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Modeling and equilibrium studies on the recovery of praseodymium (III), dysprosium (III) and yttrium (III) using acidic cation exchange resin

Modeling and equilibrium studies on the recovery of praseodymium (III), dysprosium (III) and... In this research, the possibility of using hydrogenated Dowex 50WX8 resin for the recovery and separation of Pr(III), Dy(III) and Y(III) from aqueous nitrate solutions were carried out. Dowex 50WX8 adsorbent was characterized before and after sorption of metal ions using Fourier-transform infrared spectroscopy (FT-IR), Scanning Electron Microscope (SEM) and Energy Dispersive X-Ray Analysis (EDX) techniques. Sorption parameters were studied which included contact time, initial metal ion concentration, nitric acid concentration and adsorbent dose. The equilibrium time has been set at about 15.0 min. The experimental results showed that the sorption efficiency of metal ions under the investigated conditions decreased with increasing nitric acid concentration from 0.50 to 3.0 M. The maximum sorption capacity was found to be 30.0, 50.0 and 60.0 mg/g for Pr(III), DY(III) and Y(III), respectively. The desorption of Pr(III) from the loaded resin was achieved with 1.0 M citric acid at pH = 3 and found to be 58.0%. On the other hand, the maximum desorption of Dy(III) and Y(III) were achieved with 1.0 M nitric acid and 1.0 M ammonium carbonate, respectively. The sorption isotherm results indicated that Pr(III) and Y(II) fitted with nonlinear Langmuir isotherm model with regression factors 0.995 and 0.978, respectively; while, Dy(III) fitted with nonlinear Toth isotherm model with R = 0.966. A Flow sheet which summarizes the sorption and desorption processes of Pr(III), DY(III) and Y(III) using Dowex 50WX8 from nitric acid solution under the optimum conditions is also given. Keyword: Modeling, Dowex 50WX8, Adsorption, Rare earth metals Introduction industries, color televisions, computer monitors and tem- Yttrium (Y), Dysprosium (Dy) and Praseodymium (Pr) perature sensors [1, 2]. Praseodymium is used with neo- known as segment of the rare earth elements (REEs) are dymium in combination for goggles to shield glassmakers spirited components in fluorescent lamps, glass polish - against sodium glare, permanent magnets and cryogenic ing and ceramics, computer monitors, lighting, radar, refrigerant [3]. Dysprosium alloy with neodymium is televisions, and X-ray intensifying films. Yttrium is exten - used for permanent magnets, catalysts, speakers, com- sively used in the manufacturing of several high-tech- pact discs and hard discs and medium source rare-earth devices such as microwave communication for satellite lamps within the film industry. [4] Ion exchange separa - tion of rare earth elements was used by Spedding and Powell to separate REEs from fission products obtained from nuclear reactors [5–7]. Sorption processes for the *Correspondence: betaam24@yahoo.com; Botros.masry@eaea.org.eg separation of rare earths have been reviewed in several Chemistry of Nuclear Fuel Department, Hot Laboratories Centre, Egyptian articles [8–11]. Strongly acidic cation exchangers were Atomic Energy Authority, Cairo, Egypt © The Author(s) 2022. Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article’s Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http:// creat iveco mmons. org/ licen ses/ by/4. 0/. The Creative Commons Public Domain Dedication waiver (http:// creat iveco mmons. org/ publi cdoma in/ zero/1. 0/) applies to the data made available in this article, unless otherwise stated in a credit line to the data. Masry et al. BMC Chemistry (2022) 16:37 Page 2 of 12 the first artificial functional polymers used for the sepa - results indicated that REEs have a tendency to behave as ration of REE ions, and they are resumed predominating two different groups that can be separated into two frac - in the fields of chemistry and chemical technology under tions as La, Pr, Nd and Sm, Eu, Gd. Dowex 50wx8 was consideration [11]. Styrene and divinylbenzene copoly- used previously for the reversible ion exchange of cerium mers bearing SO H group are utilized. Now, modifica - (III) sulfate and Cerium (III) nitrate where the experi- tions of these exchangers are manufactured under the mental results indicate that the continuous liquid flow trade names Amberlite, Dowex, Lewatit, Purolit, which reactor studies show a capacity of 0.72  mmol/g sorbent differ by the degree of cross linking sorption capac - for the Ce nitrate and 0.96  mmol/g sorbent for the Ce ity, grain size, pore diameter, and other parameter [12]. sulfate [20]. Dowex 50  W-X8 is one of the ion-exchange resins that The main objective of the present work is directed to have been used for separation of REEs from other ions study the sorption and separation of Praseodymium, as well as separation of individual REEs from a mixture Dysprosium and Yttrium from nitric acid solution using of REEs. Al-y Th abat and Zhang, studied the recovery of strongly acidic cationic exchange resin (Dowex 50WX8) REEs resulting from phosphoric acid with Dowex 50WX4 using batch technique. The effects different parameters and Dowex 50WX8 resins. Their results indicated that on the sorption and separation processes will be inves- the REE-extraction efficiency of Dowex 50WX8 was tigated such as contact time, nitric acid concentration, almost twice that of Dowex 50WX4 resin. This can be as well as v/m ratio and temperature. Desorption inves- explained by the higher exchange capacity, producing tigations will be also carried out and evaluated. Separa- more sulfonic groups, of Dowex 50WX8 even though tion feasibility between the investigated REEs are also its lower surface area and larger bead size [13]. Felipe discussed based on the difference between their sorption et  al., studied the recovery of rare earth elements from and desorption behavior. acid mine drainage by ion exchange [14] and reported that the highest loading capacities were 0.212  mmol Experimental −1 −1 g for La and 0.169  mmol g for Ce (Dowex 50WX8) Materials and chemicals −1 −1 and 0.210  mmol g for La and 0.173  mmol g for Ce The chemicals used in this work were of analytical rea - (Lewatit MDS 200 H). Recovery of rare earth elements gent grade (AR) and most of them were used without fur- from uranium concentrate by using cation exchange resin ther purification. Stock solutions of Pr(III), DY(III) and (Dowex 50WX8) was studied and the authors reported Y(III) (1000 mg/L) were prepared by dissolving a known that the maximum REE sorption capacity was found to amount of the metal oxide in minimum concentrated 82.74 mg/g which represents about 93.23% of the original nitric acid and evaporated to near dryness and then made capacity of the studied resin [15]. Sorption of rare earth up to the mark in a measuring flask with double distilled elements from nitric acid solution with macroporous sil- water. The desired required concentrations of test solu - ica-based bis(2-ethylhexyl)phosphoric acid impregnated tions were prepared by favorable dilution with a known polymeric adsorbent has been studied by Shu et  al. [16] concentrated nitric acid of the stock solutions. Dowex Their results indicated that the adsorption capacity of 50WX8 which is a strong acid cation resin containing 8% −1 Gd (III) was found to be 0.315  mmol g by bis(2-ethyl- divinylbenzene (DVB) [20], Fig.  1 was purchased from hexyl)phosphoric acid/SiO -P in 0.1  M H NO . Adsorp- sigma Aldrich. The chemical and physical specifications 2 3 tion and separation of terbium(III) and gadolinium(III) of Dowex 50X8 are given in table given in Table 1. from aqueous nitrate medium has been investigated using TVEX-PHOR resin by Madbouly et  al. [17]. Their Sorption experiments work showed that the maximum sorption capacity of The sorption experiments were carried out under the fol - this material was 15.49 mg/g and 24.93 mg/g for Gd(III) lowing conditions, v/m = 0.05 L/g, Pr(III), DY(III) and and Tb(III) from 0.1  M NaNO solution, respectively Y(III) concentrations = 100.0  mg/L in 0.50  M nitric acid at pH = 5.2 and V/m = 0.1. El-Dessouky et  al. studied solution. In each adsorption experiment, 5.0  ml of the the sorption of praseodymium (III), holmium (III) and investigated metal ions solution was added to 0.1  g of cobalt (II) from nitrate medium using TVEX–PHOR Dowex 50WX8 resin (100–200 mesh) in stoppered glass resin [18] and reported that 85% sorption was achieved bottles which were then shaken at (25 ± 1  °C) in a water for holmium (III), 75% for praseodymium (III), and 12% thermostatic shaker. The concentrations of Pr(III), Dy(III) for cobalt (II) which enables the possibility of separation and Y(III) ions were measured using UV-visible spectro- of cobalt (II) from the investigated lanthanide elements. photometer (a Shimadzu UV-160, Japan) with Arsenazo The extraction and separation of some rare earths from (III) method [21, 22], and the adsorption capacity ( q ) at nitric acid solutions by Cyanex 272 impregnated XAD-7 equilibrium was given by equation: resin has been examined by İnan et al. [19] The obtained M asry et al. BMC Chemistry (2022) 16:37 Page 3 of 12 Desorption investigations Various reagents such as mineral acids, sodium carbon- ate, ammonium carbonate and citric acid (at different pH) were used for the desorption investigations of the metal ions under study. In this context, 0.1  g of Dowex 50WX8 loaded with about 100.0 mg/L of each individual Dy(III) or Pr(III) or Y(III) was shaken with 5.0 mL of the stripping solution for 20.0  min under the same sorption experimental conditions. Results and discussion Characterization of Dowex 50WX8 Figure  2a–d shows the FT-IR spectra of Dowex 50WX8 before and after loading of rare earth metal ions (Pr(III), DY(III) and Y(III)), The spectrum of (Pure Dowex 50WX8) showed adsorption peaks in the ranges of Fig.1 Chemical structure of hydrogenated Dowex 50WX8 resin −1 −1 3330–3450  cm and 1632–1645  cm , which may be attributed to stretching vibrations of the O–H functional group in the structure of the adsorbents [20]. Moreo- −1 Table 1 Specification data sheet of Dowex 50WX8 ver, bands at 1658–1648  cm correspond to the alkene group (C=C) in the Dowex skeleton and bands at1350– Product specification −1 1340  cm are assigned to the stretching S=O of sulfonic Appearance (Color) Faint Yellow to Brown acid. Dowex 50WX8 gives characteristic IR bands for the Appearance (Form) Beads −1 −1 SO vibration (1169  cm ), (S–C) vibration (1121  cm ), Chemical form Strongly acidic hydrogen form containing −1 and (S–O) vibrations (1093 and 1037  cm ) [23]. Previ- 8% divinylbenzene (DVB) ous studies have shown that hydration of the sulfonate Mesh size 100–200 mesh site with H O leads to the formation of hydronium ion Particle size Distribution > 90% within 300 to 1180 UM (H O ‏) species which is the interaction moiety with Wet capacity > 1.7 _MEQ/ML metal ions. Moisture content 50–60% q = (C − C ) × (1) e i e The sorption efficiency (S %) at equilibrium was calcu - (d) DOWEX-Y lated from the equation: C −C i e S% = × 100 (2) (c) DOWEX-Pr where C and C are the initial and equilibrium metal ions i e DOWEX-Dy concentrations (mg/L) of metal ions, respectively; v is the (b) volume of the used aqueous solution in liter (L) and w is the weight of the adsorbent (g). (a) DOWEX Characterization techniques Scanning electron microscopy coupled with energy dis- Before Dy Pr Y persive X-ray spectroscopy (SEM/EDX) was used to examine the morphology and determine the elemen- 4000 3500 3000 2500 2000 1500 1000 500 tal composition of the metal ions bonding to Dowex -1 50WX8 resin under the used experimental conditions. Wavenumbers (Cm ) The functional groups included in the used adsorbent Fig. 2 FT-IR spectra of, a Dowex 50WX8, b Dowex -Dy, c Dowex -Pr, d were investigated using Fourier transform infrared (FT- Dowex -Y for sorption of rare earth metal ions from nitrate medium IR) spectroscopy (Bruker) in the scanning range of 4000– −1 400  cm and pH was measured using Hannah pH meter. % Transmittance Masry et al. BMC Chemistry (2022) 16:37 Page 4 of 12 The FT-IR spectrum of Dowex after interaction with The results of the EDX and Map analyses indicate REE metal ions, indicate that adsorbing species (Dowex/ the presence of different elements on the surface of the Pr/Dy/Y) were formed at the counter ion of the Dowex Dowex 50WX8, including Praseodymium, Dysprosium 50WX8 (H ) which protonates with H O to form the and yttrium, with the elements distributed uniformly Dowex 50WX8(H O ) species [20]. across the resin surface Fig.  4(a–d). Consequently, the The morphology investigations and particle surface results of the EDX and Map analyses affirm the success - variations of the sorbent were given by EDX. Map and ful bonding of the metal ions on the surface of Dowex SEM analyses were performed both before and after the 50WX8. adsorption of metal ions, Fig. 3a–d. The obtained results show the presence of a variety of pores with a wide range Sorption batch experiments of pore size on the surface of the Dowex 50WX8 resin; Effect of shaking time the pore space could be attributed to the adsorption The impact of contact time on the sorption efficiency process. of Pr(III), Dy(III) and Y(III) ions using Dowex 50WX8 Fig. 3 SEM images of, a Dowex 50WX8 before sorption process, b after sorption of Pr(III), c after sorption of Dy(III), d after sorption of Y(III) from nitrate medium M asry et al. BMC Chemistry (2022) 16:37 Page 5 of 12 sorbent from nitrate medium was carried out in the was investigated in the range of 0.02–0.25  L/g, Fig.  5b. range 1.0–90.0  min. The results indicated that the rare The obtained results show that the adsorption efficiency earth ions sorption process took 1–15  min to occur and yield takes the order DY(III) > Pr(III) > Y(III) enhanced was based on the availability of vacant active sites The abruptly by increasing v/m from 0.1  L/g up to 0.25  L/g. rate of adsorption on the surface of the adsorbents was Based on the obtained results, the optimal adsorbent significantly decreased at contact times beyond 15.0 min, dosage on Dowex was fixed at 0.05 L/g in all experiments Fig. 5a possibly because of the saturation of the available carried out in this work. active sites on the sorbent surface; accordingly the equi- librium contact time for the sorption of the investigated Effect of nitric acid concentration metal ions using Dowex adsorbent was fixed at 15.0 min. The adsorption of Pr(III), Dy(III) and Y(III) from differ - ent nitric acid concentrations is given in Fig.  5c and the Adsorbent dosage experimental results revealed that the adsorption effi - The sorbent dosage is another key factor imposing large ciency of Dowex ion exchanger decreased rapidly upon contribution to the sorption process, as it can determine increasing nitric acid concentration from 0.50 to 3.0  M. the adsorption efficiency of the sorbent for a given ini - This may be attributed to the compensation of H with tial concentration of the investigated metal ions [24]. In higher increasing of acid concentration which leads to this respect, the impact of the sorbent dosage (v/m) on a decrease in the exchange rate between hydrogen ion the adsorption efficiency of Pr(III), Dy(III) and Y(III) ions Fig. 4 EDX-analysis of a Dowex 50WX8 before sorption process, b after sorption of Pr(III), c after sorption of Dy(III), d after sorption of Y(III) from nitrate medium Masry et al. BMC Chemistry (2022) 16:37 Page 6 of 12 Fig. 5 a Eec ff t of contact time on the adsorption efficiency of Pr(III), Dy(III) and Y(III) using Dowex 50WX8 from nitrate medium (temperature: 25 °C, initial ion concentration: 100 mg/L, v/m = 0.05 L/g, b Eec ff t of the sorbent dosage on the adsorption efficiency (at optimal pH value, contact time = 15.0 min, initial metal ion concentration 100 mg/L, temperature: 25 °C, c Eec ff t of nitric acid concentration, d Eec ff t of metal ion concentrations on the sorption of Dy, Pr and Y using Dowex 50WX8 and metal ions; with further increase in the acid molar- by Dowex from nitrate medium. The experiments were ity higher than 3.0 M the adsorption capacity became sta- carried out by shaking 5.0  mL of the investigated metal ble, Fig. 5c. However, the experiments were performed at ions solution individually with 0.05 g of the adsorbent for 0.5 M HNO . 15.0  min at 25  °C. The obtained data are represented in Fig.  5d, The adsorption efficiency increased as the con - Effect of metal ions concentration centration of R EEs increased and the highest adsorp- The effect of the initial concentration of Pr(III), Dy(III) tion capacities of 29.0  mg/g, 25.0  mg/g and 24.0  mg/g and Y(III) on the adsorption capacity ( q ) was studied were achieved at 500  mg/L for Dy, Pr and Y, respec- −1 in the range of 50–500  mg L through their sorption tively. This saturation can be ascribed to the interactions M asry et al. BMC Chemistry (2022) 16:37 Page 7 of 12 −1 between the adsorbent active sites and these metal ions. concentration in solution (mg L ), Q the maximum −1 [25]. capacity of the adsorbent. (mg g ), and b the Langmuir −1 adsorption constant (L mg ). Nonlinear Freundlich iso- therm equation is given as: + + Sorption mechanism of REE with Dowex‑H 1/n q = K C (6) Based on the experimental results and considering that e f M (NO ) is the predominant species in 1.0  M nitric 3 2 where K is the Freundlich constant (mg/g). acid solution [21, 26], where M represents Pr(III), Dy(III) Nonlinear Temkin isotherm model which takes into and Y(III),The ion exchange extraction mechanism of account the interactions of ions of the aqueous solution REEs metal ion (M) with Dowex-H was suggested to pro- and the adsorbent and is given as: ceed via different reaction pathways from Eqs. (3) and (4), [20] RT q = ln(A C ) (7) e T e + + 3DOWEX − SO − 3H + M(NO ) 3 3 where R is the universal gas constant (8.314  J/mol K), T ⇋ 2DOWEX − SO − MNO 3 3 (3) + the absolute temperature, b a constant related to the heat + HNO3 + DOWEX − SO − H of sorption (J/mol), A the equilibrium binding constant (L/g) and b the adsorption constant (J/mol K). 3DOWEX − SO − 3H + M(NO ) 3 3 2 Toth isotherm model is another empirical equation ⇋ DOWEX − SO − MNO 3 3 (4) developed to improve Langmuir isotherm fittings and take into consideration both low and high-end boundary +2DOWEX − SO − 2H of the concentration and is given as, [30, 31] Equation  (3) suggests that the extraction mechanism q = q exp(−βε ) (8) occurs via partial ion exchange reactions during the e m REE diffusion and interaction at the Dowex active sites SO -H where the extracted metal ions species according ε = RT ln 1 + (9) to Eq. (3) were found to be Dowex-SO -Pr(NO ), Dowex- 3 3 SO -Dy(NO ) and Dowex-SO -Y(NO ) for Pr, Dy and Y 3 3 3 3 respectively. E = (10) 0.5 (2β) Adsorption isotherm of Pr, Dy and Y on the Dowex 50WX8 The relationship between q and C for each nonlinear iso- e e cation exchanger therm model is plotted in (Fig.  6 a–e) and the values of the Adsorption isotherms were used to describe the distri- obtained parameters are tabulated in Table  2. The results bution of metal ions between the sample solution (liquid indicate that Pr and Y fitted with nonlinear Langmuir iso - phase) and the resin (solid phase) when the ion exchange therm model with regression factors 0.995 and 0.978 respec- process reaches equilibrium [27, 28]. The Langmuir iso - tively, while, Dy was fitted with nonlinear Toth isotherm therm model describes a homogeneous monolayer chem- model with R = 0.966. ical adsorption process, while the Freundlich isotherm model describes a heterogeneous physical adsorption Desorption, reusability and separation process [29]. Non-liner models achieved the most flexible between Dy, Pr and Y from nitrate medium using curve fitting functionality. In this context, Langmuir, Fre - Dowex 50WX8 undlich, Temkin, D–R isotherm and Toth isotherm were The most effective separation obtained between the employed for studying the nonlinear adsorption isotherm investigated metal ions was obtained from the stripping of Pr, Dy and Y on the cation exchanger resin (Dowex process. This process was carried out by contacting the 50WX8). loaded Dowex 50WX8 with different stripping agents Nonlinear Langmuir isotherm equation is given as: at experimental conditions (contact time = 60.0  min, v/m = 0.05 at 25 ± 1 °C). The results illustrated in Table  3 bC q = Q (5) e show that the maximum stripping of Pr(III) is 58% and 1 + bC was achieved with 1.0 M citric acid at pH = 3. In the case where q is the equilibrium adsorption capacity of ions of Dy(III) and Y(III) the maximum desorption is 55% −1 on the adsorbent (mg g ), C is the equilibrium ions e Masry et al. BMC Chemistry (2022) 16:37 Page 8 of 12 Fig. 6 a Nonlinear isotherm plot of Langmuir model, b Nonlinear isotherm plot of Freundlich model, c Nonlinear isotherm plot of D-R, d Nonlinear isotherm plot of Temkin model, d Nonlinear isotherm plot Toth model for adsorption of Pr(III), DY(III) and Y(III) onto Dowex 50WX8 Furthermore, the separation ratio (S-ratio) between and 56% and was achieved with [H NO ] = 1.0  M and the investigated metal ions were calculated by divid- [(NH ) CO ] = 1.0  M, respectively. A flow sheet which 4 2 3 ing their desorption percentages. The results indicate illustrates the sorption and desorption processes of the that the maximum S-ratios are 56.0, 35.0 and 4.6 for Y/ investigated rare earth using D-50WX8 from 0.5  M Pr, Dy/Pr and were achieved with [(NH ) CO ] = 1.0 and HNO solution at v/m = 0.05 at 25 ± 1  °C is given in 4 2 3 [HNO ] = 5.0 M respectively, Table 3. Fig. 7. Finally, the reported results show that Dowex 50WX8 The desorption results indicate that Pr(III) can be sepa - resin is relatively selective, high efficient and cost effec - rated from Dy(III) and Y(III) as follows: tive for Pr(III), Dy(III) and Y(III) adsorption and is also easily regenerated rather than other reported adsorbent/ i. Stripping of Dy(III) and Y(III) using [(NH ) CO ] = 1.0 M 4 2 3 ion exchangers which were used in the adsorption from from Loaded Dowex 50WX8 after 2 cycles acidic nitrate medium. The reusability was carried out for ii. Dowex 50WX8 containing Pr(III) was then 4.0 adsorption stages with sorption capacity of 15.0, 30.0, stripped with 1.0 M citric acid at pH = 3 after two 35.0 mg/g for Pr, DY and Y, respectively, under the used stripping cycles experimental conditions. M asry et al. BMC Chemistry (2022) 16:37 Page 9 of 12 Table 2 Nonlinear Freundlich, Langmuir, Dubinin–Radushkevich, Temkin and Toth isotherm parameters for adsorption of metal ions onto Dowex 50WX8 Isotherm Parameters Metal ions DY(III) Pr(III) Y(III) Langmuir Qo (mg/g) 62.32 36.94 48.76 b (ml/mg) 0.0041 0.0074 0.0035 R 0.707 0.575 0.739 R 0.956 0.995 0.978 Chi^2 5.36 0.43 1.97 Freundlich K (mg/g) 0.632 1.044 0.491 1/n 0.719 0.569 0.694 R 0.944 0.971 0.959 Chi^2 6.765 2.604 3.597 Dubinin–Radushkevich q 245.38 116.96 142.26 2 2 β mol /kJ 0.0078 0.0064 0.0086 R 0.952 0.484 0.971 E 7.996 8.846 7.612 DR Chi^2 2.20 E-10 7.11E-11 3.23E-10 Tempkin Q , kJ/mol 280.66 351.33 328.04 K , mmol/g 0.0888 0.1017 0.0657 R 0.8989 0.9738 0.9119 Chi^2 12.3 2.34 7.77 Toth isotherm q , mg/g 23.19 25.02 49.11 Fig. 7 Flow sheet for the sorption and desorption processes of Pr, DY K 0.035 0.04 0.017 and Y using Dowex 50WX8 N 1.018 1.057 1.048 R 0.9668 0.987 0.991 x 1.504 1.19 1.688 Conclusions Dowex 50WX8 was successfully used for the recovery of Comparison study of REEs/Dowex 50WX8 with other DY(III), Pr(III) and Y(III) from acidic nitrate medium. reported materials The calculated maximum capacity of Dowex 50WX8 Comparison of REEs/Dowex 50WX8 system under the is 30, 50, 60  mg/g for Pr, DY and Y respectively at the used optimum conditions of batch technique with other optimum batch conditions; the maximum stripping of commercially reported materials [18, 32–51] and given Pr(III) is 58.0% and was achieved with 1.0 M citric acid at in Table 4, shows the advantages and efficiency of Dowex pH = 3. The results indicate that Pr(III) and Y(III) fitted 50WX8 adsorbent. The results of comparison in the with nonlinear Langmuir isotherm model with regres- term of maximum capacity (Q ) (30, 50, 60  mg/g for Pr, sion factors 0.995 and 0.978 respectively. The regenerated DY and Y), pH = 1, and contact time (15 min) and which Dowex 50WX8 gave sorption capacities of 15.0, 30.0, were achieved in the current study indicate that Dowex 35.0  mg/g for Pr, DY and Y, respectively under the used 50WX8 is more efficient and affordable than other experimental conditions. reported materials. Masry et al. BMC Chemistry (2022) 16:37 Page 10 of 12 Table 3 Desorption of metal ions (III) with different reagents after their adsorption with the Dowex 50WX8 resin at v/m = 0.05 at 25 ± 1 °C Stripping agent, M Dy(III) Pr(III) Y(III) S-ratio Dy/Pr Y/Pr Dy/Y HNO , 1.0 M 24.9 23.7 28 1.05 1.2 1 HNO , 5.0 M 55.4 12 43 4.6 3.6 1.2 HCl, 1.0 M – – 7.72 – – – H SO , 1.0 M 32.9 32.6 31 1 – 1.05 2 4 Na CO , 1.0 M 21 25.9 20 – – 1 2 3 (NH ) CO , 1.0 M 35 – 56 35 56 – 4 2 3 Citric acid (1.0 M) pH 1 – – – – – pH 3 40.12 58.37 39.25 – 1 pH 5 18.11 35.26 20.46 – – Table 4 Comparison study of REEs/Dowex 50WX8 with other reported materials Metal ion Adsorbent Q , mg/g pH Contact Time Refs Zeolitic imidazolate frameworks nanoparticles 430.4 7.0 7.0 h [1] Oxidized multi-walled carbon nanotubes 78.12 5.0 2.0 h [2] Silica/polyvinyl imidazole/H2PO4-core–shell NPs 150 4.0 0.5 h [3] Hybrid Lewis base ligands functionalized alumina-silica 125.4 4.0 3.0 h [4] polyethylenimine–acrylamide/SiO hybrid hydrogel 50–100 2-7 6.0 h [9] Microcapsules containing dibenzoylmethane 70.85 6.0 60.0 h [12] D113 resin 292.7 6.0 – [15] Macroporous poly(vinylphosphoramidic acid) resin 101 4-5 – [14] Zr-modified mesoporous silica supported H4[PMo VO ] 52.63 5.0 1.0 h [13] 11 40 Polyacrylic acid grafted silica fume 251.20 1-6 1.0 h [11] Pr(III) Lanthanide-ion imprinted polymers (L-IIPs) 125.3 6.0 1.5 h [5] Polyethylenimine sodium phosphonate resin (PEIPR.Na) 6.23 4.0 250 min [18] Fe O @TiO @P 0 nanoparticles 10.2 5.0 – [19] 3 4 2 2 4 TVEX–PHOR resin 49 3.5 1.0 h [20] magnetic nanoparticles functionalized with a phosphonic group 17.6 4.0 1.0 h [21] silica gel modified with diglycol amic acid 12.72 1.0 – [22] Graphene Oxide Nanosheets 135 6.0 2.0 h [6] Graphene oxide nanosheets with cross-linked by high-gluten flour 32.84 7.5 2.0 h [7] Y(III) Porous three-dimensional graphene oxide-corn zein composites 14.2 – 3.33 h [8] Carbon nanotubes reinforced silica composite 68.8 4.0 24.0 h [10] Functionalized silica in the hybridization process with chitosan 159 4.0 24.0 h [16] Diglycolamic-acid modified chitosan sponges 40.7 0.5–7 12.0 h [17] Funding Declaration Open access funding provided by The Science, Technology & Innovation Funding Authority (STDF) in cooperation with The Egyptian Knowledge Acknowledgements Bank (EKB). Science, Technology & Innovation Funding Authority (STDF) and Authors are thankful to the Egyptian Atomic Energy Authority for its continu- springer nature open access agreement. ous support for scientific research and development. Availability of data and materials Author contributions All data generated or analyzed during this study are included in this published BAM: Conceptualization, writing—original draft, data analysis. EMAE and SER: article [and its supplementary information files]. Methodology, resources, formal analysis, and data analysis. All authors read and approved the final manuscript. M asry et al. BMC Chemistry (2022) 16:37 Page 11 of 12 22. Marczenko Z. Spectrophotometric determination of elements; Ellis Declarations Harwood. Poland: Ltd; 1976. 23. RM Silverstein FX Webster DJ Kiemle 2005 Spectrometric Identification of Ethics approval and consent to participate organic compounds Hoboken John Wiley 502 35 The manuscript does not contain studies with animal subjects. 24. Masry BA, Elhady MA, Mousaa IM. Fabrication of a novel polyvinylpyr- rolidone/abietic acid hydrogel by gamma irradiation for the recovery of Consent for publication Zn Co Mn and Ni from aqueous acidic solution. Inorg Nano Met Chem,. All authors approved the paper submission. 2022. https:// doi. org/ 10. 1080/ 24701 556. 2022. 20348 60. 25. El-saied HA, Shahr El-Din AM, Masry BA, Ibrahim AM. A promising supera- Competing interests bsorbent nanocomposite based on grafting biopolymer/nanomag- The authors declare that they have no competing interests. 134 85 60 netite for capture of Cs, Sr and Co radionuclides. J Polym Environ. 2020;28(6):1749. Received: 24 March 2022 Accepted: 10 May 2022 26. Masry BA, Aly MI, Khalifa NA, Zikry AAF, Gasser MS, Daoud JA. 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Modeling and equilibrium studies on the recovery of praseodymium (III), dysprosium (III) and yttrium (III) using acidic cation exchange resin

BMC Chemistry , Volume 16 (1) – May 25, 2022

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Abstract

In this research, the possibility of using hydrogenated Dowex 50WX8 resin for the recovery and separation of Pr(III), Dy(III) and Y(III) from aqueous nitrate solutions were carried out. Dowex 50WX8 adsorbent was characterized before and after sorption of metal ions using Fourier-transform infrared spectroscopy (FT-IR), Scanning Electron Microscope (SEM) and Energy Dispersive X-Ray Analysis (EDX) techniques. Sorption parameters were studied which included contact time, initial metal ion concentration, nitric acid concentration and adsorbent dose. The equilibrium time has been set at about 15.0 min. The experimental results showed that the sorption efficiency of metal ions under the investigated conditions decreased with increasing nitric acid concentration from 0.50 to 3.0 M. The maximum sorption capacity was found to be 30.0, 50.0 and 60.0 mg/g for Pr(III), DY(III) and Y(III), respectively. The desorption of Pr(III) from the loaded resin was achieved with 1.0 M citric acid at pH = 3 and found to be 58.0%. On the other hand, the maximum desorption of Dy(III) and Y(III) were achieved with 1.0 M nitric acid and 1.0 M ammonium carbonate, respectively. The sorption isotherm results indicated that Pr(III) and Y(II) fitted with nonlinear Langmuir isotherm model with regression factors 0.995 and 0.978, respectively; while, Dy(III) fitted with nonlinear Toth isotherm model with R = 0.966. A Flow sheet which summarizes the sorption and desorption processes of Pr(III), DY(III) and Y(III) using Dowex 50WX8 from nitric acid solution under the optimum conditions is also given. Keyword: Modeling, Dowex 50WX8, Adsorption, Rare earth metals Introduction industries, color televisions, computer monitors and tem- Yttrium (Y), Dysprosium (Dy) and Praseodymium (Pr) perature sensors [1, 2]. Praseodymium is used with neo- known as segment of the rare earth elements (REEs) are dymium in combination for goggles to shield glassmakers spirited components in fluorescent lamps, glass polish - against sodium glare, permanent magnets and cryogenic ing and ceramics, computer monitors, lighting, radar, refrigerant [3]. Dysprosium alloy with neodymium is televisions, and X-ray intensifying films. Yttrium is exten - used for permanent magnets, catalysts, speakers, com- sively used in the manufacturing of several high-tech- pact discs and hard discs and medium source rare-earth devices such as microwave communication for satellite lamps within the film industry. [4] Ion exchange separa - tion of rare earth elements was used by Spedding and Powell to separate REEs from fission products obtained from nuclear reactors [5–7]. Sorption processes for the *Correspondence: betaam24@yahoo.com; Botros.masry@eaea.org.eg separation of rare earths have been reviewed in several Chemistry of Nuclear Fuel Department, Hot Laboratories Centre, Egyptian articles [8–11]. Strongly acidic cation exchangers were Atomic Energy Authority, Cairo, Egypt © The Author(s) 2022. Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article’s Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http:// creat iveco mmons. org/ licen ses/ by/4. 0/. The Creative Commons Public Domain Dedication waiver (http:// creat iveco mmons. org/ publi cdoma in/ zero/1. 0/) applies to the data made available in this article, unless otherwise stated in a credit line to the data. Masry et al. BMC Chemistry (2022) 16:37 Page 2 of 12 the first artificial functional polymers used for the sepa - results indicated that REEs have a tendency to behave as ration of REE ions, and they are resumed predominating two different groups that can be separated into two frac - in the fields of chemistry and chemical technology under tions as La, Pr, Nd and Sm, Eu, Gd. Dowex 50wx8 was consideration [11]. Styrene and divinylbenzene copoly- used previously for the reversible ion exchange of cerium mers bearing SO H group are utilized. Now, modifica - (III) sulfate and Cerium (III) nitrate where the experi- tions of these exchangers are manufactured under the mental results indicate that the continuous liquid flow trade names Amberlite, Dowex, Lewatit, Purolit, which reactor studies show a capacity of 0.72  mmol/g sorbent differ by the degree of cross linking sorption capac - for the Ce nitrate and 0.96  mmol/g sorbent for the Ce ity, grain size, pore diameter, and other parameter [12]. sulfate [20]. Dowex 50  W-X8 is one of the ion-exchange resins that The main objective of the present work is directed to have been used for separation of REEs from other ions study the sorption and separation of Praseodymium, as well as separation of individual REEs from a mixture Dysprosium and Yttrium from nitric acid solution using of REEs. Al-y Th abat and Zhang, studied the recovery of strongly acidic cationic exchange resin (Dowex 50WX8) REEs resulting from phosphoric acid with Dowex 50WX4 using batch technique. The effects different parameters and Dowex 50WX8 resins. Their results indicated that on the sorption and separation processes will be inves- the REE-extraction efficiency of Dowex 50WX8 was tigated such as contact time, nitric acid concentration, almost twice that of Dowex 50WX4 resin. This can be as well as v/m ratio and temperature. Desorption inves- explained by the higher exchange capacity, producing tigations will be also carried out and evaluated. Separa- more sulfonic groups, of Dowex 50WX8 even though tion feasibility between the investigated REEs are also its lower surface area and larger bead size [13]. Felipe discussed based on the difference between their sorption et  al., studied the recovery of rare earth elements from and desorption behavior. acid mine drainage by ion exchange [14] and reported that the highest loading capacities were 0.212  mmol Experimental −1 −1 g for La and 0.169  mmol g for Ce (Dowex 50WX8) Materials and chemicals −1 −1 and 0.210  mmol g for La and 0.173  mmol g for Ce The chemicals used in this work were of analytical rea - (Lewatit MDS 200 H). Recovery of rare earth elements gent grade (AR) and most of them were used without fur- from uranium concentrate by using cation exchange resin ther purification. Stock solutions of Pr(III), DY(III) and (Dowex 50WX8) was studied and the authors reported Y(III) (1000 mg/L) were prepared by dissolving a known that the maximum REE sorption capacity was found to amount of the metal oxide in minimum concentrated 82.74 mg/g which represents about 93.23% of the original nitric acid and evaporated to near dryness and then made capacity of the studied resin [15]. Sorption of rare earth up to the mark in a measuring flask with double distilled elements from nitric acid solution with macroporous sil- water. The desired required concentrations of test solu - ica-based bis(2-ethylhexyl)phosphoric acid impregnated tions were prepared by favorable dilution with a known polymeric adsorbent has been studied by Shu et  al. [16] concentrated nitric acid of the stock solutions. Dowex Their results indicated that the adsorption capacity of 50WX8 which is a strong acid cation resin containing 8% −1 Gd (III) was found to be 0.315  mmol g by bis(2-ethyl- divinylbenzene (DVB) [20], Fig.  1 was purchased from hexyl)phosphoric acid/SiO -P in 0.1  M H NO . Adsorp- sigma Aldrich. The chemical and physical specifications 2 3 tion and separation of terbium(III) and gadolinium(III) of Dowex 50X8 are given in table given in Table 1. from aqueous nitrate medium has been investigated using TVEX-PHOR resin by Madbouly et  al. [17]. Their Sorption experiments work showed that the maximum sorption capacity of The sorption experiments were carried out under the fol - this material was 15.49 mg/g and 24.93 mg/g for Gd(III) lowing conditions, v/m = 0.05 L/g, Pr(III), DY(III) and and Tb(III) from 0.1  M NaNO solution, respectively Y(III) concentrations = 100.0  mg/L in 0.50  M nitric acid at pH = 5.2 and V/m = 0.1. El-Dessouky et  al. studied solution. In each adsorption experiment, 5.0  ml of the the sorption of praseodymium (III), holmium (III) and investigated metal ions solution was added to 0.1  g of cobalt (II) from nitrate medium using TVEX–PHOR Dowex 50WX8 resin (100–200 mesh) in stoppered glass resin [18] and reported that 85% sorption was achieved bottles which were then shaken at (25 ± 1  °C) in a water for holmium (III), 75% for praseodymium (III), and 12% thermostatic shaker. The concentrations of Pr(III), Dy(III) for cobalt (II) which enables the possibility of separation and Y(III) ions were measured using UV-visible spectro- of cobalt (II) from the investigated lanthanide elements. photometer (a Shimadzu UV-160, Japan) with Arsenazo The extraction and separation of some rare earths from (III) method [21, 22], and the adsorption capacity ( q ) at nitric acid solutions by Cyanex 272 impregnated XAD-7 equilibrium was given by equation: resin has been examined by İnan et al. [19] The obtained M asry et al. BMC Chemistry (2022) 16:37 Page 3 of 12 Desorption investigations Various reagents such as mineral acids, sodium carbon- ate, ammonium carbonate and citric acid (at different pH) were used for the desorption investigations of the metal ions under study. In this context, 0.1  g of Dowex 50WX8 loaded with about 100.0 mg/L of each individual Dy(III) or Pr(III) or Y(III) was shaken with 5.0 mL of the stripping solution for 20.0  min under the same sorption experimental conditions. Results and discussion Characterization of Dowex 50WX8 Figure  2a–d shows the FT-IR spectra of Dowex 50WX8 before and after loading of rare earth metal ions (Pr(III), DY(III) and Y(III)), The spectrum of (Pure Dowex 50WX8) showed adsorption peaks in the ranges of Fig.1 Chemical structure of hydrogenated Dowex 50WX8 resin −1 −1 3330–3450  cm and 1632–1645  cm , which may be attributed to stretching vibrations of the O–H functional group in the structure of the adsorbents [20]. Moreo- −1 Table 1 Specification data sheet of Dowex 50WX8 ver, bands at 1658–1648  cm correspond to the alkene group (C=C) in the Dowex skeleton and bands at1350– Product specification −1 1340  cm are assigned to the stretching S=O of sulfonic Appearance (Color) Faint Yellow to Brown acid. Dowex 50WX8 gives characteristic IR bands for the Appearance (Form) Beads −1 −1 SO vibration (1169  cm ), (S–C) vibration (1121  cm ), Chemical form Strongly acidic hydrogen form containing −1 and (S–O) vibrations (1093 and 1037  cm ) [23]. Previ- 8% divinylbenzene (DVB) ous studies have shown that hydration of the sulfonate Mesh size 100–200 mesh site with H O leads to the formation of hydronium ion Particle size Distribution > 90% within 300 to 1180 UM (H O ‏) species which is the interaction moiety with Wet capacity > 1.7 _MEQ/ML metal ions. Moisture content 50–60% q = (C − C ) × (1) e i e The sorption efficiency (S %) at equilibrium was calcu - (d) DOWEX-Y lated from the equation: C −C i e S% = × 100 (2) (c) DOWEX-Pr where C and C are the initial and equilibrium metal ions i e DOWEX-Dy concentrations (mg/L) of metal ions, respectively; v is the (b) volume of the used aqueous solution in liter (L) and w is the weight of the adsorbent (g). (a) DOWEX Characterization techniques Scanning electron microscopy coupled with energy dis- Before Dy Pr Y persive X-ray spectroscopy (SEM/EDX) was used to examine the morphology and determine the elemen- 4000 3500 3000 2500 2000 1500 1000 500 tal composition of the metal ions bonding to Dowex -1 50WX8 resin under the used experimental conditions. Wavenumbers (Cm ) The functional groups included in the used adsorbent Fig. 2 FT-IR spectra of, a Dowex 50WX8, b Dowex -Dy, c Dowex -Pr, d were investigated using Fourier transform infrared (FT- Dowex -Y for sorption of rare earth metal ions from nitrate medium IR) spectroscopy (Bruker) in the scanning range of 4000– −1 400  cm and pH was measured using Hannah pH meter. % Transmittance Masry et al. BMC Chemistry (2022) 16:37 Page 4 of 12 The FT-IR spectrum of Dowex after interaction with The results of the EDX and Map analyses indicate REE metal ions, indicate that adsorbing species (Dowex/ the presence of different elements on the surface of the Pr/Dy/Y) were formed at the counter ion of the Dowex Dowex 50WX8, including Praseodymium, Dysprosium 50WX8 (H ) which protonates with H O to form the and yttrium, with the elements distributed uniformly Dowex 50WX8(H O ) species [20]. across the resin surface Fig.  4(a–d). Consequently, the The morphology investigations and particle surface results of the EDX and Map analyses affirm the success - variations of the sorbent were given by EDX. Map and ful bonding of the metal ions on the surface of Dowex SEM analyses were performed both before and after the 50WX8. adsorption of metal ions, Fig. 3a–d. The obtained results show the presence of a variety of pores with a wide range Sorption batch experiments of pore size on the surface of the Dowex 50WX8 resin; Effect of shaking time the pore space could be attributed to the adsorption The impact of contact time on the sorption efficiency process. of Pr(III), Dy(III) and Y(III) ions using Dowex 50WX8 Fig. 3 SEM images of, a Dowex 50WX8 before sorption process, b after sorption of Pr(III), c after sorption of Dy(III), d after sorption of Y(III) from nitrate medium M asry et al. BMC Chemistry (2022) 16:37 Page 5 of 12 sorbent from nitrate medium was carried out in the was investigated in the range of 0.02–0.25  L/g, Fig.  5b. range 1.0–90.0  min. The results indicated that the rare The obtained results show that the adsorption efficiency earth ions sorption process took 1–15  min to occur and yield takes the order DY(III) > Pr(III) > Y(III) enhanced was based on the availability of vacant active sites The abruptly by increasing v/m from 0.1  L/g up to 0.25  L/g. rate of adsorption on the surface of the adsorbents was Based on the obtained results, the optimal adsorbent significantly decreased at contact times beyond 15.0 min, dosage on Dowex was fixed at 0.05 L/g in all experiments Fig. 5a possibly because of the saturation of the available carried out in this work. active sites on the sorbent surface; accordingly the equi- librium contact time for the sorption of the investigated Effect of nitric acid concentration metal ions using Dowex adsorbent was fixed at 15.0 min. The adsorption of Pr(III), Dy(III) and Y(III) from differ - ent nitric acid concentrations is given in Fig.  5c and the Adsorbent dosage experimental results revealed that the adsorption effi - The sorbent dosage is another key factor imposing large ciency of Dowex ion exchanger decreased rapidly upon contribution to the sorption process, as it can determine increasing nitric acid concentration from 0.50 to 3.0  M. the adsorption efficiency of the sorbent for a given ini - This may be attributed to the compensation of H with tial concentration of the investigated metal ions [24]. In higher increasing of acid concentration which leads to this respect, the impact of the sorbent dosage (v/m) on a decrease in the exchange rate between hydrogen ion the adsorption efficiency of Pr(III), Dy(III) and Y(III) ions Fig. 4 EDX-analysis of a Dowex 50WX8 before sorption process, b after sorption of Pr(III), c after sorption of Dy(III), d after sorption of Y(III) from nitrate medium Masry et al. BMC Chemistry (2022) 16:37 Page 6 of 12 Fig. 5 a Eec ff t of contact time on the adsorption efficiency of Pr(III), Dy(III) and Y(III) using Dowex 50WX8 from nitrate medium (temperature: 25 °C, initial ion concentration: 100 mg/L, v/m = 0.05 L/g, b Eec ff t of the sorbent dosage on the adsorption efficiency (at optimal pH value, contact time = 15.0 min, initial metal ion concentration 100 mg/L, temperature: 25 °C, c Eec ff t of nitric acid concentration, d Eec ff t of metal ion concentrations on the sorption of Dy, Pr and Y using Dowex 50WX8 and metal ions; with further increase in the acid molar- by Dowex from nitrate medium. The experiments were ity higher than 3.0 M the adsorption capacity became sta- carried out by shaking 5.0  mL of the investigated metal ble, Fig. 5c. However, the experiments were performed at ions solution individually with 0.05 g of the adsorbent for 0.5 M HNO . 15.0  min at 25  °C. The obtained data are represented in Fig.  5d, The adsorption efficiency increased as the con - Effect of metal ions concentration centration of R EEs increased and the highest adsorp- The effect of the initial concentration of Pr(III), Dy(III) tion capacities of 29.0  mg/g, 25.0  mg/g and 24.0  mg/g and Y(III) on the adsorption capacity ( q ) was studied were achieved at 500  mg/L for Dy, Pr and Y, respec- −1 in the range of 50–500  mg L through their sorption tively. This saturation can be ascribed to the interactions M asry et al. BMC Chemistry (2022) 16:37 Page 7 of 12 −1 between the adsorbent active sites and these metal ions. concentration in solution (mg L ), Q the maximum −1 [25]. capacity of the adsorbent. (mg g ), and b the Langmuir −1 adsorption constant (L mg ). Nonlinear Freundlich iso- therm equation is given as: + + Sorption mechanism of REE with Dowex‑H 1/n q = K C (6) Based on the experimental results and considering that e f M (NO ) is the predominant species in 1.0  M nitric 3 2 where K is the Freundlich constant (mg/g). acid solution [21, 26], where M represents Pr(III), Dy(III) Nonlinear Temkin isotherm model which takes into and Y(III),The ion exchange extraction mechanism of account the interactions of ions of the aqueous solution REEs metal ion (M) with Dowex-H was suggested to pro- and the adsorbent and is given as: ceed via different reaction pathways from Eqs. (3) and (4), [20] RT q = ln(A C ) (7) e T e + + 3DOWEX − SO − 3H + M(NO ) 3 3 where R is the universal gas constant (8.314  J/mol K), T ⇋ 2DOWEX − SO − MNO 3 3 (3) + the absolute temperature, b a constant related to the heat + HNO3 + DOWEX − SO − H of sorption (J/mol), A the equilibrium binding constant (L/g) and b the adsorption constant (J/mol K). 3DOWEX − SO − 3H + M(NO ) 3 3 2 Toth isotherm model is another empirical equation ⇋ DOWEX − SO − MNO 3 3 (4) developed to improve Langmuir isotherm fittings and take into consideration both low and high-end boundary +2DOWEX − SO − 2H of the concentration and is given as, [30, 31] Equation  (3) suggests that the extraction mechanism q = q exp(−βε ) (8) occurs via partial ion exchange reactions during the e m REE diffusion and interaction at the Dowex active sites SO -H where the extracted metal ions species according ε = RT ln 1 + (9) to Eq. (3) were found to be Dowex-SO -Pr(NO ), Dowex- 3 3 SO -Dy(NO ) and Dowex-SO -Y(NO ) for Pr, Dy and Y 3 3 3 3 respectively. E = (10) 0.5 (2β) Adsorption isotherm of Pr, Dy and Y on the Dowex 50WX8 The relationship between q and C for each nonlinear iso- e e cation exchanger therm model is plotted in (Fig.  6 a–e) and the values of the Adsorption isotherms were used to describe the distri- obtained parameters are tabulated in Table  2. The results bution of metal ions between the sample solution (liquid indicate that Pr and Y fitted with nonlinear Langmuir iso - phase) and the resin (solid phase) when the ion exchange therm model with regression factors 0.995 and 0.978 respec- process reaches equilibrium [27, 28]. The Langmuir iso - tively, while, Dy was fitted with nonlinear Toth isotherm therm model describes a homogeneous monolayer chem- model with R = 0.966. ical adsorption process, while the Freundlich isotherm model describes a heterogeneous physical adsorption Desorption, reusability and separation process [29]. Non-liner models achieved the most flexible between Dy, Pr and Y from nitrate medium using curve fitting functionality. In this context, Langmuir, Fre - Dowex 50WX8 undlich, Temkin, D–R isotherm and Toth isotherm were The most effective separation obtained between the employed for studying the nonlinear adsorption isotherm investigated metal ions was obtained from the stripping of Pr, Dy and Y on the cation exchanger resin (Dowex process. This process was carried out by contacting the 50WX8). loaded Dowex 50WX8 with different stripping agents Nonlinear Langmuir isotherm equation is given as: at experimental conditions (contact time = 60.0  min, v/m = 0.05 at 25 ± 1 °C). The results illustrated in Table  3 bC q = Q (5) e show that the maximum stripping of Pr(III) is 58% and 1 + bC was achieved with 1.0 M citric acid at pH = 3. In the case where q is the equilibrium adsorption capacity of ions of Dy(III) and Y(III) the maximum desorption is 55% −1 on the adsorbent (mg g ), C is the equilibrium ions e Masry et al. BMC Chemistry (2022) 16:37 Page 8 of 12 Fig. 6 a Nonlinear isotherm plot of Langmuir model, b Nonlinear isotherm plot of Freundlich model, c Nonlinear isotherm plot of D-R, d Nonlinear isotherm plot of Temkin model, d Nonlinear isotherm plot Toth model for adsorption of Pr(III), DY(III) and Y(III) onto Dowex 50WX8 Furthermore, the separation ratio (S-ratio) between and 56% and was achieved with [H NO ] = 1.0  M and the investigated metal ions were calculated by divid- [(NH ) CO ] = 1.0  M, respectively. A flow sheet which 4 2 3 ing their desorption percentages. The results indicate illustrates the sorption and desorption processes of the that the maximum S-ratios are 56.0, 35.0 and 4.6 for Y/ investigated rare earth using D-50WX8 from 0.5  M Pr, Dy/Pr and were achieved with [(NH ) CO ] = 1.0 and HNO solution at v/m = 0.05 at 25 ± 1  °C is given in 4 2 3 [HNO ] = 5.0 M respectively, Table 3. Fig. 7. Finally, the reported results show that Dowex 50WX8 The desorption results indicate that Pr(III) can be sepa - resin is relatively selective, high efficient and cost effec - rated from Dy(III) and Y(III) as follows: tive for Pr(III), Dy(III) and Y(III) adsorption and is also easily regenerated rather than other reported adsorbent/ i. Stripping of Dy(III) and Y(III) using [(NH ) CO ] = 1.0 M 4 2 3 ion exchangers which were used in the adsorption from from Loaded Dowex 50WX8 after 2 cycles acidic nitrate medium. The reusability was carried out for ii. Dowex 50WX8 containing Pr(III) was then 4.0 adsorption stages with sorption capacity of 15.0, 30.0, stripped with 1.0 M citric acid at pH = 3 after two 35.0 mg/g for Pr, DY and Y, respectively, under the used stripping cycles experimental conditions. M asry et al. BMC Chemistry (2022) 16:37 Page 9 of 12 Table 2 Nonlinear Freundlich, Langmuir, Dubinin–Radushkevich, Temkin and Toth isotherm parameters for adsorption of metal ions onto Dowex 50WX8 Isotherm Parameters Metal ions DY(III) Pr(III) Y(III) Langmuir Qo (mg/g) 62.32 36.94 48.76 b (ml/mg) 0.0041 0.0074 0.0035 R 0.707 0.575 0.739 R 0.956 0.995 0.978 Chi^2 5.36 0.43 1.97 Freundlich K (mg/g) 0.632 1.044 0.491 1/n 0.719 0.569 0.694 R 0.944 0.971 0.959 Chi^2 6.765 2.604 3.597 Dubinin–Radushkevich q 245.38 116.96 142.26 2 2 β mol /kJ 0.0078 0.0064 0.0086 R 0.952 0.484 0.971 E 7.996 8.846 7.612 DR Chi^2 2.20 E-10 7.11E-11 3.23E-10 Tempkin Q , kJ/mol 280.66 351.33 328.04 K , mmol/g 0.0888 0.1017 0.0657 R 0.8989 0.9738 0.9119 Chi^2 12.3 2.34 7.77 Toth isotherm q , mg/g 23.19 25.02 49.11 Fig. 7 Flow sheet for the sorption and desorption processes of Pr, DY K 0.035 0.04 0.017 and Y using Dowex 50WX8 N 1.018 1.057 1.048 R 0.9668 0.987 0.991 x 1.504 1.19 1.688 Conclusions Dowex 50WX8 was successfully used for the recovery of Comparison study of REEs/Dowex 50WX8 with other DY(III), Pr(III) and Y(III) from acidic nitrate medium. reported materials The calculated maximum capacity of Dowex 50WX8 Comparison of REEs/Dowex 50WX8 system under the is 30, 50, 60  mg/g for Pr, DY and Y respectively at the used optimum conditions of batch technique with other optimum batch conditions; the maximum stripping of commercially reported materials [18, 32–51] and given Pr(III) is 58.0% and was achieved with 1.0 M citric acid at in Table 4, shows the advantages and efficiency of Dowex pH = 3. The results indicate that Pr(III) and Y(III) fitted 50WX8 adsorbent. The results of comparison in the with nonlinear Langmuir isotherm model with regres- term of maximum capacity (Q ) (30, 50, 60  mg/g for Pr, sion factors 0.995 and 0.978 respectively. The regenerated DY and Y), pH = 1, and contact time (15 min) and which Dowex 50WX8 gave sorption capacities of 15.0, 30.0, were achieved in the current study indicate that Dowex 35.0  mg/g for Pr, DY and Y, respectively under the used 50WX8 is more efficient and affordable than other experimental conditions. reported materials. Masry et al. BMC Chemistry (2022) 16:37 Page 10 of 12 Table 3 Desorption of metal ions (III) with different reagents after their adsorption with the Dowex 50WX8 resin at v/m = 0.05 at 25 ± 1 °C Stripping agent, M Dy(III) Pr(III) Y(III) S-ratio Dy/Pr Y/Pr Dy/Y HNO , 1.0 M 24.9 23.7 28 1.05 1.2 1 HNO , 5.0 M 55.4 12 43 4.6 3.6 1.2 HCl, 1.0 M – – 7.72 – – – H SO , 1.0 M 32.9 32.6 31 1 – 1.05 2 4 Na CO , 1.0 M 21 25.9 20 – – 1 2 3 (NH ) CO , 1.0 M 35 – 56 35 56 – 4 2 3 Citric acid (1.0 M) pH 1 – – – – – pH 3 40.12 58.37 39.25 – 1 pH 5 18.11 35.26 20.46 – – Table 4 Comparison study of REEs/Dowex 50WX8 with other reported materials Metal ion Adsorbent Q , mg/g pH Contact Time Refs Zeolitic imidazolate frameworks nanoparticles 430.4 7.0 7.0 h [1] Oxidized multi-walled carbon nanotubes 78.12 5.0 2.0 h [2] Silica/polyvinyl imidazole/H2PO4-core–shell NPs 150 4.0 0.5 h [3] Hybrid Lewis base ligands functionalized alumina-silica 125.4 4.0 3.0 h [4] polyethylenimine–acrylamide/SiO hybrid hydrogel 50–100 2-7 6.0 h [9] Microcapsules containing dibenzoylmethane 70.85 6.0 60.0 h [12] D113 resin 292.7 6.0 – [15] Macroporous poly(vinylphosphoramidic acid) resin 101 4-5 – [14] Zr-modified mesoporous silica supported H4[PMo VO ] 52.63 5.0 1.0 h [13] 11 40 Polyacrylic acid grafted silica fume 251.20 1-6 1.0 h [11] Pr(III) Lanthanide-ion imprinted polymers (L-IIPs) 125.3 6.0 1.5 h [5] Polyethylenimine sodium phosphonate resin (PEIPR.Na) 6.23 4.0 250 min [18] Fe O @TiO @P 0 nanoparticles 10.2 5.0 – [19] 3 4 2 2 4 TVEX–PHOR resin 49 3.5 1.0 h [20] magnetic nanoparticles functionalized with a phosphonic group 17.6 4.0 1.0 h [21] silica gel modified with diglycol amic acid 12.72 1.0 – [22] Graphene Oxide Nanosheets 135 6.0 2.0 h [6] Graphene oxide nanosheets with cross-linked by high-gluten flour 32.84 7.5 2.0 h [7] Y(III) Porous three-dimensional graphene oxide-corn zein composites 14.2 – 3.33 h [8] Carbon nanotubes reinforced silica composite 68.8 4.0 24.0 h [10] Functionalized silica in the hybridization process with chitosan 159 4.0 24.0 h [16] Diglycolamic-acid modified chitosan sponges 40.7 0.5–7 12.0 h [17] Funding Declaration Open access funding provided by The Science, Technology & Innovation Funding Authority (STDF) in cooperation with The Egyptian Knowledge Acknowledgements Bank (EKB). Science, Technology & Innovation Funding Authority (STDF) and Authors are thankful to the Egyptian Atomic Energy Authority for its continu- springer nature open access agreement. ous support for scientific research and development. Availability of data and materials Author contributions All data generated or analyzed during this study are included in this published BAM: Conceptualization, writing—original draft, data analysis. EMAE and SER: article [and its supplementary information files]. Methodology, resources, formal analysis, and data analysis. All authors read and approved the final manuscript. M asry et al. BMC Chemistry (2022) 16:37 Page 11 of 12 22. Marczenko Z. Spectrophotometric determination of elements; Ellis Declarations Harwood. Poland: Ltd; 1976. 23. 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Journal

BMC ChemistrySpringer Journals

Published: May 25, 2022

Keywords: Modeling; Dowex 50WX8; Adsorption; Rare earth metals

References