关企业和院校经过20多年的攻关,尽管已经形成涵盖重、磁、浮、电多种选矿方法、包括主流程和微细粒级浮选流程在内的相当复杂的钛回收系统,回收率有所提高,但仍然停留在20%左右。近年来主流工艺已发展成为“强磁——浮选”流程,虽然选矿方法有所简化,但钛铁矿回收率也仅有30%左右。而且仍然存在选矿方法多、流程复杂以及微细粒级钛铁矿难以有效回收等不足。随着我国钛工业的不断发展,对原料的需求与日俱增。如何更好地回收利用攀枝花钒钛磁铁矿资源,改进选矿方法,提高钛回收率显得十分紧迫,对我国钛工业的科技进步以及相关产业的发展意义重大。
本论文在“简化选矿方法,缩短选矿流程,全粒级入选,提高选矿指标”的基本技术路线指导下,创新性地提出了全粒级单一浮选方案。通过大量的试验对全粒级入选全浮选回收工艺进行了系统而深入的研究,解决了一系列技术难题,使得全浮选方案获得成功。这样就简化了选矿方法和流程,而且大幅度提高了选矿指标——钛精矿品位大于47%,回收率达到50%以上。本论文还通过单矿物的浮选机理研究为全浮选方案提供了理论依据。
在工艺方面,通过本论文的研究发现,要使攀枝花钒钛磁铁矿矿石中钛铁矿的全粒级全浮选方案取得成功,必须把握以下几个技术关键点：彻底的除铁预处理、高效捕收剂的采用、pH值的精确控制以及合理的流程结构。
在理论研究方面,本文首次发现了(钛)磁铁矿矿物在浮选中的“优先浮选效应”和“磁团聚效应”。这两个效应会对钛铁矿的浮选带来不利影响,因此浮选前彻底的除铁十分必要。在理论研究方面的另一个重要创新,是用实验证实了硫酸的活化作用,因而证明了硫酸在钛铁矿浮选过程中的“双重作用”,即既是pH值调整剂又是浮选活化剂。确定了pH值4.5～5.5是钛铁矿浮选的最佳pH值区间。在此区间内,钛铁矿具有最佳的可浮性和选择性,而且在浮选不同阶段对pH值有不同的要求,粗选和精选应分别选择pH值5和pH值4.5为宜。
本研究通过对不同捕收剂的对比和筛选,证明新型高效捕收剂SYB2#的采用是全浮选方案获得成功的关键之一。在对比了多种抑制剂对脉石的抑制效果以及对钛铁矿的分选性后,最终证明羧甲基纤维素是现有抑制剂中最为有效的,同时对羧甲基纤维素的抑制机理进行了探讨。
The vanadium titano-magnetite ore in Panzhihua district is one of the most important titanium resources in China. The major industrial titanium-containing mineral in the ore is ilmenite. However, because of the complexity of the ore composition, low grade of titanium, ilmenite recovery has always been a big problem. For many years, some scholars and mining workers have done a lot of depth and detailed research on the comprehensive utilization of vanadium titano-magnetite ore in Panzhihua district, and many suggestions about the comprehensive utilization of the ore were provided.
China is the first country that can extract iron, vanadium and titanium from complex vanadium titano-magnetite ore in industrial-scale, which is a great achievement. The general technical line of the comprehensive utilization of vanadium titano-magnetite ore in Panzhihua district is consisted of three parts. Firstly, we concentrate magnetite and titano-magnetite. Secondly, vanadium is recoverd from the titano-magnetite in metallurgy process. Finally, ilmenite is separated from the tailings of magnetic separation. The traditional separating process of ilmenite was consisted of gravity separation, magnetic separation, floatation and electrostatic separation. But the recovery of ilmenite is very low(about 20%). Nowerdays, the most popular separating process of ilmenite is "high intensity magnetic separation——floatation". This process is able to recover more ilmenite and the recovery is about 30%. But there are still many disadvantages. For example, the process is too long and complicated, the recovery of ilmenite is still low, ilmenite of fine fraction can not be recovered effectively and so on. The demand for raw materials is increasing with the continuous development of China's titanium industry. It is very important to improve the separating process of ilmenite and get better utilization of the vanadium titano-magnetite ore in Panzhihua district.
The basic technical line of the study is "simplifying the methods, shortening the process, all-partical-fraction and improving the indicators ". A systematic and in-depth study of recovering ilmenite from the vanadium titano-magnetite ore in Panzhihua district by all-partical-fraction-floatation process("APF-floatation") was carried out through a lot of experiments. A series of technical problems were solved. Finally, the "APF-floatation" is successful with the concentrate grade≥47% and recovery≥50%. Meanwhile, the study of monominerals floatation mechanism provides a theoretical basis.
Overall the "APF-floatation" has the following key technical points:complete removal of titano-magnetite pretreatment, the usage of efficient collector, precise control of pH value and reasonable flow structure.
The study discovered the titano-magnetite has "Priority Floating Effect" and "Magnetic Agglomeration Effect". The two effects have bad influence on ilmenite floatation. The pre-removal of residual magnetite before concentrating ilmenite from magnetic separation tailings by floatation is essential. It is noteworthy that the sulfuric acid is not only the pH conditioner but also the important activator in the ilmenite flotation. The activation was studied and confirmed in this paper. The effect of pH value on the performance of ilmenite floatation is investigated. It is found that a pH value range of 4.5-5.5 is the best one for ilmenite floatation, within which ilmenite presents the most optimal floatability and selectivity. And pH values of 5 and 4.5 are considered to be the best pH values for roughing and cleaning respectively according to the different demands.
This research compared the effects of a variety of collectors and depressants in ilmenite flotation by detailed monominerals floatation tests and carried out detailed analysis and discussion. Finally we consider that the usage of new and efficient collector SYB2# is the key to the success of "APF-floatation" in this study. The other conclusion is that carboxymethyl cellulose is the most effective depressant.
中国是世界上第一个实现了在工业规模上从复杂钒钛磁铁矿矿石中综合提取铁、钒、钛的国家,取得这样的成绩极为不易。攀枝花钒钛磁铁矿矿石中含铁和含钛的工业矿物分别是(钛)磁铁矿和钛铁矿。综合利用总的技术路线是首先选铁,由于钒主要赋存于(钛)磁铁矿中,因此选铁的同时钒进入铁精矿,在冶炼过程中进行回收。选铁的尾矿进行选钛。相比于选铁而言,钛铁矿的回收难度要大得多。为了更好地回收钛,相关企业和院校经过20多年的攻关,尽管已经形成涵盖重、磁、浮、电多种选矿方法、包括主流程和微细粒级浮选流程在内的相当复杂的钛回收系统,回收率有所提高,但仍然停留在20%左右。近年来主流工艺已发展成为“强磁——浮选”流程,虽然选矿方法有所简化,但钛铁矿回收率也仅有30%左右。而且仍然存在选矿方法多、流程复杂以及微细粒级钛铁矿难以有效回收等不足。随着我国钛工业的不断发展,对原料的需求与日俱增。如何更好地回收利用攀枝花钒钛磁铁矿资源,改进选矿方法,提高钛回收率显得十分紧迫,对我国钛工业的科技进步以及相关产业的发展意义重大。
本论文在“简化选矿方法,缩短选矿流程,全粒级入选,提高选矿指标”的基本技术路线指导下,创新性地提出了全粒级单一浮选方案。通过大量的试验对全粒级入选全浮选回收工艺进行了系统而深入的研究,解决了一系列技术难题,使得全浮选方案获得成功。这样就简化了选矿方法和流程,而且大幅度提高了选矿指标——钛精矿品位大于47%,回收率达到50%以上。本论文还通过单矿物的浮选机理研究为全浮选方案提供了理论依据。
在工艺方面,通过本论文的研究发现,要使攀枝花钒钛磁铁矿矿石中钛铁矿的全粒级全浮选方案取得成功,必须把握以下几个技术关键点：彻底的除铁预处理、高效捕收剂的采用、pH值的精确控制以及合理的流程结构。
在理论研究方面,本文首次发现了(钛)磁铁矿矿物在浮选中的“优先浮选效应”和“磁团聚效应”。这两个效应会对钛铁矿的浮选带来不利影响,因此浮选前彻底的除铁十分必要。在理论研究方面的另一个重要创新,是用实验证实了硫酸的活化作用,因而证明了硫酸在钛铁矿浮选过程中的“双重作用”,即既是pH值调整剂又是浮选活化剂。确定了pH值4.5～5.5是钛铁矿浮选的最佳pH值区间。在此区间内,钛铁矿具有最佳的可浮性和选择性,而且在浮选不同阶段对pH值有不同的要求,粗选和精选应分别选择pH值5和pH值4.5为宜。
本研究通过对不同捕收剂的对比和筛选,证明新型高效捕收剂SYB2#的采用是全浮选方案获得成功的关键之一。在对比了多种抑制剂对脉石的抑制效果以及对钛铁矿的分选性后,最终证明羧甲基纤维素是现有抑制剂中最为有效的,同时对羧甲基纤维素的抑制机理进行了探讨。
The vanadium titano-magnetite ore in Panzhihua district is one of the most important titanium resources in China. The major industrial titanium-containing mineral in the ore is ilmenite. However, because of the complexity of the ore composition, low grade of titanium, ilmenite recovery has always been a big problem. For many years, some scholars and mining workers have done a lot of depth and detailed research on the comprehensive utilization of vanadium titano-magnetite ore in Panzhihua district, and many suggestions about the comprehensive utilization of the ore were provided.
China is the first country that can extract iron, vanadium and titanium from complex vanadium titano-magnetite ore in industrial-scale, which is a great achievement. The general technical line of the comprehensive utilization of vanadium titano-magnetite ore in Panzhihua district is consisted of three parts. Firstly, we concentrate magnetite and titano-magnetite. Secondly, vanadium is recoverd from the titano-magnetite in metallurgy process. Finally, ilmenite is separated from the tailings of magnetic separation. The traditional separating process of ilmenite was consisted of gravity separation, magnetic separation, floatation and electrostatic separation. But the recovery of ilmenite is very low(about 20%). Nowerdays, the most popular separating process of ilmenite is "high intensity magnetic separation——floatation". This process is able to recover more ilmenite and the recovery is about 30%. But there are still many disadvantages. For example, the process is too long and complicated, the recovery of ilmenite is still low, ilmenite of fine fraction can not be recovered effectively and so on. The demand for raw materials is increasing with the continuous development of China's titanium industry. It is very important to improve the separating process of ilmenite and get better utilization of the vanadium titano-magnetite ore in Panzhihua district.
The basic technical line of the study is "simplifying the methods, shortening the process, all-partical-fraction and improving the indicators ". A systematic and in-depth study of recovering ilmenite from the vanadium titano-magnetite ore in Panzhihua district by all-partical-fraction-floatation process("APF-floatation") was carried out through a lot of experiments. A series of technical problems were solved. Finally, the "APF-floatation" is successful with the concentrate grade≥47% and recovery≥50%. Meanwhile, the study of monominerals floatation mechanism provides a theoretical basis.
Overall the "APF-floatation" has the following key technical points:complete removal of titano-magnetite pretreatment, the usage of efficient collector, precise control of pH value and reasonable flow structure.
The study discovered the titano-magnetite has "Priority Floating Effect" and "Magnetic Agglomeration Effect". The two effects have bad influence on ilmenite floatation. The pre-removal of residual magnetite before concentrating ilmenite from magnetic separation tailings by floatation is essential. It is noteworthy that the sulfuric acid is not only the pH conditioner but also the important activator in the ilmenite flotation. The activation was studied and confirmed in this paper. The effect of pH value on the performance of ilmenite floatation is investigated. It is found that a pH value range of 4.5-5.5 is the best one for ilmenite floatation, within which ilmenite presents the most optimal floatability and selectivity. And pH values of 5 and 4.5 are considered to be the best pH values for roughing and cleaning respectively according to the different demands.
This research compared the effects of a variety of collectors and depressants in ilmenite flotation by detailed monominerals floatation tests and carried out detailed analysis and discussion. Finally we consider that the usage of new and efficient collector SYB2# is the key to the success of "APF-floatation" in this study. The other conclusion is that carboxymethyl cellulose is the most effective depressant.
引文
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