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ARAB JOURNAL OF BASIC AND APPLIED SCIENCES University of Bahrain 2023, VOL. 30, NO. 1, 68–73 https://doi.org/10.1080/25765299.2022.2157954 ORIGINAL ARTICLE Investigation of the extraction of samarium and gadolinium from leaching solutions of phosphorus-containing raw materials using solid extractants Denis Sergeevich Lutskiy , Elena Sergeevna Lukyantseva , Valeria Yurievna Mikheeva and Lyudmila Vladislavovna Grigorieva Physical Chemistry Department, Saint Petersburg Mining University, Saint-Petersburg, Russian Federation ABSTRACT ARTICLE HISTORY Received 20 October 2021 In accordance with the State Program of the Russian Federation «Development of Industry Revised 6 December 2022 and Its Competitiveness», as well as the absence of balance deposits of rare earth metals on Accepted 9 December 2022 the territory of the Russian Federation, it is urgent to study methods for the extraction and separation of rare earth metals from technological solutions obtained during the processing KEYWORDS of apatite concentrates. The article is devoted to the study of the kinetic features of solid- Apatite concentrate; phase extraction of samarium (III) and gadolinium (III) from simulated industrial phosphoric extraction; rare earth acid solutions. Levextrel resine (co-polymerization product of styrene and divinylbenzene) metals; SES; SES-D2EHPA; containing Di-2-ethylhexylphosphoric acid (D2EHPA) – was used as a solid-phase extraction solid extractant system agent. Significant dependence of samarium (III) and gadolinium (III) extraction rate constant on the stirring rate was revealed using the formal first-order kinetic equation. Based on the linear dependences of the logarithm of the reaction rate constant on the reciprocal tempera- ture, the activation energies for the extraction of Gd and Sm from phosphate model solu- tions were established, which, respectively, were 42.47 and 28.48 kJ/mol. The obtained values of the activation energies indicate that the limiting stage of the extraction process on a solid extractant can be considered a chemical reaction between ions of rare-earth metals and functional groups of the extractant. Separation of elements at the extraction stage is possible at temperature of 333 K under non-equilibrium conditions with separation coeffi- cient up to 1.8 in 5 min. 1. Introduction the state balance includes 26.9 tons of the amount of rare earth metals, with 70% of the reserves concen- Rare earth metals form a group of 17 elements, includ- trated in the deposits of the Northwestern Federal ing scandium, yttrium, lanthanum, and the lanthanides District, 17% in the Far Eastern Federal District and 13% (cerium, praseodymium, neodymium, promethium, in the Siberian Federal District. samarium,europium, gadolinium,terbium,dysprosium, Mineral ores are still the main source of rare earth holmium, erbium, tulium, ytterbium, lutetium), while metals. In the Russian Federation, the state balance possessing similar chemical and physical properties of mineral deposits includes 17 primary deposits, (Binnemans, Jones, Muller, & Yurramendi, 2018). Rare where rare earth metals can be isolated as a by- earths metals (REM) are widely used in various high- product during the processing of raw materials. tech industries due to their unique optical, electrical, Currently, only the Lovozero deposit of loparite ores and magnetic properties. Due to the development of is engaged in the associated extraction of rare earth industry, the share of the use of rare earth metals is metals, their concentration and further separation increasing every year (Tunsu & Petranikova, 2018). In with the release of oxides of rare earth metals and the Russian Federation, rare earth metals are extracted their compounds, since this deposit contains about exclusively as a by-product during the processing of 25% of the reserves of rare earth metals in the ores and the extraction of the main components from Russian Federation. them due to their low content in the extracted ores. In An important aspect of the development of any terms of reserves of rare earth metals, Russia is firmly in technology is the choice of a sequence of optimal second place in the world, giving priority to the technological processes that reduce the economic People’s Republic of China (Guimei, Yong, Wendong, costs of an enterprise when introducing stages for Raimund, & Zewen, 2023). In the Russian Federation, the extraction of rare earth metals and their further CONTACT Denis Sergeevich Lutskiy denis.lutskii@gmail.com Physical Chemistry Department, Saint Petersburg Mining University, Saint- Petersburg, Russian Federation 2023 The Author(s). Published by Informa UK Limited, trading as Taylor & Francis Group on behalf of the University of Bahrain. This is an Open Access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. The terms on which this article has been published allow the posting of the Accepted Manuscript in a repository by the author(s) or with their consent. ARAB JOURNAL OF BASIC AND APPLIED SCIENCES 69 Table 1. The relative content of rare earth metal oxides in volatile, and toxic organic solvents. The formation of EPA solutions. interfacial emulsion can also be attributed to undesir- REM Content, REM Content, REM Content, able side effects of the solvent extraction process. The oxide rel. % oxide rel. % oxide rel. % use of solid-phase extraction has a number of advan- La O 15.07 Sm O 3.18 Tb O 0.43 2 3 2 3 2 3 tages compared to solvent extraction during the pro- Ce O 37.54 Eu O 0.96 Dy O 1.92 2 3 2 3 2 3 Pr O 4.67 Gd O 3.51 Ho O 0.34 2 3 2 3 2 3 cess of extracting the target component, such as Nd O 18.34 Y O 12.51 2 3 2 3 compatibility with a continuous stream of acidic Er O 0.88 2 3 Yb O 0.51 2 3 saline solutions, which can provide scalability of the process (Artiushenko et al., 2020). The disadvantage separation into the scheme (Litvinova, 2015; Wang of this technology is the need for additional space et al., 2010). and equipment to ensure the regeneration of materi- The Khibinskoye apatite deposit located on the als used as solid carriers for reuse (Akkaya, 2014). Kola Peninsula can be a promising source of rare Currently, solid extractants systems (SES) are prom- earth metals. During the decomposition of apatite ising products for the separation of rare earth metals raw materials with concentrated sulfuric acid, two (Babu, Binnemans, & Roosen, 2018; Bao, Tang, Zhang, products are formed containing rare earth metals— &Liang, 2016). Solid state extractants are a product of phosphoric acid and a solid residue of phosphogyp- suspension copolymerization of styrene and divinyl- sum—the calcium salt of sulfuric acid. benzene and an extractant (TBP, D2EHPA, as well as Extractive phosphoric acid (EPA) contains about any other organophosphorus extractants in a total vol- 20% of the total of rare earth metals and is a prom- ume of up to 70%) (Razieh, Rezvan, & Mehdi, 2022). ising source for the extraction of rare earth metals. Compared to liquid extraction in SES, the extractant is Attractive is the fact that the use of extraction phos- in a droplet-liquidstate andhas improvedkinetic phoric acid does not require a significant increase in characteristics (H er es et al., 2018; Kabay, Cortina, production stages and associated capital costs. Table 1 Trochimczuk, & Streat, 2010; Valenzuela et al., 2012). shows the relative content of oxides of rare earth The absence of physicochemical characteristics of metals in solutions of extraction phosphoric acids. solid-phase extraction of REE by D2EHPA-containing When using the volumes of extraction phosphoric extraction resins from concentrated phosphoric acid acids existing in the Russian Federation, it is possible solutions and the necessity to confirm technological to obtain up to 4-5 thousand tons of rare earth advantages of their use determined the subject of metal oxides per year, which will help to significantly this study. The study of the kinetic features of solv- reduce the need for the purchase of rare earth met- ent and solid-phase extraction of Gd (III) and Sm (III) als from companies in other countries. using Levextrel resin containing groups of di-2-ethyl- Taking into account the production of such high hexylphosphoric acid, which is a selective extractant volumes of extraction phosphoric acids, one of the with relation to REE, is the subject of this research promising technologies for the extraction of Sm and (Kaibo et al., 2022). Gd is the hydrometallurgical method, which includes the stages of the stage-by-stage separation of the 2. Research methods sum of light, medium and heavy rare earth elements Experimental studies on the sorption extraction of Sm from the extraction phosphoric acid, followed by their isolation and separation using solid extractants. based and Gd were carried out from phosphate solutions on D2EHPA (Abu Elgoud, Ismail, El-Nadi, & Aly, 2020; simulating in their composition the solutions released after the leaching of apatite concentrate. Model acid Artiushenko, Avila, Nazarkovsky, & Zaitsev, 2020). leach solution consisted of: orthophosphoric acid In industrial practice, during the hydrometallurgi- (C ¼ 0.5 M); sulfuric acid (C ¼ 0.19 M); gado- cal processing of raw materials, the isolation and H3PO4 H2SO4 concentration of rare earth metals occurs using the linium nitrate (C ¼ 0.00704 M) and samarium nitrate Gd following methods: (C ¼ 0.00989 M) (Wang et al., 2010). Sm To study the processes of extraction of Gd and Extraction extraction and separation of rare earth Sm, SES—D2EHPA was used as a solid extractant (Kabay et al., 2010). This solid extractant is a macro- metals (main method) (Voropanova & Pukhova, 2018); porous resin with an extractant fixed by adsorption. Separation of rare earth metals by the ion This sorbent is used to extract metal ions from acidic exchange method (Zhang, Ye, & Chen, 2012; solutions. The working temperature of the sorbent is 0 3 Zheng, Bao, Zhang, & Chen, 2018). no more than 80 C, the bulk density is 600 g/dm , the working range of pH values is 1.0–4.0. A well-known factor complicating the implementa- The process of solid-phase extraction was studied tion of solvent extraction is the use of flammable, under static conditions at a phase ratio L: S ¼ 1:10. 70 D. S. LUTSKIY ET AL. Table 2. The degree of extraction of gadolinium into a solid extractant at different temperatures. The degree of extraction of Gd into a solid extractant, % Extraction time, min. 298 R 308 R 318 R 333 R 0 0000 5 20.60 21.59 22.58 24.43 15 26.70 25.99 30.53 33.52 30 28.41 32.52 33.38 40.76 45 30.26 35.36 39.34 46.44 60 31.25 37.21 43.60 51.56 120 34.66 40.19 50.71 54.11 Figure 1. Kinetic dependence of the degree of extraction of Gd in a solid extractant at different temperatures. Table 3. Sm recovery into solid extractant at different temperatures. The degree of extraction of Sm into a solid extractant, % Extraction time, min. 298 R 308 R 318 R 333 R 0 0000 5 17.46 14.96 18.82 15.27 15 20.78 18.01 23.62 25.04 30 21.55 24.84 26.68 32.35 45 24.65 25.76 32.14 35.57 60 27.17 27.81 34.51 41.54 120 30.49 33.97 41.29 42.24 The process was carried out in a thermostatic system Figure 2. Kinetic dependence of the degree of extraction of with an oscillation rate of 75 rpm. The mass of the samarium in a solid extractant at different temperatures. solid extractant was 1.0000 ± 0.0005 g. The stirring time for each sample was 5, 15, 30, 45, 60, and ln 2 0, 693 s ¼ ¼ (2) 1=2 120 minutes. Experimental dependences were k k obtained at 298 K, 308 K, 318 K, and 333 K (Callura To determine the half-extraction time and rate et al., 2019; Cheremisina, Schenk, Cheremisina, & constants of the processes of extraction of Sm and Ponomareva, 2019). After reaching the specified con- Gd ions using the solid-phase extractant SES— tact time, the aqueous phase was separated from D2EHPA, kinetic dependences were obtained, pre- the solid extractant using a Schott filter with a por- sented in Tables 2 and 3 and in Figures 1 and 2. osity of 160 lm. The extractant was sent for regener- ation, and the equilibrium solutions were analyzed 3. Results and discussion for the content of metal ions by an X-ray fluores- cence method using an energy-dispersive X-ray The experimental results showing the degree of fluorescence spectrometer PANalytical Epsilon 3 gadolinium extraction in SES-D2EHPA at tempera- (Cheremisina, Sergeev, Fedorov, & Iliyna, 2019; tures of 298 K, 308 K, 318 K, 333 K, depending on the Praveenkumar, 2021). time of contact of the phases, are presented in Table 2 From the point of view of formal kinetics, such and in Figure 1. extraction processes can be represented as a first- Figure 1 shows the dependences of the degree of order kinetic reaction (Li, 2019; Lutskiy, Ignatovich, & extraction of Gd into SES—D2EHPA. Sulimova, 2019). In first-order reactions, the reaction As can be seen from the data obtained, the rate is related to the rate of change in the concen- dependence of the effect of temperature on the tration of substance A by Equation (1): extraction of metal in SES is traced, reaching its max- 1 C imum value by 120 minutes. However, an increase in k ¼ ln (1) s C temperature from 318 to 333 K gives a very insignifi- where C is the initial concentration of the starting cant increase in the degree of extraction of gadolin- material, mol/l; C is the concentration of the starting ium into the sorbent, while increasing the power substance, mol/l by the time s, min, k is the reaction consumption required to maintain a constant tem- rate constant, min . perature of the solution. The optimal process can be To characterize the reaction rate, along with the considered as taking place at 318 K and 120 minutes. rate constant, the half-transformation time (s )is The experimental results showing the degree of 1/2 often used—the time during which half of the initial samarium extraction in SES—D2EHPA at 298 K, 308 K, amount of the substance will react. For first-order 318 K, 333 K depending on the time of contact of reactions, the half-life is defined as: the phases are presented in Table 3. ARAB JOURNAL OF BASIC AND APPLIED SCIENCES 71 Figure 3. Dependence of the logarithm of the concentration of Gd ions in the aqueous phase on the time of the process when using the solid extractant SES—D2EHPA at different temperatures. Figure 4. Dependence of the logarithm of the concentration of Sm ions in the aqueous phase on the time of the process when using the solid extractant SES—D2EHPA at different temperatures. Figure 2 shows the dependences of the degree of Table 4. Linear forms of equations for approximation of isotherms for extraction of Gd ions using solid extractant extraction of Sm into SES—D2EHPA. SES—D2EHPA. As can be seen from the data presented in Approximation equation Figure 2, the phase contact time also affects the T,K Gadolinium Samarium degree of Sm extraction into the sorbent, and an 298 ln C ¼5:264 0:0011 s ln C ¼4:82 0:0018 s increase in temperature from 318 K to 333 K with a 308 ln C ¼5:264 0:0027 s ln C ¼4:82 0:0020 s phase contact time of 120 minutes is insignificant, 318 ln C ¼5:264 0:0042 s ln C ¼4:82 0:0038 s 333 ln C ¼5:264 0:0070 s ln C ¼4:82 0:0055 s although at a temperature of 333 K and a phase con- tact time of 60 minutes we obtain the same degree Table 5. Values of the rate constants for liquid extraction of Sm extraction as at 318 K and the phase contact (k) and the half-extraction time (s ) of gadolinium and 1/2 time of 120 minutes. samarium using the solid extractant SES—D2EHPA. To obtain the kinetic characteristics of the process Gadolinium Samarium for the isotherms presented in Figures 1 and 2, linear 1 1 T,K k, min s min k, min s min 1/2, 1/2, forms of the kinetic dependences shown in Figures 3 298 0.0011 630.13 0.0018 385.08 and 4 were constructed. 308 0.0027 256.72 0.0020 346.57 318 0.0042 165.04 0.0038 182.40 The linear forms of the equations for approximat- 333 0.0070 99.02 0.0055 126.02 ing the extraction isotherms presented in Figures 3 and 4 are presented in Table 4. From the linear forms of the kinetic dependencies activation energies of the reaction for the extraction presented in Table 4, the values of the rate con- of Sm and Gd. stants of liquid extraction (k) and the half-extraction The linear dependences of the logarithm of the time (s ) presented in Table 5 were obtained. reaction rate constant on the reciprocal temperature 1/2 The processing of the dependences of the is described by empirical equations for the slope reaction rate constant on temperature, shown in coefficients of which the values of activation ener- Figure 5, makes it possible to determine the gies are set, presented in Table 6. 72 D. S. LUTSKIY ET AL. Figure 5. Linear forms of the dependences of the reaction rate constant on temperature during the extraction of Gd (a) and Sm (b) using a solid extractant SES—D2EHPA. Table 6. Equations of linear dependences of the logarithm of the reaction rate constant on the reciprocal temperature and activation energy of the reactions of extraction of Gd and Sm using the solid extractant SES—D2EHPA. Gadolinium Samarium Approximation equation Activation energy, J / mol Approximation equation Activation energy, kJ / mol 5108, 6 3426:6 ln k ¼ þ 10:496 42.47 ln k ¼ þ 5:0947 28.48 T T The obtained values of the activation energies Separation coefficient of 1.8 between Gd and Sm is ensured by the short phase contact time (up to indicate that the limiting stage of the extraction pro- 5 min). Solid extractants have an undoubted techno- cess on a solid extractant can be considered a chem- logical advantage. Such resins are characterized by ical reaction between ions of rare-earth metals and high mechanical strength, high chemical stability in functional groups of the extractant. aqueous solutions of acids and alkalis, and can be used in coarse systems and bulk filters. The absence of significant amounts of flammable solvents, which 4. Conclusions accompany liquid extraction, complies with the prin- ciples of green chemistry. In this work, the kinetic dependences of the extrac- According to the values of the rate constants of tion of Gd and Sm from phosphate solutions were ion-exchange adsorption and the half-exchange established, simulating in their composition the solu- tions released after leaching the apatite concentrate time, it is shown that the use of solid extractant SES- using the solid extractant SES-D2EHPA. The efficiency D2EHPA for the extraction of Gd and Sm ions from of this extractant for the extraction of Gd and Sm phosphate solutions is promising in comparison with from phosphate media is shown. Isotherms of extrac- its analogues. tion of Gd and Sm from a model phosphate solution from PJSC PhosAgro (Balakovo Branch of Apatit, Saratov Region, Balakovo District, Russia) as a prod- Disclosure statement uct of apatite processing were obtained. The effect of temperature on the degree of The authors declare no conflict of interest. extraction of Gd and Sm from model solutions is shown. For a number of temperatures, the values of ORCID the extraction rate constants (k) and the half-extrac- Denis Sergeevich Lutskiy http://orcid.org/0000-0002- tion time of Gd and Sm (s ) were determined. 1/2 9124-0418 Experimental data obtained indicate differences of Elena Sergeevna Lukyantseva http://orcid.org/0000- Gd and Sm extraction kinetics from a phosphoric 0002-7221-8688 acid medium. In case of Gd, the process is limited by Lyudmila Vladislavovna Grigorieva http://orcid.org/ a chemical reaction with an activation energy of 0000-0003-3287-5947 42.47 kJ/mol. In case of Sm, diffusion becomes the limiting stage, characterized by a decrease in activa- tion energy to 28.4 kJ/mol. The diffusion process Data availability statement determines the rate Sm extraction over a wide tem- The datasets generated during and/or analyzed during the perature range. Based on the revealed differences in current study are available from the corresponding author the element extraction kinetics, it is possible to carry out their separation at the extraction stage. upon reasonable request. ARAB JOURNAL OF BASIC AND APPLIED SCIENCES 73 preparation and their applications. Reactive and References Functional Polymers. 70(8), 484–496. doi:10.1016/j.reac- Abu Elgoud, E. M., Ismail, Z. H., El-Nadi, Y. A., & Aly, H. F. tfunctpolym.2010.01.005 (2020). Separation of Cerium (IV) and Yttrium (III) from Kaibo, H., Lu, X., Yi, N., Xuewei, L., Haifeng, D., & citrate medium by solvent extraction using D2EHPA in Hongshuai, G. (2022). Removal of aluminum to obtain kerosene. 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Arab Journal of Basic and Applied Sciences – Taylor & Francis
Published: Dec 31, 2023
Keywords: Apatite concentrate; extraction; rare earth metals; SES; SES-D2EHPA; solid extractant system
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