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By Katsutoshi Inoue

The sulfuric acid leaching of spent hydrodesulfurization catalysts yields an acidic solution rich in rare metals such as molybdenum, vanadium, cobalt, and nickel in addition to aluminum. For the purpose of separating and recovering the rare metals from the solution, basic solvent extraction characteristics of the metals involved with commercially available acidic organophosphorus reagents like TR-83, PC-88A, PIA-8 and CYANEX 272 as well as aliphatic alpha-hydroxyoxime LIX 63 from sulfuric acid media were investigated in the present work. It was demonstrated that CYANEX 272, PIA-8 and LIX 63 possessed excellent selectivity for molybdenum and vanadium over the other metals at comparatively low pH. Further, recovery of molybdenum and vanadium from the total leach liquor by the selected extractants was discussed. Additionally, in order to achieve preferential separation and recovery of cobalt and nickel over an appreciable amount of aluminum from the raffinate obtained after recovering molybdenum and vanadium, a systematic investigation was conducted on synergistic extraction behaviors of the mixed solvents of LIX 63 in combination with a series of acidic extractants such as CYANEX 272, PIA-8, PC-88A, D2EHPA, TR-83 and OPEHPA for cobalt, nickel and aluminum. It was elucidated that all of these mixtures could exhibit a good synergistic effect for extraction of cobalt and nickel, and that the lower the pKa of the acidic extractants, the greater the synergism. Contrarily, the extraction of aluminum, was considerably suppressed by LIX 63. Effective extraction of cobalt and nickel away from aluminum was accomplished from the sulfate solution at low pH (1.0 - 2.5) with the mixtures. In particular, the mixtures consisting of LIX 63 and CYANEX 272 or PIA-8 appeared to be the most feasible and economic from an industrial point of view, yielding acceptable separation efficiency for cobalt and nickel over aluminum and .a low acidity requirement for stripping cobalt and nickel as well as negligible degradation of LIX 63. Aluminum can be readily recovered as sulfate salt from the raffinate obtained after recovering molybdenum, vanadium, cobalt and nickel as outlined above by conventional crystallization method.

Jan 1, 1995

By Zhenzhong Bian, Ruiyang Zhang, Xiaofeng Zhong, Zhangxuan Ning, Yuanping Zhang, Jie Lu, Airan Zhang

This study addressed the separation and recovery of vanadium(IV), iron, and titanium from synthetic and real leach solutions of vanadium-bearing titanomagnetite using extractant P204 (di-(2-ethylhexyl) phosphate) and P507 (2-ethylhexyl hydrogen- 2-ethylhexyl phosphonate). Based on the speciation analysis of vanadium in sulfuric acid medium, the single-stage extraction efficiency of vanadium, iron, and titanium was 94.21%, 3.45%, and 5.32%, respectively, under the optimal extraction condition of P204-P507 concentration of 15% (v/v), P204 to P507 ratio of 3:1 (v/v), TBP (Tributyl phosphate) concentration of 5%, sulfonated kerosene concentration of 80%, initial pH of 1.8, contact time of 8 min, and phase ratio (O/A) of 2:1. By confirming the predictions of the McCabe-Thiele diagram, a five-stage countercurrent extraction was carried out and the desirable extraction efficiency for vanadium reached 98.13%. The maximum co-extraction coefficient and distribution ratio of vanadium were 2.58 and 26.23, respectively. The stripping efficiencies and concentrations of a vanadium-rich solution by three stages of countercurrent experiments with 20 vol.% sulfuric acid reached 99.14% and 0.58 g/L, respectively, while almost all of the titanium remained in the organic phase. The mechanism of synergistic extraction between hydrogen ions of P–O–H and VO2+ in acidic conditions was confirmed by ATR-FTIR spectroscopy and molecular structure derivation. Besides, the separated impurity ions ( Fe2+) after oxidation, precipitation, and roasting process form a qualified iron oxide pigment with a total iron content of 97.2%.

Apr 25, 2023

By CHENGLONG XU, HAORAN LI, YALI FENG, JINRONG JU, Shunliang Liu

With the depletion of mineral resources and the growing demand for metal resources from industrial development, the recovery of metal resources from secondary resources has attracted increased attention. Among all secondary resources, spent catalyst is one of the most important as it contains valuable metals such as vanadium, nickel, molybdenum, cobalt, and aluminum. Compared with the extraction of metals from minerals, the recovery of valuable metals from spent catalysts has the advantages of a simple process, a short production cycle, lower investment cost, and less environmental impact.

Apr 1, 2023

By CHENGLONG XU, HAORAN LI, YALI FENG, JINRONG JU, Shunliang Liu

In order to realize the resource utilization of spent hydrodesulfurization catalyst, a solvent extraction-oxalic acid precipitation process is studied in this paper for efficiently recovering vanadium, nickel, and aluminum from the acid leaching solution of spent hydrodesulfurization catalyst. The process conditions for extracting vanadium with Cyanex 272 and precipitating nickel using oxalic acid as a precipitation agent were explored in detail. The results show that vanadium (IV) in the sulfuric acid medium containing nickel and aluminum was efficiently and selectively extracted by Cyanex 272. After three-stage countercurrent extraction, the extraction efficiency of vanadium was 99.76%, and the co-extraction efficiencies of nickel and aluminum were only 2.47% and 1.87%, respectively. Thermodynamic calculation shows that the extraction of vanadium (IV) from the sulfuric acid medium with Cyanex 272 is an endothermic reaction. The innovative method of oxalic acid precipitation was used to recover nickel from the raffinate, achieving selective extraction of nickel from the solution containing a high concentration of aluminum. The precipitation efficiency of nickel was 98.58%, while that of aluminum was only 0.75% under optimal conditions. The proposed flowsheet for the separation of vanadium, nickel, and aluminum from acid leaching solution may provide a new idea for the comprehensive recovery of valuable metals from spent hydrodesulfurization catalyst.

Nov 30, 2022

By Morton Handelman

The extraction of aluminum oxide_ from its ore is the initial step in the commerical production of metallic aluminum. This is most commonly done by the Bayer Process in which a caustic solution is used to dissolve hydrated alumina from the insoluable materials with which it is associate in bauxite. At the two-thousand ton per day Sherwin Alumina Plant of Reynolds Metals Company, the extraction residue from Caribbean ores is removed from the main pro¬cess stream as the underflow of a continuous clarifier-thickener operation. This sludge, prior to its ultimate r4jection from the process, is washed in a nine-step continuous countercurrent decantation system to recover physically-entrained mother liquor. Control of alumina production costs requires the optimum recovery of solubles from this residue which is generated at the same rate as the finished product. The equipment, operating techniques, controls and process variables which affect the efficiency of this soda recovery from Bayer Process red mud will be discussed.

Jan 1, 1959

By P. M. Prasad

Off-grade molybdenite concentrates, mainly derived from secondary sources as by-products of the processing of copper, uranium and tungsten ores, do not satisfy the purity requirements (percent MoS2) for the production of molybdenum bearing products. This investigation is a continuation of a successful effort to refine a low-grade molybdenite concentrate to prepare a high-grade MoS2 using a mixed acid (HF + HCl) leach procedure. Specifically, this investigation is concerned with an understanding of the separation chemistry underlying the removal of the oxide/silicate gangue and the base-metal sulfide associations present in the low-grade molybdenite by their selective dissolution in the two acids. Experiments were conducted on an off-grade concentrate containing 42.6% Mo. Results of the controlled dissolution tests indicate that both HCl and HF are suitable for the removal of the associated alumina and both work well for iron, nickel and copper. However, HF was found to be the most effective for dissolving silica/silicate and magnesia. An attempt was made to rank the leaching efficiencies of the acids used singly, sequentially or in a mixed mode. Scale-up (300 to 2,000 g) experiments were conducted to validate this approach. Excellent purification of the concentrate was possible by processing the off-grade concentrate with 10% HCl plus 15% HF at 363 K for 7.2 ks in open polypropylene reactors with internal stirring. These conditions leached practically all of the oxide and silicate gangue and 96% of the metallic impurities. Starting from the low-grade molybdenite concentrate (42.6% Mo; 71.1% MoS2) it was found feasible to obtain a refined product containing 97.8% MoS2, which is suitable for industrial use.

Jan 1, 2007

By Norman F. Schulz

The technical excellence of separation achieved in a mineral concentration process, or any other process where two constituents of any kind are physically separated from each other, is expressed uniquely and quantitatively by the Separation Efficiency: ES = (R ? Rg) where R is the percentage of the valuable constituent and Rg the percentage of the waste appearing in the concentrate. The Separation Efficiency meets all the usual requirements of a true efficiency and is independent of the nature of the process used. It can be visualized as the percentage of the feed material that, in effect, actually undergoes complete separation while the rest of the feed is distributed randomly and unchanged into the two separation products.

Jan 1, 1969

By Chuanlin Fan

The process of flotation separation and recycling of spent potlining (SPL) was described. On the basis of the laboratory investigations, the effects of influencing factors in froth flotation process, such as grain size, flotation agent dosage, pH value, pulp density, and dissolved components concentration, etc, were carefully studied. And the influence on environment of the process was also discussed. It was found that flotation separation can be used as an environment-friendly method for treatment of SPL residue. Carbon and other compounds (include cryolite, sodium fluoride, calcium fluoride and diaoyudaonite, etc.) from SPL were separated and recycled as flotation products respectively.

Jan 1, 2009

By Kauko T. Ingerttilä, Jouko O. Kallioinen, Jaakko O. Leppinen, Alexander V. Lashkul, Vladimir E. Nenno

"Separation in Froth (SIF) is a process for the separation of mineral particles during their descent downwards through a moving froth layer, generated on the surface of water or some other liquid media by means of a bubble generator and frother. Due to the special operation principles of SIF it is possible to separate mineral particles that are about 10 times coarser than the optimal particle size for conventional flotation. In this paper the performance of the SIF technique is presented in the separation of apatite, calcite and silicate minerals from various industrial sources, based on tests with laboratory and pilot plant-scale SIF machines. Basic laboratory test results of the flotation of pure diamonds are also presented.It was shown that calcite, apatite and diamonds with particle size up to about 3 mm can be successfully floated with SIF at high recovery and grade, provided that the degree of liberation is sufficiently high. Coarse calcite (+0.25-2.8 mm) was concentrated with reverse SIF in one flotation step at 87% recovery with better than 99% grade. Apatite particles coarser than 0.2 mm are not well floated in the conventional flotation circuit leading to high P2O5 content in the coarse size fractions of flotation tailings. On the contrary, SIF is capable of recovering such coarse particles at high recovery. However, P2O5 content of the SIF tailings starts to increase at about 0.7 mm due to insufficient liberation of apatite. At higher particle size the lack of hydrophobicity of apatite particles is also likely to lower the recovery.The pilot plant testwork showed that SIF can be successfully used at operating plants not only for preliminary upgrading of the feed of conventional flotation, but also for producing final grade calcite concentrate (>99.5%) from the screen overflow or from the cyclone underflow in a particle size range up to 1 mm. It was particularly promising that the separation took place in one SIF flotation step, instead of several stages of the conventional flotation circuit, with over 90% calcite recovery. The specific capacity determined with the 1 m2 pilot plant unit was approximately 30 t/m2h. Simultaneously the consumption of chemicals was significantly lower than for conventional flotation."

Jan 1, 2003

By Kauko T. Ingerttilä, Jouko O. Kallioinen, Jaakko O. Leppinen, Alexander V. Lashkul, Vladimir E. Nenno

The Separation in Froth (SIF) technique is based on the idea that the pulp is fed directly onto the froth layer prepared on the surface of liquid medium providing an effective method for separation of coarse particles up to a few millimeters size. Thus the SIF process can result in substantial savings in grinding energy and flotation chemicals. In this work flotation of apatite, calcite and silicate minerals from various industrial sources was investigated using laboratory and pilot plant-scale SIF machines. Flotation of diamonds was also investigated on laboratory scale. It was observed that all the minerals mentioned above can be successfully floated up to about 3 mm particle size. Beneficiation tests with the coarse fractions of classification circuits indicated that final grade calcite concentrate can be obtained with over 90% recovery in one SIF step in this grain size (typically 0,1 to 1,5 mm). Similarly, substantial upgrading of coarse apatite was achieved without grinding it to the fineness required by conventional flotation. SIF could also be applied to the recovery of coarse apatite from the tailings of a conventional flotation process. The capacity measured in the pilot plant test runs for a 1 m2 cell was typically 30 t/m2h. Presently, a full-scale process using the SIF technology is being installed for coarse apatite recovery.

Jan 1, 2003

By G. N. Shannon

Keywords: inclusions, slag, modeling, interfacial energy, capillary force, particle flotation, particle separation A previously introduced model of inclusions separating across a steel-slag interface, developed by Nakajima/Okamura and Bouris/Bergeles, is expanded to include different inclusions shapes (octahedral and plate-like, besides spherical) as well as comparison between model ladle-, tundish-, and mold-slags. Investigation of the relation of these shapes with the interfacial capillary force ? which arises due to the dynamic interfacial energy during separation ? has shown that the force has a significant effect on whether the inclusion separates rapidly or settles at the interface. For the slags considered, the most significant physical property is found to be viscosity, which resulted in fast separation times for inclusions in the mold and ladle slags, relative to the more viscous tundish slag. Particle dissolution (using experimental data) is included in separation modeling.

Jan 1, 2005

By A. Iizuka

This study was aimed at separating and recovering arsenic, antimony, and tin from refining byproducts generated in a nonferrous smelter. The target byproduct was a silicate slag containing the above elements. The silicate structure of the slag was destroyed by alkali roasting, which then enabled leaching of arsenic, antimony and tin in solution effectively. Arsenic was selectively leached out by hot water after alkali roasting of the slag, while remained antimony and tin in the residue were leached out by a hot hydrochloric acid solution. However, when the solid-liquid ratio in the leaching solution was increased, hydrous gelatinous silica (gel-like silica) was formed during the hydrochloric acid treatment and filtration became difficult. Therefore, high temperature and high pressure leaching was attempted to improve the filterability of the silica leaching residue. In the high temperature and high pressure treatment, the hydrous gel-like silica was transformed into easily filterable aggregated silica, and thus, filtration became easy. By investigating the neutralization and sulfurization treatment for the obtained hydrochloric acid leachate (second leachate), it was possible to separate antimony and tin. INTRODUCTION This study aims to separate arsenic and recover valuable metals such as antimony and tin from refining byproducts generated in a nonferrous smelter. The target smelting byproduct is antimony-containing slag in this study. In many cases, alkali roasting was adopted as pretreatment for extraction and recovering valuable metals from smelting residues and wastes (Rao, 2006). For antimony-containing slag in this study, one effective method for separating arsenic is to convert arsenic to sodium arsenate (Na3AsO4) by roasting with a sodium compound and then to remove arsenic by hot water leaching. In addition, by alkali roasting, the silicate structure of the slag is destroyed, and effectively alkalizing tin and antimony is accomplished. Then, precipitating and recovering tin and antimony leached into the acid solution are considered possible by sulfurization and neutralization treatments. In this research, we conducted basic studies on the following. 1) Destruction of silicate structure in slag by alkali roasting and leachability of arsenic. 2) Conversion of hydrous gelatinous silica to aggregated silica by hydrochloric acid treatment of residues after arsenic leaching under high temperature and high pressure, as well as leachability of antimony and tin. 3) Separation and recovery of antimony and tin by sulfurization and neutralization treatments of hydrochloric acid leachate. These topics of investigation can support to consider the separation and recovery process of arsenic, antimony, and tin from antimony containing slag.

Jan 1, 2019

By A. S. Block-Bolten

Two innovations in nickel-arsenic separation have been studied on a laboratory scale. The first requires only a nitric acid atmospheric leach without preliminary roasting and leads to favorable final conditions for precipitation of arsenic as highly stable FeAsO4, The second is an NaOH-H2O2 pressure leach which is an alternative to the known NaOH-O2 pressure leach. Either method offers the possibility of rapid and efficient separation of nickel from arsenic and is applicable, for example to the high grade niccolite deposits in the Great Slave Lake area of northern Canada.

Jan 1, 1982

Sanes are utilized to make molds for metal castings in the foundry industry. Approximately a half ton of sand is disposed of for each ton of metal cast in this country. The purpose of this investigation was to study and develop a process to separate chromite sand and silica sand from reclaimed sands for a steel foundry. Physical separations were utilized to yield silica and chromite sands with desirable molding properties. Several different separation methods, including electrostatic, magnetic, and various gravitational approaches were examined. Experimental results are presented. A method was developed to separate chromite sand from silica sand after mechanical or thermal reclamation. The reclaimed sands are passed through a rare earth magnetic separator to separate chromite sand and magnetic impurities from non-magnetic silica sand. Chromite sand can be recovered from magnetic silica sand or magnetic impurities very effectively using a wet concentrating table. The applicabilities of the separation methods are discussed.

Jan 1, 1995

By Zizheng Zhou

The separation of cobalt from other base metals can be achieved using diffusion dialysis in a two-compartment reactor separated by an anion exchange membrane. In this work, a Neosepta AFX membrane was used to study the separation of various metals in an acid-chloride solution. The separation of one metal from another was investigated on the basis of the various chloro-complex stabilities. The metals investigated included cobalt, nickel, copper(II), iron(III), aluminum, zinc and cadmium. The impact of several critical experimental conditions, including the initial metal and chloride concentration in the feed solution and their initial concentration in the receiving solution, on the separation factor and the metal transfer rate is reported in this work. Effective separation of different metal pairs was achieved under the experimental conditions.

By Chen Song

Keywords: Mixed extractant, Copper, Cobalt, Nickel, Synergistic effect During separation process of copper and cobalt from nickel sulphate solution, the effects of constitutions and compositions of mixed extractant D2EHPA and PC88-A or Cyanex 272, has been studied. In one step extraction cycle, the following results are obtained:[Ni]/[Co]>4000 and [Ni]/[Cu]>40000 in nickel sulphate solution, [Co]/[Ni]>1000 and [Co]/[Cu]>30000 in cobalt chlorinate solution, [Cu]/[Ni]>10000 and [Cu]/[Co]>200 in copper sulphate solution. It was elucidated that the above-mentioned synergistic mixtures can effectively separate cobalt and copper from nickel sulphate acid solution and achieve a greater synergistic effect.

Jan 1, 2005

By G. M. Ritcey, B. H. Lucas

In the conventional alkaline leaching of concentrate containing nickel, copper and cobalt, copper is usually removed from the system, prior to nickel reduction, by sulphide precipitation. A new process is described for the selective extraction of copper and separation from cobalt and nickel, using liquid-liquid extraction. General Mills LIX-63 dissolved in a kerosene diluent is the extractant. Trace amounts of co-extracted cobalt and nickel are easily removed by a scrub treatment, and copper is recovered from the extract by sulphuric acid stripping, thus providing a solution amenable to the oroduction of electrolytic copper. Estimated processing costs are included together with a proposed flowsheet.

Jan 1, 1972

By Toshihide Takenaka

The management of radioactivated stainless steel from a terminated nuclear reactor will become an important subject in the near future. The separation of the elements in stainless steel should be effective to reduce the management labor. In this study, the separation of the elements in stainless steel by an electrorefining tcchnique was investigated in an aqueous solution. The electrochemical reactions of the elements in stainless steel werc studied by voltammetry and potentio-static electrolysis was carried out. A stainless steel anode was dissolved electro-chcmically with good anodic current etliciency in a chloride solution. The residue, where Ni was concentrated, was found on the anode after electrolysis. The electrodeposit in a stainless steel cathode consisted mainly of Fe and Cr and the Ni content in it was less than 0.5wt% under suitable condition. It is concluded that an electrorefining technique is effective for the separation of the elements in stainless steel.

Jan 1, 2003

By K. Haga

In this study, flotation tests were performed to investigate behavior of enargite and chalcopyrite ores from different sources synthetically mixed for separation of enargite. Flotation parameters including; pH, reagents concentration and type and flotation time were controlled to obtain an enargite concentrate with high As and chalcopyrite concentrate and final tailings with As content below 0.5 mass%. The copper ore bearing enargite mineral contained 5.87 mass% As and 16.50 mass% Cu while the chalcopyrite bearing ore contained 0.32 mass% As and 21.63 mass% Cu. The two ore samples were mixed at 7:3 (enargite: chalcopyrite) by weight ratio to prepare a mixed ore sample with arsenic content at 3.16 mass% and 18.25 mass% Cu for the flotation study. For enargite single ore flotation, the 38?75 µm size fraction showed that over 98% enargite was selectively recovered within 5 min at slurry pH of 4.0 and arsenic content in the final tailings was reduced to 0.22 mass%. In mix ore (enargite+chalcopyrite) flotation, 97% of enargite was first removed at pH 4 followed by chalcopyrite flotation at pH 8, and over 95% recovery was achieved in 15 min flotation time. Arsenic content in the final tailings was reduced to 0.1 mass%.

Sep 1, 2012

By Soner Top

In this study, a process to separate manganese and iron from manganiferous iron ores by reductive acid leaching followed by magnetic separation was conceived and experimentally tested. In the leaching process, sulfuric acid was used as lixiviant and oxalic acid was used as reductant. The experimental results showed that the manganese and iron separation was optimum when the concentration of the sulfuric acid and oxalic acid were 0.75 M and 30 g/L, respectively, at a temperature of 80 °C, a solid/ liquid ratio of 67 g/L, stirring speed of 400 rpm, and leaching duration of 60 min. Under this condition, 90.49% and 6.78% of Mn and Fe were dissolved, respectively, from the ore sample with a size fraction of − 106 μm. It was determined that the leaching of manganese from the ores was a second-order reaction with an activation energy (Ea) of 53.38 kJ/mol. The leaching residues obtained under the optimum condition were subjected to high-intensity wet magnetic separation tests to recover the remaining iron content. This separation process produced a concentrate containing 56.20% Fe and 1.79% Mn with iron and manganese recoveries of 56.83% and 66.73%, respectively. A magnetic separation test from an unleached ore sample was also carried out as a benchmark. To the best of our knowledge, this is the first time that a magnetic separation process was used to a residue obtained from reductive acid leaching of manganiferous iron ores to recover iron.