稀有金属(英文版) 2018,37(08),707-715

Adsorption and desorption properties for rhenium using a kind of weak-base anion resin

Hong-Zhao Liu Bo Zhang Xiao-Jing Jing Wei Wang Li-Jun Wang

Rare Metal and Metallurgy Materials Research Institute,General Research Institute for Nonferrous Metals

Zhengzhou Institute of Multipurpose Utilization of Mineral Resources

Key Laboratory of Evaluation and Multipurpose Utilization of Polymetallic Ore of Ministry of Land and Resources

作者简介：*Li-Jun Wang e-mail:gold@grinm.com;

收稿日期：4 March 2018

基金：financially supported by the National Natural Science Foundation of China (Nos.51404220 and 51504225);

Adsorption and desorption properties for rhenium using a kind of weak-base anion resin

Hong-Zhao Liu Bo Zhang Xiao-Jing Jing Wei Wang Li-Jun Wang

Rare Metal and Metallurgy Materials Research Institute,General Research Institute for Nonferrous Metals

Zhengzhou Institute of Multipurpose Utilization of Mineral Resources

Key Laboratory of Evaluation and Multipurpose Utilization of Polymetallic Ore of Ministry of Land and Resources

Abstract：

In this paper,a weak-base resin was adopted to recycle rhenium because of its excellent adsorption and desorption properties for rhenium,while the kinetics and thermodynamics properties of adsorbing rhenium from the rhenium stock solution were systematically investigated.The kinetics investigations confirm that the adsorption process of Re belongs to kinetic control by particle diffusion process and the corresponding reaction rate constant is2.68×10^-3 s^-1.Then,the Langmuir and Freundlich models were used to describe the adsorption equilibrium behaviors of Re and the thermodynamics parameters are obtained.The results show that the Langmuir model is the best-fitted model,and the Gibbs free energy change of Re adsorption onto ZS15 weak-base resin is△G⁰ =-10.59 + 12.66 T.To verify the weak-base resins for extracting rhenium in industrial application,the column experiments were operated in the spray solution generating by roasting the molybdenum concentrates.The results indicate that the weak-base resins possess excellent adsorptive selectivity for rhenium.and the ammonia solution with low concentration could sufficiently desorb rhenium from the resins.

Keyword：

Rhenium; Weak base; Thermodynamics; Kinetics;

Received： 4 March 2018

1 Introduction

Rhenium (Re) is a kind of rare metal with the second highest melting point of 3180℃in periodic table.Owing to its excellent physicochemical properties,rhenium plays an irreplaceable role in the fields of high-temperature alloys and hydrogenation catalysts [ 1, 2, 3, 4, 5] .Since a low amount of independent rhenium ore deposits exists,most rhenium resource is distributed within the molybdenite ore in the form of ReS₂,consequently rhenium is often recovered as a by-product of molybdenum (Mo) smelting.During the roasting process of molybdenite concentrates,ReS₂ is oxidized to rhenium heptoxide (Re₂O₇) which is subsequently scrubbed with water as perrhenic acid(HReO₄) after being sublimated [ 6, 7, 8] .Therefore,the spray solution in the roasting process of molybdenite concentrates is an important raw material for rhenium recovery.

Since the Re concentration is rather low in the spray solution,whereas the content of other impurity ions such as molybdate radical,sulfate radical and sulfite radical is considerably high,the beneficiation of Re is required primarily,and the separation of Re from other impurity ions must be conducted simultaneously.Up to now,the solvent extraction and the ion exchange technologies are mainly used to recover rhenium from the spay solution in industrial application [ 9, 10] .In Jiangxi Copper Corporation,the largest manufacturer for rhenium products in China,the N235-octanol-kerosene extraction system is adopted for Re recovery and the qualified ammonium perrhenate is obtained as the final product [ 11] .However,there still exist certain technical problems for the extraction method of Re recovery.Since Mo exhibits similar chemical properties with Re,it is difficult to thoroughly separate Mo from Re by extraction process [ 12, 13, 14] .Another problem is the emulsion of the system during extraction,resulting in the loss of the extracting agent and the reduction in yield [ 15] .In addition,the poisonous effect of the residual extracting agent in the raffinate could induce certain difficulties for the water treatment.

Compared with the extraction method,the ion exchange method does not pollute the environment and the operation process is convenient for Re recovery.At present,although the strong-base anion exchange resin is commonly utilized due to its excellent adsorption selectivity for rhenium [ 16, 17] ,the desorption agents of these exchangers can be accomplished with high concentration of ammonium thiocyanate or perchloric acid,which are high cost and poisonous [ 18, 19, 20] .In addition,the strong-base resin is difficult to regeneration,resulting in poor recycling performance.In contrast,the weak-base resin requires only lower concentration of ammonium hydroxide to achieve a better effect of desorption [ 21, 22, 23, 24] .However,there are neither detailed researches on weak-base resins in Re recovery,nor industrialized application.

In this paper,a weak-base anion exchange resin was adopted to recover rhenium from the rhenium stock solution and the basic adsorption parameters were optimized for recovering rhenium in roasting process of molybdenite concentrates.Firstly,different anion exchange resins were applied to investigate the adsorption/desorption properties of rhenium and a suitable weak-basic resin was selected.Then,the kinetics and thermodynamic properties of the Re adsorption process were systematically studied,and the corresponding parameters were obtained.Finally,the column experiments on adsorption and desorption properties of rhenium in spray solution system were carried out.This research laid a foundation for the industrialized application.

2 Experimental

2.1 Materials

The batch experiments were conducted in rhenium stock solutions which were prepared by dissolving NH₄ReO₄(99.99%) in distilled water.All reagents were analytical grade and were used without further purification.The column experiments were carried out in spray solutions which were obtained by leaching the molybdenum concentrate roasting gas from a molybdenum smelter in China.The results of the chemical analysis for the spray solution are shown in Table 1.To remove the alkaline and the acidic impurities,all resins were purified by 5%sodium hydroxide solutions and 5%hydrochloric acid solutions,respectively.After the pretreatment process,these resins were washed with distilled water until nearly neutral pH and dried for 24 h at 333 K,which were used for the following experiments.

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Table 1 Main chemical compositions of spray solution (mg·L^-1)

2.2 Analysis

The chemical composition of the rhenium stock solution,the spray solution,the effluent and the eluant solution were measured by inductively coupled plasma-atomic emission spectroscopy (ICP-AES,IntrepidⅡXSP,Thermo Electron,USA),while the pH of the solution was measured by S210(Mettler Toledo,Switzerland) pH meter.The morphology of the resins was observed by electron probe microanalyzer(EPMA-1720,Shimadzu,Japan),and the Fourier transform infrared spectra (FTIR) were recorded on a Nicolet 5700(Thermo Electron,USA) FTIR spectrophotometer.

2.3 Batch adsorption studies

A predetermined volume of the rhenium stock solution was charged to a conical flask and heated to a desired temperature while being magnetically stirred at a specific stirring rate.Then,a measured amount of pretreatment rein was added to the flask and the reaction time was initiated.All equilibrium adsorption experiments were inpidually conducted for 24 h at ambient temperature (except for the temperature experiments).After the required time,the resins were separated from the effluent solution by vacuum filtration and washed with distilled water.The amount of Re adsorbed per unit mass on the resins was calculated by the following mass balance equation.

where Q_e is the equilibrium adsorption capacity of rhenium(mg·g^-1),C₀ is the initial concentration of rhenium measured in rhenium stock solution (mg·L^-1),C_e is the equilibrium concentration of rhenium measured in effluent(mg·L^-1),V is the volume of rhenium solution (L) and W is the amount of resins (g).

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Table 2 Characteristics of various resins

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Table 3 Equilibrium adsorption capacity of various resins for rhenium

Fig.1 Desorption curves of different resins

2.3.1 Resins selection

In adsorption process,five different resins,each of which was 2 ml,were added into 500 ml rhenium stock solution with 200 mg·L^-1 rhenium concentration.In desorption process,100 ml ammonia solution with concentration of5%was used to desorb the saturated resins and the reaction time was 60 min.

2.3.2 Kinetics properties

Kinetics experiments were conducted to determine the equilibrium time taken by 2 ml resin with 400 ml Re solution (400 mg·L^-1).1 ml effluent solution sample was collected at certain time intervals to measure the rhenium concentration.

2.3.3 Adsorption isotherms

The investigations of the adsorption isotherms for rhenium were carried out by adding 1 ml resin in 500 ml rhenium stock solution at varying concentrations of 80,240,400,560 and 720 mg·L^-1 under 293,313 and 333 K,respectively.

2.3.4 Thermodynamic properties

The effect of the temperature on rhenium adsorption was conducted by putting 2 ml resin in 500 ml Re stock solution (200 mg·L^-1) at varying temperatures of 288,303,318 and 333 K.

2.4 Column experiments

To verify the effect of the weak-base resin for extracting rhenium in industrial application,column experiments packing with 10 ml resins were carried out in the spray solution system.The spray solution was fed at a constant flow rate of 3 bed volumes per hour (BVs·h^-1) through the column using a peristaltic pump.To elute the adsorbed metal ions,the ammonia solution with concentration of 5%was fed to the column at the flow rate of 1 BVs·h^-1.

3 Results and discussion

3.1 Resins selection

Up to now,various anion exchange resins were used to extract rhenium from the rhenium stock solution,some of which were applied in industrial application such as201×7.In order to evaluate the adsorption properties of Re for various resins,the characteristics and the equilibrium adsorption capacity of different anion exchange resins are shown in Tables 2 and 3.It can be seen that D201(113.53 mg·g^-1),ZS15 (124.49 mg·g-1) and ZS25(115.81 mg·g^-1) resins exhibit favorable adsorption properties for rhenium.

Furthermore,the desorption process of the three resins was investigated and the desorption curves are shown in Fig.1.It is found that the rhenium concentration is rather low in the eluant solution and almost keeps constant in the desorption process for D201 resins,indicating that the ammonia solution could hardly desorb from D201resins.Because of the strong affinity between and the functional group of strong-base resins,ammonium thiocyanate and perchloric acid were often used as the eluting agent.For ZS15 resins,the desorption process achieved equilibrium in 20 min and the equilibrium concentration for rhenium was 950 mg·L^-1,demonstrating that the ammonia solution with concentration of 5%could sufficiently desorb rhenium from ZS15 resins.In conclusion,the ZS15 resin was adopted as the research object and used for the following experiments.

To explain the mechanism of adsorption and desorption,FTIR spectra of ZS15 resins in the range of400-4000 cm^-1 are shown in Fig.2.The wide adsorption band at 850-1150 cm^-1 of bare resins is typical for or ,which verifies that the bare resins are in the form.In addition,the narrow strong adsorption bands at 1030-1070 cm^-1 of (NH₄)2MoO₄ saturation resins and 870-930 cm^-1 of NH₄ReO₄ saturation resins are characteristic for and ,respectively,which indicates that the molybdate ions and perrhenate ions could observably adsorb on the resins.Compared with the bare resins,the desorption resins exhibit similar curves,which is in accordance with the desorption curves of ZS15 resins.The adsorption reaction of perrhenate ions is depicted in Reaction (2),as well as the desorption reaction depicted in Reaction (3).

where NR₂ represents the polymer resin matrix and the functional group.

3.2 Kinetics properties

The kinetics studies on the adsorption of inpidual element are necessary for determining the rate controlling mechanisms and to predict the time taken by the resin to reach equilibrium.The concentration profiles of Re during adsorption process are shown in Fig.3.It can be seen that Re concentration sharply decreases from 400.00 to84.87 mg·L^-1 at initial 180 min and it tends to approach a constant value after 480 min.As a result,Re adsorption process is considered to reach the equilibrium state in 24 h.

Re in the pregnant solution is adsorbed onto the weakbase anion resin as the perrhenate anion .The adsorption process of is normally controlled by three diffusive transport processes:(1) diffuse to the surface of the resin through the liquid film of the solution;(2) diffuse from the surface of the resin to the interior sites of the resin;(3) the ion exchange reaction of occurs onto the active sites in the resin [ 25] .Therefore,the adsorption process of Re is affected by the three steps of film diffusion,particle diffusion and chemical reaction,while one of the steps with the slowest reaction rate is the limiting step.The moving boundary model was used to describe the controlling mechanisms of the adsorption process,and the linear equations can be expressed as:

Fig.2 FTIR spectra of bare resins,desorption resins,saturation resins of ammonium molybdate and saturation resins of ammonium perrhenate

Fig.3 Concentration profiles of rhenium during adsorption

Film diffusion:

Particle diffusion:

Chemical reaction:

where F is the adsorptivity;Q_t is the adsorption capacity at certain time (mg·g^-1);t is the reaction time (min);k is the reaction rate constant (s^-1).Evidence on the rate controlling process is sought by examining the correlation coefficient (R).It can be seen from Fig.4 that the particle diffusion curve shows the best linear relation in terms of correlation coefficient (R²) of 0.9869.Hence,the diffusion process of the in the resin is the limiting step of the adsorption process for Re,and the corresponding rate constant obtained from the fitted curve slope of the particle diffusion is 2.68×10^-3 s^-1.

3.3 Adsorption isotherms

Although the thermodynamics properties of recovering rhenium have been investigated,there is a lack of comprehensive information on the weak-base resin system.The adsorption isotherms are important for the description of the degree of the adsorption process onto the resin surface at different temperatures [ 26] .In this study,Langmuir and Freundlich models were used to fit the experimental data through nonlinear regression techniques to check for their adequacy [ 27] .

The adsorption isotherms of Re are presented in Fig.5.It is obvious that the equilibrium adsorption capacity of Re decreases with temperature increasing,whereas it increases with the initial Re concentration increasing.The Langmuir model is based on the following assumptions:(1) the adsorption process is a uniform adsorption of the surface monolayer;(2) the binding sites of ion adsorption are equivalent;(3) an interaction force between the homogeneous molecules adsorbed on the surface of resin does not exist;(4) the adsorption equilibrium is dynamic and the interaction effect among the substances adsorbed on the surface does not exist.The Langmuir model can be expressed as:

Fig.4 Determination of limiting step for adsorption process of Re

Fig.5 Adsorption isotherms of rhenium

where Q_max is the maximum adsorption capacity (mg·g^-1),and K_L is the Langmuir constant (L·mg^-1).

The linear fitting curves of C_e versus Q_e are shown in Fig.6,and the fitting parameters are listed in Table 4.It could be observed that all the determination coefficients(R²) are larger than 0.99,indicating that the Langmuir model exhibits excellent fitting degree.Additionally,the maximum adsorption capacity (Q_max) decreases from416.67 to 361.01 mg·g^-1 with the temperature increasing from 293 to 333 K.

The Freundlich equation is an empirical adsorption model whereby it is based on the hypothesis that the adsorption energy of a metal binding to a site on an adsorbent depends on whether the adjacent sites are already occupied [ 28] .Nevertheless,this model could not clearly illustrate the relationship between the amount of the solute in the solution and the adsorbing capacity of the solute on the adsorbent.The Freundlich model can be expressed as:

Fig.6 Fitting curves of Langmuir model

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Table 4 Fitting parameters of Langmuir model

In Eq.(9),both n and K_F are the model parameters,in which K_F represents the adsorption ability of the resin and n represents the difficulty degree of the adsorption reaction.The plots of lgC_e versus lgQ_e were drawn and the fitting curves are shown in Fig.7,while the fitting parameters are listed in Table 5.In the Freundlich model,the value range of n from 1 to 10 indicates that the Re adsorption process is easily implemented.It could be observed from Table 5 that the value of n is from 3 to 4,demonstrating that the adsorption processes of Re on the resin are easily conducted under various temperatures.In addition,the value of K_F decreased from 78.48 to 56.69 with temperature increasing from 293 to 333 K,which indicates that lower temperature is significantly beneficial for the Re adsorption process.

The criterion that judges the fitting result between Langmuir model and Freundlich model is the determination coefficient obtained from the fitted curves.Based on the abovementioned experimental parameters,it could be concluded that the Langmuir model is a better fitted model for the adsorption equilibrium relationship of Re on the resin.This fact may be due to the homogenous distribution of active sites on the resin,since the Langmuir model assumes that the surface of the adsorbent is homogenous.

Fig.7 Fitting curves of Freundlich model

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Table 5 Fitting parameters of Freundlich model

Fig.8 Effect of temperature on equilibrium adsorption capacity

3.4 Thermodynamic properties

The temperature has substantial effect on rhenium adsorption degree of the resins,and the summarized results are shown in Fig.8.It can be seen that the equilibrium adsorption capacity decreases from 118.38 to113.31 mg·g^-1 with temperature increasing from 288 to333 K.The effect of the temperature on the adsorption behavior is determined by the thermodynamic properties of Re adsorption,and the thermodynamic parameters such as Gibbs free energy change (ΔG⁰),enthalpy change (ΔH⁰)and entropy change (ΔS⁰) for the adsorption system can be calculated using the following equations [ 28] :

where R is the gas constant (8.314 J·mol^-1·K^-1),T is the absolute temperature (K),K_ad is adsorption equilibrium constant and C_a is the concentration of rhenium on the adsorbent at the equilibrium (mg·L^-1).The curve between lnK_ad and 1/T is drawn in Fig.9,in which the fitted straight slope representsΔH⁰/R and the intercept isΔS⁰/R.The calculated thermodynamic parameters are shown in Table 6.It could be observed that the value ofΔG⁰increases from-6.903 to-6.289 kJ·mol^-1 with temperature increasing from 288 to 333 K,indicating that the adsorption reaction of Re on the resin is a spontaneous process.Moreover,the variation of the Gibbs free energy verifies that the degree of the spontaneous reaction for Re adsorption is much stronger at lower temperature.

Fig.9 Fitting curve of adsorption process for rhenium

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Table 6 Thermodynamic parameters of adsorption process for rhenium

The value ofΔH⁰ obtained from the fitting curve is-10.59 kJ·mol^-1,demonstrating that the adsorption process of Re is an exothermic reaction [ 29] .Hence,the lower temperature is beneficial for the adsorption process,which is in accordance with the variation of the equilibrium adsorption capacity under various temperatures.The value ofΔS⁰ obtained from the intercept of the fitted curve is-12.66 J·mol^-1·K^-1,indicating that the chaos decreases in the adsorption process.This phenomenon is attributed to the fact that the perrhenate ions transform from the unordered free state to the ordered adsorbed state on the active sites of the resin in adsorption process [ 30] .

3.5 Column experiments

To verify the effect of the weak-base resins for recycling rhenium in industrial application,the column experiments in the spray solution system were conducted.The saturation ratio (C/C₀) was used to evaluate the adsorption ability of the resins,and 10%is defined as the breakthrough point.The adsorption behavior of Re and Mo in the spray solution along with other impurity ions such as S,F,Si,Se is shown in Fig.10.It is clear that the saturation ratio of Re is less than 1%when the volume of the spray solution is less than 100 BVs and the breakthrough of Re takes place after 170 BVs.Meanwhile,the saturation ratio of Mo rapidly increases and achieves100%at 40 BVs.As rhenium and molybdenum elements exist similar characteristics,the resins possess excellent adsorption selectivity of rhenium.

Fig.10 Adsorption curves of Re and Mo in spray solution

Fig.11 Desorption curves of Re and Mo in spray solution

The desorption curve for Re shown in Fig.11 reveals that the Re concentration is rather low in the initial stage and rapidly increases after 0.92 BVs.The peak value of Re concentration is 18664 mg·L^-1 which appears at 1.65 BVs of stripping.Then,the Re concentration sharply decreases to 165 mg·L^-1 at 3.80 BVs.It is evident that the desorption process of Re centralizes in the range of 0.92-3.80 BVs,which proves that the desorption process of Re possesses fast kinetics properties.On the contrary,it could be observed that the Mo concentration in the eluant solution increases to the maximum value of 2074 mg·L^-1 at 1.37BVs and then rapidly decreases to 224 mg·L^-1 at 2.58BVs.Compared to Re concentration,Mo concentration in the desorption solution is obviously smaller,which is in accordance with the adsorption curve of Mo.

Fig.12 EPMA images of resins:a loaded resins,b desorption resins,c scanning Mo of loaded resins,d scanning Mo of desorption resins,e scanning Re of loaded resins and f scanning Re of desorption resins

EPMA images of loaded resins and desorption resins are shown in Fig.12.It can be seen that large amounts of rhenium and molybdenum are adsorbed on the loaded resins and display uniform distribution.For desorption resins,it can be clearly observed that rhenium almost totally disappears on the resins,demonstrating that the loaded rhenium could be completely desorbed by the ammonia solution with low concentration.Meanwhile,only very little molybdenum exists on the resins,which could not affect the adsorption and desorption properties for rhenium.The column experiments confirm the fact that the weak-base resins could effectively recycle rhenium from actual spray solution in the roasting process of molybdenum concentrates.

4 Conclusion

The adsorption and desorption properties of four different resins were investigated for ,and the weak-base resin ZS15 shows the best performance.The kinetics studies confirm that the adsorption process of Re is controlled by particle diffusion process,and the corresponding reaction rate constant is evaluated as 2.68×10^-3 s^-1.The Langmuir model fits the adsorption isotherms for Re very well with a determination coefficient (R²) of 0.99,which is due to the homogenous distribution of active sites on the resin.At normal temperature,the values of the Gibbs free energy change and the enthalpy change are all negative,representing that the adsorption process of Re is a spontaneous and exothermic process.The value of entropy change of-12.66 J·mol^-1·K^-1 indicates the reduction in disorder in the adsorption process.In column experiments,the breakthrough of rhenium took place after 170 BVs,whereas the molybdenum concentration achieves saturation at 40 BVs.Meanwhile,the loaded resins are effectively eluted using ammonia solution concentration of 5%.

Acknowledgements This study was financially supported by the National Natural Science Foundation of China (Nos.51404220 and51504225).

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