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By M. S. Safarzadeh, V. Agarwal

"The solvent extraction of cerium(III) and samarium(III) from mixed solutions of all rare earth elements (REEs) except promethium using PC88A (2-ethyl hexyl phosphonic acid mono-2-ethyl hexyl ester), an acidic extractant, was investigated. The effects of aqueous equilibrium pH, various acids (sulfuric acid (H2 SO4 ), hydrochloric acid (HCl) and nitric acid (HNO3 )), initial metal ion concentration and extractant concentration on the solvent extraction of Ce(III) and Sm(III) were systematically studied. From the experimental results, HNO3 and HCl were found to be the preferred aqueous media for the solvent extraction of both Sm(III) and Ce(III). The most promising experimental conditions of pH, PC88A concentration and metal ion concentration were identified for the extraction of Ce(III) and Sm(III). Separation results showed that H2 SO4 at pH 2 provided the best separation between Sm(III) and Ce(III). IntroductionIn recent years, demand for rare earth elements (REEs) has increased significantly because of their many commercial applications. REEs have especially important high-tech applications owing to their unique physical and chemical properties, and they are used in a wide range of areas such as catalysts, ceramics, magnets, lasers, glass, neutron absorption and alloys. As REEs have very similar physicochemical properties, their separation and purification from each other is challenging and gaining significant interest. Samarium (Sm) and cerium (Ce) are found in different REE minerals, including bastnäsite ((Ce,La,Nd(CO3)F), xenotime (YPO4) and monazite ((Ce,La,Nd,Th)PO4) at major production sites in the United States and China, as listed in Table 1 (Bleiwas and Gambogi, 2013). The most common acidic organophosphorous extractants used for REEs extraction and separation are DEHPA (di-(2-ethylhexyl)phosphoric acid), PC88A (2-ethyl hexyl phosphonic acid mono-2-ethyl hexyl ester), Cyanex 272 (bis-2,4,4-trimethylpentyl phosphinic acid) and Cyanex 301 (bis(2,4,4-trimethylpentyl)dithiophosphinic acid) (Sarangi, Reddy and Das, 1999; Surampally et al., 2012; Tian, Jia and Liao, 2013). Out of these extractants, PC88A is known for providing higher separation factors (Acharya, Mishra and Misra, 2015). El-Hefny et al. (2010) investigated the kinetics of the solvent extraction of Sm from chloride media using sodium salt of Cyanex 272 and reported the extracted species to be Sm(OH)A2•2HA. Lee et al. (2005) investigated the solvent extraction of Sm(III) with PC88A and saponified PC88A from chloride solutions and found the stoichiometry of the extraction reactions to be 1.5 with PC88A and 3 with saponified PC88A."

Jan 1, 2017

By D. Mohapatra

The possibility of using 2,2,4-trimethyl-1,3-pentanediol dissolved in tetrachloromethane as extractant for boron recovery is discussed. The parameters optimized for this purpose are contact time, boron concentration in the aqueous phase, extractant concentration, equilibrium pH and phase ratio. NaOH is used as stripping agent for boron recovery from the loaded organic phase. Boron extraction is found to be a slow process (equilibrium time 20 minutes) compared to boron stripping, which is reasonably fast (equilibrium time 5 min). Maximum boron extraction is possible at a broad pH range from 1.0 to 6.0. Using 1.0M extractant concentration, a 1:1 phase ratio (organic: aqueous) and two stages, ~99% boron extraction is achieved. More than 97% boron stripping is possible using 0.5M NaOH at a 1:1 (organic: aqueous) phase ratio in two stages. Overall, a 95.6% boron recovery was achieved. Loss of solvent into the aqueous phase and co-extraction of Ca, Na and K into the organic phase at higher equilibrium pH are two major concerns in his process.

Jan 1, 2008

By G. Bacon

The past decade has witnessed unprecedented growth in the development and implementation of solvent extraction technology in the extractive metallurgy of nickel and cobalt. Solvent extraction is proving to be a powerful tool, opening new opportunities for simpler, more cost efficient and environmentally sound metal refining processes. These advances, however, could not have been possible without the cooperative efforts between the nickel industry and the people and organizations involved with reagents, materials and equipment development and supply as well as solvent extraction research, aided by the accumulated knowledge and practical experience from the copper and uranium solvent extraction operations. This paper provides an overview of these developments and some of the challenges ahead.

Jan 1, 2002

By N. Dave

"IntroductionIn the mineral processing industry, certain minerals such as uranium, thorium and vanadium, etc., are selectively extracted with high degree of purity from solutions containing variety of other impurities by solvent extraction process. This separation process consists of bringing two immiscible or partially soluble liquid phases in contact, where mass transfer of one or more components takes place by ion exchange under certain controlling parameters such as pH, salt concentration and temperature. The processes taking place are primarily physical because the solutes being transferred are ordinarily recovered without chemical change. For efficient extraction more than one stage is required and the solutions are recycled counter currently through other stages. A multi-stage counter current solvent extraction plants essentially consist of four circuits namely: extraction, water wash, stripping, and solvent scrubbing. In extraction circuit the desired mineral is extracted at a certain pH from an aqueous solution onto an organic solvent by bringing them in contact with mixing in large mixer-settler units. The mixed solutions are allowed to settle and separate into component organic and aqueous phases in horizontal settlers by providing sufficient residence time. The solutions are then moved counter currently to other units- the aqueous from the underflow and the solvent organics from the overflow of the settler. The solution streams coming out of extraction circuit are loaded organics and barren aqueous or raffinate solution. The loaded organics are washed with water in a water wash circuit to remove transported impurities from extraction circuit. In the stripping circuit, the desired mineral is stripped selectively from the solvent phase back into an aqueous phase with a stripping agent at a selected pH. The solution stream leaving, stripping circuit are stripped organics and pregnant strip (aqueous) solution. The stripped organics are scrubbed off other loaded impurities with a conditioning solution in, scrubbing circuit and the cleaned solvent is re-used in the extraction circuit.A typical solvent extraction plant for uranium extraction and purification at Agnew Lake Mine is described in this chapter."

Jan 1, 1989

By E. Robles

The Tati Activox® Project (TA®P) is the first step towards the implementation of the Norilsk Nickel Activox® process. The ultrafine grinding (UFG) and autoclave pressure leach process conditions are the heart of the Activox® patent. Low grade base metal sulphide concentrates are leached in the process to recover the base metals and to produce LME grade nickel and copper cathodes and cobalt carbonates. The downstream processing of the metal-containing liquor produced by this process includes solvent extraction circuits to extract and concentrate metal-rich solutions, before the various final products are obtained. This paper gives an overview of many of the relevant design aspects taken into consideration in the design of the Tati Activox® solvent extraction circuits. It addresses key design elements related to leach process conditions such as scaling, materials selection for corrosive solutions, pH control, crud formation and treatment, multiple SX trains designed to prevent organic cross-contamination, and design aspects related to the mitigation of fire risks.

Jan 1, 2009

By P. M. Cole

An unprecedented expansion of the global zinc industry is currently under way. While most new projects and plant upgrades remain committed to traditional processing technologies, recent advances in zinc solvent extraction (SX) have created opportunities for new process routes for both primary and secondary materials. The first commercial plant to use zinc SX for the mainstream processing of a low-grade ore is under construction and promises to become one of the lowest cost zinc producers. Several other oxide and sulphide projects in various stages of feasibility are considering the inclusion of SX in their process flowsheet. Zinc SX has also proved advantageous in the reprocessing of secondary materials, particularly for the treatment of zinc residues and furnace dusts. This review focuses on recent installations and projects underdevelopment that feature zinc SZ as the key separation step.

Jan 1, 2002

The mixer that is commonly encountered in hydro metallurgical operations consists of a single turbine and tank combination. However, it would be advantageous to examine some common solvent extraction mixing systems in the light of the fundamentals of chemical reactor design. The basic concepts of reactor design are commonly used in the chemical industry, and it should not be too difficult to apply them to solvent extraction. The factors that affect the engineering design of a reactor are: the reacting system; the type of reaction; and the configuration of the reactor. The reaction system in solvent extraction consists of a heterogeneous liquid phase, involving two immiscible liquids. It is essential f or the process that the reactor product can be separated efficiently in the subsequent settler. The type of reaction in solvent extraction system may be quite complex, and the picture is complicated by the presence of competing and side reactions. The reactors themselves have been generally continuous stirred tanks, and the nature of the mixer-settler makes it unlikely that the pumping mixer can be dispensed with. However, it appears that there should be some definite advantages to a system of stirred reactors in series. The kinetic experiments which are carried out should have the definition of optimum reaction conditions as one of their goals. The data obtained from these experiments must also be applicable to the design of reaction equipment. Reactor selection and design is often a unique problem for each chemical process, and does not lend itself to a systematic general approach. However, the application of chemical and physical principles to mixer design in solvent extraction should result in practical, more efficient plants.

Jan 1, 1979

By D. Mohapatra

Extraction of Al(III) from aqueous sulfuric acid solutions into organic Cyanex 272®-carbon tetrachloride systems was investigated from a multi-component mixture containing aluminum, cobalt and nickel. Al(III) extraction efficiency was quantitative with 1.0 M Cyanex 272® in two stages at an aqueous: organic (A:O) phase ratio of 1:1 and an equilibrium pH of 3.2. The stripping of Al(III) from the loaded organic (LO) with different acids indicated sulfuric acid to be the best stripping agent. More than 99% stripping of Al(III) from the LO was achieved using 2 M H2SO4 at an A:O phase ratio of 1:1 in a single stage. The stoichiometry of the extracted species of Al(III) was determined by the slope analysis method. The extraction reaction proceeded via the cation exchange mechanism and the extracted species was assumed to be AlA3?3HA, where HA refers to the dimeric and A the anionic form of the extractant, Cyanex 272®. The extraction of Al(III) was studied in the presence of various ions to ascertain the tolerance limit of individual ions.

Jan 1, 2008

By F. Dakubo

"Solvent extraction of copper pregnant solution (PLS) obtained from ammonium peroxodisulfate assisted leach was modeled using response surface methodology. Mixing speed, pH, reagent concentration and organic to aqueous (O/A) ratio were selected for testing. A pitched blade mixer was used in the experiment. Mixer speed contributed significantly to copper extraction significant, while pH had minimal effect on copper extraction. The response model developed has an R2 = 0.97 and Adeq precision of 28.3. A parallel kinetic comparing study using a straight blade Rushton turbine in a turbulent regime of mixing showed no difference (p-value =0.308) between peroxodisulfate assisted leach PLS and conventional ferric/sulfuric acid leach PLS- the power draw data support this conclusion. INTRODUCTION High arsenic chalcopyrite concentrates are a problem to the smelters all over the world due to high arsenic gas emissions during smelting. Therefore leaching is often the alternative for extracting the copper in these concentrates if dilution with low arsenic concentrate is not possible. High-pressure autoclave leaching is used. Alternatively, the use of stronger oxidants such as peroxodisulfate has been proposed [16, 18]. There is a concern brought up by the hydrometallurgy community about the faith of the organic extracting reagent coming into contact with stronger oxidant residue in the pregnant leach solution (PLS) and hence the efficiency of such extraction process. This work, therefore, looks to answer such concerns. PLS generated from leaching of chalcopyrite concentrate with the peroxodisulfate ion was used in this solvent extraction experiment. As a liquid-liquid extraction, solvent extraction involves contacting the aqueous PLS with organic extractant via mixing. Mixing is known to increase the interfacial area for mass transfer by decreasing the diffusion path length (Jussi et al.1997). EXPERIMENT Instruments and Reagents Reagent grade Acorga 5910 reagent was used in the experiment was supplied by Cytec (Current name Solvay), Ammonium peroxodisulfate and sulfuric acid were reagent grade obtained from Amazon. Apparatus The solvent extraction tests were carried in a 2000 ml plastic cylindrical reactor equipped with four 0.5” baffles. In the hypothesis test, the reactor was a 4000 ml cylindrical reactor with four 1” thick baffles arranged evening in the reactor. Comparison between peroxodisulfate and ferric leach PLS via hypothesis test"

Jan 1, 2018

By P. D. Navarro

The behavior and operability of LIX 1104SM extraction was studied at laboratory scale on the Solvent Extraction at Sb3+, from high concentration sulfuric acid. In order to evaluate the reactant batch tests were made at laboratory scale as well for extraction as for re-extraction of Sb3+. Experiences achieved were: extraction kinetics, temperature effects, selectivity tests and re-extraction selectivity. A extraction kinetics was found, reaching equilibrium in 2 min, high selectivity of Sb3+ extraction in front of Cue , existing As5+ co-extraction and Fe3+ At the re-extraction stage, equilibrium was reached in 3 min, getting high Sb3+ re-extraction efficiency with HCl concentrations within 6 and 8 M. A high selectivity was achieved on Sb3+ re-extraction in front of As+5, existing Fe+5 re-extraction.

Jan 1, 1999

By V. K. Chandaliya

N-Methyl-2-pyrollidone (NMP) has already been proven a good solvent for extraction of coal. It is believed that organic components of coal are likely to be dissolved with the solvolytic power of NMP. During dissolution process, original coal also gets disintegrated and thus helps in further extraction. Coal extraction highly depends on temperature, coal to solvent ratio, N-Methyl-2-pyrollidone (NMP) to Ethylenediamine (EDA) ratio and the size of coal particles. The process has been established in the laboratory. There is no reference available beyond lab scale. In present study, we are running a bench scale plant with 40 kg/batch capacity. Design of experiment was done in such a way that the optimum zone of the process gets evaluated for clean coal having low ash with high yield. Bench scale plant trial was conducted based on optimum zone developed during design of experiments (DOE). From the DOE analysis it was observed that feed size and coal to solvent ratio are important parameters for this process. Total 27 experiments (four factors with 3 level of variation) were designed through Box-Behnken model. It was observed that -0.5 mm feed size of coal, 150 °C extraction temperature, 17:1 NMP to EDA ratio, 1:9 coal to solvent ratio was optimum conditions. The results obtained at optimum conditions are 50% clean coal yield with 5% ash.

Sep 1, 2012

By George Owusu

A study has been carried out on the use of solvent extraction, instead of the traditional zinc dust cementation process, to remove copper from concentrated zinc sulphate leach solutions. In a series of experiments using plant solution containing 1.9 g/L Cu, 2 g/L Fe, 173 g/L Zn, 7.9 g/L H,SO,, 0.25 g/L Cd, 15 mg/L Co etc. and LIX 622 in SX-1, up to about 97-98 % of copper present in the zinc sulphate leach solution was extracted with negligible co-extractions of zinc, iron, cadmium, cobalt, etc. pH modification was not required for this reagent. The copper loaded organic was almost completely stripped using 150 g/L sulphuric acid. Investigations into the effect of any possible organiclextractant contamination on zinc electrowinning showed (if any) little effect on current efficiency if the organic contamination is less than 45 ppm; current efficiencies of 95-97 % were obtained. At organic contaminations higher than 45 ppm, the current efficiency dropped to about 92- 94 %. Visually, the organic-contaminated cathode sheets had rough surface morphology, becoming more intense with increasing organic concentration, compared to the non-contaminated cathode sheets.

Jan 1, 1998

By R. Sharma, I. Miskovic, S. Miskovic

Solvent extraction (SX) is a widely used method for the extraction of copper from pregnant leach solutions or other ionic solutions in hydrometallurgical applications. About 17% of total refined copper production worldwide is produced using SX followed by electrowinning (EW). Conventional SX units, such as mixer-settlers, consume a large amount of extractant, offer poor process control and yield low extraction efficiency. Extraction efficiency is poor due to low specific interface area, crud formation, emulsification, and slow phase separation stage. Micro solvent extraction (micro-SX) is a rapidly developing technology that provides an opportunity for improved process control, higher extraction efficiency, lower residence time and, as such, has a potential to reduce the environmental footprint of SX operation. In this research, extraction of copper ions in an acetate buffer media is investigated using D2EHPA with kerosene as a diluent. Chemical factors such as extractant concentration and ionic concentration of aqueous phase are varied to determine the optimum conditions. Subsequently, the extraction efficiency and reaction time of new micro-SX reactors are compared against previous bulk SX studies. Extraction in the microfluidic reactor was observed to be faster with a residence time more than an order of magnitude lesser than bulk SX. This study forms a prelude for developing new modular micro-SX units which will enable continuous, effective, and safe operation on a large scale. In future studies, numerical and analytical models validated through this work will help eliminate rigorous experimentation and enable faster design and fabrication of micro-SX units. INTRODUCTION Conventional industrial solvent extraction (SX) units such as mixer-settlers, extraction columns present various disadvantages. Low specific interfacial area, crud formation, and emulsification in industrial reactors lead to long extraction times and severely hamper extraction efficiency (Priest et al., 2011; Chen et al., 2017). Microfluidic extraction considerably improves upon the current extraction practices by (1) creating a large surface to volume ratio that enables rapid mass transfer across the interface, (2) better process control, and (3) easier separation of phases (Kashid, Renken, & Kiwi-Minsker, 2011; Ciceri, Perera, & Stevens, 2014). These factors establish micro-SX as a crucial mode for process intensification. Although, a micro SX unit has significantly low processing volume than conventional extraction methods, their throughput can be increased via massive parallelisation (‘numbering up’), which is an area of active research (Darekar, Singh, Mukhopadhyay, & Shenoy, 2016a; Kriel, Woollam, Gordon, Grant, & Priest, 2016).

Jan 1, 2019

By Jiang Feng, Li Chuanhua, Zhang Libo, Peng Jinhui, Ju Shaohua

Solvent extraction of Cu2+ from the leaching liquor contain Cu and Fe use a microfluidic technology. Currently, the conventional copper extraction process has many problems such as long distance and small driving force of mass transfer. In order to solve the problems, studies are carried out on the extraction process of low grade copper leaching liquid using Lix984N as an extractant with a new microfluidic solvent extraction technology. The effects of flow rate on the separation and extraction efficiency between Cu and Fe are studied, and the results show that a steady liquid-liquid interface of laminar flow is form in the micro-extractor, and extraction efficiency is 78 % and 2.5 % for Cu and Fe at the contact times of 0.84s respectively. Besides, the separation coefficient between Cu and Fe is as high as 140.04. The studied microfluidic technology has the advantages like improving extraction efficiency and reducing reaction time and providing the potential application in the hydrometallurgy extraction of Cu.

Jan 1, 2015

By Gus Van Weert

Solvent extraction of iron from zinc refinery liquors has been investigated before, mainly on the MEHPA / HC1 stripping combination. Leakage of chloride into the zinc electrolyte and the costs of handling the ferric chloride eluate have prevented this option from being adopted. This work explores the stripping of the ferric loaded organic phase with nitric acid to take advantage of the possibility of regenerating up to 6N nitric acid, and clean spheroidal hematite production by autoclave treatment of ferric nitrate solution. The work was carried out with DEHPA (di 2-ethyl-hexyl phosphoric acid) in kerosine. Degradation testing proved the DEHPA to be very stable, when exposed to nitric acid solutions up to 6N and temperatures up to 70" C over a period of five days. Ferric iron was removed completely froma synthetic hot acid leach liquor, irrespective of the DEHPA concentration. Stripping the ferric turned out to be the problematic step. Although the stripping efficiency was considerable better at 50 than at 20° C, it decreased with increasing DEHPA/Fe ration in the organic phase. Eluates of no more than 5-10 g/l ferric nitrate were produced. surprisingly, nitric acid was found to be a less efficient stripping agent than sulphuric at equivalent normality and its efficacy levelled off above 4N. It was concluded that DEHPA does not appear to be the S.X. reagent to take advantage of the low cost autoclave decomposition of ferric nitrate opportunity in zinc hydrometallurgy and that another S.X. reagent, also resistant to nitric acid, but based on weaker compound formation is needed.

Jan 1, 1998

By Harold Wahlborg, George Owusu

In a study using butyl diglyme as an organic extractant, essen­tially complete extraction of gold from chloride leach solution was achieved. The extraction kinetics are so fast that the process could be completed in 30 seconds. Except for iron, co-extraction of other ionic species was insignificant. Co-extracted iron species were successfully scrubbed from the loaded organic using 10% HCl solution. High grade, >99.9%, gold was recov­ered from the loaded organic using 5% oxalic acid solution as the stripping agent at a temperature of 70°C to 80°C. Over 99% of the organic-loaded gold was stripped from the organic phase. The butyl diglyme extractant is being tested on a variety of gold-bearing feedstocks. Presented here are results obtained from two gravity concentrates.

Jan 1, 1999

By M. J. Gula, S. S. Xue, E. P. Horwitz

A study has been conducted to remove iron from sulfate solutions using Eichrom's Dipexo® extractant, P,P'-di(2ethylhexyl) methanediphosponic acid (H2DEH[MDP]). It is found that this extractant can effectively and selectively extract ferric ion from highly acidic solutions. Ninety-nine percent of the iron was extracted from a simulated feed solution in a single stage. The separation factor, Fe/Zn, was 106. Over 90% of the iron in a loaded organic can be recovered in an aqueous solution by reductive stripping. This paper presents the experimental results. A new process for iron removal using Dipex extractant is described and discussed.

Jan 1, 1999

By G. Haesebroek

In L969 Metallurgie Hoboken-Overpelt started an industrial plant for the separation of iron and zinc from a concentrated CoCL2 solution. Iron and zinc are extracted in column contactors by a solvent containing 12 vol % of tertiary amines in xylene. The extracted metals are stripped from the pregnant organic phase by precipitation with a NaOH solution at pH LL. In this paper an overview is given of the industrial process. In order to overcome some drawbacks of this process (low flash point of the diluent, reagent consumption, batchwise stripping) an alternative solvent extraction process has been examined. In this alternative process, iron and zinc are extracted with an or¬ganic phase containing 50 vol % of TBP in Escaid 110. The pregnant solvent is stripped with water in conventional mixer settlers. Despite the ability of this process to overcome most of the inconveniences due to the use of tertiary amines, it suffers from the poor stability of TBP in concentrated chloride solutions, resulting in unavoidable and inacceptable precipitation phenomena in the stripping section.

Jan 1, 1988

By G. Thorsen

An alternative way to the normal practice of precipitation of jarosite, goethite, or hematite for removal of iron from zinc sulphate process liquors/ is to employ the techniques of solvent extraction. The process presented avoids the addition of any external alkali for the extraction of iron by integrating the leaching and solvent extraction steps in a hydrometallurgical zinc plant. By starting the leaching of zinc from the solid zinc calcine material with an organic solution of an acid liquid cation exchanger, the organic phase is loaded with the organic zinc salt from the direct reaction with zinc oxide. The residue from the organic leaching is transferred to a hot acid leach circuit where the remaining zinc oxide and the zinc ferrites will dissolve form¬ing an aqueous sulphate solution of zinc and iron. In the subsequent solvent extraction of iron from this aqueous leach solution, iron is exchanged with zinc from the organic phase. The commercial carboxylic acid Versatic 10 (Shell) is highly efficient for this integrated process of leaching and solvent extraction. The resulting iron-loaded organic phase is heated to 150-200 C in the presence of water whereby the iron will be directly precipitated from the organic phase as iron oxide of high purity and the regenerated organic acid is recycled to the organic leaching step for reloading with zinc.

Jan 1, 1980

By S. H. Seyedein, Hamed Tavakkoli, Mohammad Reza Aboutalebi, S. N. Asharafizadeh

The liquid–liquid extraction behavior of lutetium from different acidic solutions was investigated using two extractants, D2EHPA and PC88A, in kerosene. Lutetium extraction reactions with D2EHPA and PC88A from HNO3 and H2SO4 solutions were chemically and thermodynamically analyzed. It was found that each Lu cation was complexed with six monomers of the organic extractant and released three protons. Simultaneously, the Lu cation was instituted in the P–O–H group of the extractants. Thermodynamic analysis of reactions between extractants and acidic solutions showed that the D2EHPA-HNO3 system is the most favorable for extracting lutetium. It is noted that the calculated equilibrium constant of the reaction in this system was approximately six times larger than that of the D2EHPA-H2SO4 system. However, the value of the equilibrium constant for the D2EHPA-HNO3 system was evaluated to be approximately 200 times greater than that of the PC88A-HNO3 system. Therefore, one can conclude that the extraction behavior of lutetium is more influenced by the extractant type than the solutionmedium. The synergistic effect of different mixtures of extractants on the solvent extraction of lutetium was also examined, and the highest synergistic factor was obtained for a binary mixture of PC88A:D2EHPA at the ratio of 4:1 for both aqueous solutions.

Mar 15, 2021