Adsorption of Au (III) from Aqueous Solution by Calcined Gibbsite

Jan 10, 2014 - Our findings show that the amount of Au(III) adsorbed onto the GBs is related to the specific surface area and the number of hydroxyl g...
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Adsorption of Au(III) from Aqueous Solution by Calcined Gibbsite Fumihiko Ogata and Naohito Kawasaki* Faculty of Pharmacy, Kinki University 3-4-1 Kowakae, Higashi-Osaka, Osaka 577-8502, Japan ABSTRACT: Gibbsite (GB) was prepared in this work by calcination between (200 and 1000) °C (GB200 and GB1000, respectively). Properties of the GBs prepared over this range of temperatures, such as their morphologies, crystallinities, specific surface areas, the number of hydroxyl groups, pore volumes, and mean pore diameters were investigated. The amount of Au(III) adsorbed onto the GBs was also evaluated. Our findings show that the amount of Au(III) adsorbed onto the GBs is related to the specific surface area and the number of hydroxyl groups. In this study, GB400, that is, GB calcined at 400 °C, had the largest specific surface area and number of hydroxyl groups, as well as the largest amount of adsorbed Au(III). Furthermore, the most suitable pH for the adsorption of Au(III) onto GB400 was approximately 6.0, and the gold chloro-hydroxy species [AuCl2(OH)2]− was selectively adsorbed at this temperature. The equilibrium for adsorption was reached within 24 h, and the experimental data were fit to the pseudo-second-order model. The adsorption isotherm data were better characterized by the Langmuir model than the Freundlich model. The presence of chloride ions (Cl−) affected the adsorption of Au(III) onto GB400. The increase of ΔG with temperature showed that the adsorption was endothermic and more favorable at higher temperatures. The positive ΔH values also indicated that Au(III) adsorption on GB400 was endothermic. The positive ΔS values suggest an increase in randomness at the solid−solution interface during the adsorption process. GB400 could be used for at least three Au(III) adsorption/desorption cycles. Collectively, these results suggest that GB400 would be useful for the adsorption of Au(III) from aqueous solutions.

1. INTRODUCTION Precious metals such as gold (Au), silver (Ag), platinum (Pt), and palladium (Pd) are indispensable to many high-technology industries because they serve as raw materials for catalysts, electronic components, and other parts.1 Because of their limited availability and relatively high value, recovery of these metals from aqueous and other types of waste solutions is economically attractive.2 Electronic and electrical waste (e-waste) causes harm to the environment and adversely affects the supply of vital raw materials. Recycling and reuse of materials, in particular, is crucial for preventing the practice of excessive mining and maintaining the overall supply of primary metals. In most cases, the waste generated from these products contains appreciable amounts of valuable metals like gold. In some cases, the content of gold in the discarded waste is much higher than that in the ore.3,4 Consequently, there is a significant need to develop precious metal recovery and reuse technologies from ewastes.5,6 The most widely studied method for precious metal recovery is extraction with various adsorbents such as natural zeolite,7 resin,8−10 molecular-imprinted biosorbent,11 chitosan resin modified with magnetic particles,12 and modified magnetic particles.13,14 Adsorptive recovery of precious metals has recently emerged as a potentially attractive and environmentally benign alternative to traditional reclaiming treatments.15 Compared to conventional methods, adsorption offers distinct advantages for metal ion recovery such as high efficiency, low operating cost, and minimal sludge volume.16 © 2014 American Chemical Society

Gibbsite (GB), one of the mineral forms of aluminum hydroxide, offers a number of advantages in precious metal recovery. It is recyclable, easily obtained from bauxite, inexpensive, and widely used in many fields. Moreover, it is capable of anion exchange in aqueous solutions. Aluminum compounds can be used in the recovery of Pt group metals.17,18 However, to the best of our knowledge, this is the first study to show that GB can be used for the adsorption of Au(III) in aqueous solution. Among GBs calcined between 200 °C and 1000 °C, we find that GB calcined at 400 °C (GB400) had the highest specific surface area and the largest number of hydroxyl groups.19 However, the mechanism by which Au(III) is adsorbed by GB400 has not been reported in detail. The present study aims to clarify the adsorption mechanism and establish the conditions for efficient adsorption of Au(III) by GB400.

2. MATERIALS AND METHODS 2.1. Preparation of Compounds and Measurements of Their Properties. Gibbsite (GB, H-42M: amorphous aluminum hydroxide) was purchased from Showa Denko, Japan. It was composed of moisture (0.23 %), Al(OH)3 (99.6 %), Fe2O3 (0.01 %), SiO2 (0.01 %), Na2O (0.03 %), and ωNa2O (0.05 %). The bulk density and moisture adsorption capacity were (0.2 to 0.5) g·cm−3 and 0.90 %, respectively. Received: October 7, 2013 Accepted: January 6, 2014 Published: January 10, 2014 412

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Chemical Co., Ltd.) was added at the following concentrations: (0.1, 0.5, 1.0, and 10.0) mmol·L−1. The concentration of Au(III) and Cl− was measured by an ICP-AES and an ion chromatograph, respectively. 2.6. Amount of Au(III) Adsorbed onto and Desorbed from GB400 with Sodium Hydroxide Solution. GB400 (0.5 g) was added to 300 mL of Au(III) solution at 30 mg·L−1 (pH = 5.2), and the suspension was shaken under the same conditions described in Section 2.2. The amount of Au(III) adsorbed was then calculated using eq 1. GB400 was collected after the adsorption step using a 0.45 μm membrane filter and then dried at room temperature. It (300 °C, and the existence of boehmite structure was confirmed at 400 °C. The structure of aluminum oxide changed from boehmite to γ, δ, and θ(transition state) aluminum oxides. GB1000 was stable α aluminum oxide that appeared upon calcination above 1000 °C.22 For GB400, the number of hydroxyl groups (0.46 mmol· g−1) and specific surface area (295.3 m2·g−1) was greater than those of the other GBs. However, the mean pore diameter, mesopores, and macropores were not related to the aluminum oxide structure. In general, based on their volume, pores are divided into micropores (5 Å < d ≤ 20 Å), mesopores (20 Å < d ≤ 500 Å), and macropores (d > 500 Å). Moreover, increasing the specific surface area decreases the mean pore diameter. This study also observed a similar trend: the specific surface area and micropore volume showed a positive correlation.17 Figure 1 shows the pH drift test for GB400. The pH of the zero charge, pHpzc, corresponds to that at which the curve crosses the straight line that fits the points pHinitial = pHfinal. The pHpzc of the GB400 was determined from this figure (7.1). Therefore its surface also has a neutral character. 3.2. Amount of Au(III) Adsorbed onto GBs. The amount of Au(III) adsorbed onto GBs is shown in Figure 2. GB400 showed the highest amount of Au(III) adsorbed compared to the other GBs. Overall, the amount of Au(III) adsorbed decreased with increasing calcination temperatures. The relationship between the amount of Au(III) adsorbed and the properties of the GBs is shown in Figure 3. The correlation coefficients between the amount adsorbed and the specific surface area and the hydroxyl group were 0.897 and 0.946, respectively. These results suggest that the adsorption mechanism of Au(III) using calcined GB is related to specific surface area and the number of hydroxyl groups. Moreover, the correlation coefficient between the amount adsorbed and the

(1) −1

where X is the amount adsorbed (mg·g ), C0 is the concentration before the adsorption (mg·L−1), Ce is the concentration after the adsorption (mg·L−1), V is the volume of the solvent (L), and M is the mass of the adsorbent (g). 2.3. Effect of Solution pH and Contact Time on the Adsorption of Au(III) onto GB400. The procedure described in Section 2.2 was followed with minor modifications. In this case, GB400 was added to the Au(III) solution at different pH, which was adjusted by hydrochloric acid and sodium hydroxide solution. Moreover, the time was varied from (0.5 to 24) h. 2.4. Adsorption Isotherm of Au(III) onto GB400. The procedure described in Section 2.2 was followed with minor modifications: the concentration of the Au(III) solution was varied from (0.5 to 20) mg·L−1 (pH = 5.2), and the temperature was varied from (5 to 45) °C. In addition, the concentration of Cl− was measured before and after adsorption. Cl− was measured by an ion chromatograph (Prominence HICNS, Shimadzu). The measurement was performed using the following: column: Shim-pack IC-A3 (Shimadzu); mobile phase: 8.0 mmol·L−1 p-hydroxyl benzoic acid, 3.2 mmol·L−1 bis-tris, and 50 mmol·L−1 boric acid (1:1:1); flow rate: 1.2 mL· min−1; temperature: 40 °C; detector: CDD-6A conductivity detector (Shimadzu); and sample volume: 50 μL. 2.5. Effect of Cl− on the Adsorption of Au(III) onto GB400. The procedure described in Section 2.2 was followed with minor modifications: Cl− (chlorine water; KISHIDA 413

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Figure 4. Amount of Au(III) adsorbed onto GB400 at different pH conditions. Initial concentration: 10 mg·L−1, sample volume: 50 mL, adsorbent: 0.02 g, temperature: 25 °C, contact time: 24 h, 100 rpm.

solution at approximately pH 6.0, indicating that the [AuCl2(OH)2]− species was most effective at the adsorption of Au(III) from aqueous solution.23−26 3.4. Effect of Contact Time for the Adsorption of Au(III) onto GB400. Figure 5 shows the effect of contact time

Figure 1. Determination of the pHpzc of GB400.

Figure 2. Amount of Au(III) adsorbed onto GBs. Initial concentration: 10 mg·L−1, sample volume: 50 mL, adsorbent: 0.02 g, temperature: 25 °C, solution pH: 5.2, contact time: 24 h, 100 rpm. Figure 5. Effect of contact time for Au(III) adsorption by GB400. Initial concentration: 10 mg·L−1, sample volume: 50 mL, adsorbent: 0.02 g, temperature: 25 °C, solution pH: 5.2, contact time: (0.5 to 48) h, 100 rpm.

on the adsorption capacity of Au(III) onto GB400 at 25 °C. Adsorption equilibrium of Au(III) onto GB400 was achieved within 24 h (amount adsorbed: 12.09 mg·g−1). The adsorption rates for Au(III) were analyzed in terms of the pseudo-firstorder, as well as the pseudo-second-order adsorption kinetic models (Figure 6). The Lagergren equations for the pseudofirst-order and the pseudo-second-order kinetic models are expressed by eqs 3 and 4, respectively.

Figure 3. Relationship between amount of Au(III) adsorbed and specific surface area or amount of hydroxyl group of GBs.

pore volumes was found to be: micropore: 0.672, mesopore 0.439, and macropore: 0.043 (data not shown). 3.3. Effect of Solution pH on the Adsorption of Au(III) onto GB400. It is well-established that solution pH has a significant effect on the adsorption process. Figure 4 shows that Au(III) adsorption reaches a maximum at a pH 6. The adsorption capacity of Au(III) is highest between pH values of 5 and 7. The [AuCl2(OH)2]− species was predominant in the

ln(qe − qt ) = ln qe − k1t

(3)

t /qt = 1/k 2qe 2 + t /qe

(4)

In these equations, qe and qt are the amount of Au(III) adsorbed (mg·g−1) at equilibrium and at time t, respectively, and k1 (h−1) and k2 (g·mg·h−1) are the pseudo-first-order and pseudo-second-order rate constants, respectively.26 The correlation coefficients and rate constants, k1 and k2, evaluated according to these two models are listed in Table 1. 414

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Figure 6. Pseudo-first/second-order kinetic plots for the adsorption of Au(III) onto GB400.

Table 1. Kinetic Parameters for Adsorption of Au(III) onto GB400 pseudo-first-order model

pseudo-second-order model

qe,exp

qe,cal

k1

qe,cal

k2

sample

mg·g−1

mg·g−1

h−1

R2

g·mg·h−1

g·mg·h−1

R2

Au(III)

12.09

6.40

0.13

0.903

12.20

0.03

0.994

tration of Cl− increased after Au(III) adsorption. The chlorine atom combines with Au(III) as a ligand. Subsequent exchanging of two Cl− with hydroxyl ions (OH−) from GB400 generates [AuCl2(OH)2]−. Therefore, there is an increase in the Cl− concentration after adsorption, which suggests that the adsorption mechanism of Au(III) onto GB400 occurred by a ligand substitution reaction. Moreover, the rate of this reaction increased with temperature. The adsorption equilibrium of Au(III) between aqueous solution and GB400 can be described by an adsorption isotherm. The Langmuir and Freundlich models were investigated, as described by eqs 5 and 6, respectively.

The values found by experiment (qe,exp) and calculated with the pseudo-second-order model (qe,cal) were the same. The correlation coefficients of the pseudo-first-order and pseudosecond-order models were 0.903 and 0.994, respectively. Moreover, the pseudo-second-order rate constant (k2) of Pt(IV), Pd(II), and Mo(VI) adsorption on GB400 was greater than that of Au(III) adsorption, which suggest that GB400 was suitable for adsorption of Au(III) compared to Pt(IV), Pd(II), and Mo(VI).27,17 Therefore, the data obtained in this study were characterized significantly better by the pseudo-secondorder model with respect to the pseudo-first-order model. 3.5. Adsorption Isotherm of Au(III) onto GB400. Adsorption isotherms for Au(III) onto GB400 at different temperatures are shown in Figure 7. The amount of Au(III) adsorbed increased with increasing temperature. The concen-

q = qmKLCe/(1 + KLCe)

(5)

log q = log KF + (1/n)log Ce

(6)

As known, the Langmuir equation is applicable to homogeneous adsorption, while the Freundlich equation describes heterogeneous systems. q and Ce are the adsorption capacity (mg·g−1) and the residual Au(III) concentration (mg·L−1) in solution at equilibrium, respectively. KL and qm are the Langmuir constant (L·mg−1) and maximum adsorption capacity (mg·g−1), respectively, and KF and n are Freundlich constants.28 By using the experimental data for the adsorption isotherms of Au(III) onto GB400 in eqs 5 and 6, the relevant Langmuir and Freundlich constants, respectively, were obtained (Table 2 and Figure 8). The correlation coefficient for the fit to the Langmuir and Freundlich equations was 0.931 to 0.983 and 0.807 to 0.841, respectively. The experimental data correlated well with the Langmuir equation. When 1/n > 2, adsorption is considered difficult.29 Our results indicate that Au(III) was easily adsorbed onto GB400 (1/n = 0.82 to 1.25). Moreover, the Langmuir constant (KL) of Au(III) adsorption on GB400 was greater than that of rhodium(III) adsorption.30 GB400 is a

Figure 7. Adsorption isotherms of Au(III) onto GB400 at different temperatures. Initial concentration: (0.5 to 20) mg·L−1, sample volume: 50 mL, adsorbent: 0.02 g, contact time: 24 h, temperature: (5 to 45) °C, solution pH: 5.2, 100 rpm; ●, 5 °C; □, 25 °C; ▲, 45 °C. 415

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Table 2. Freundlich and Langmuir Constants of Adsorption Isotherms of Au(III) onto GB400

Table 3. Thermodynamic Parameters for Adsorption of Au(III) onto GB400 ΔH

Langmuir constants qm

KL

°C

log KF

1/n

R2

mg·g−1

L·mg−1

R2

5 25 45

0.16 0.28 0.26

0.82 1.02 1.25

0.807 0.829 0.841

10.72 14.93 22.52

0.27 0.46 0.29

0.931 0.983 0.960

temperature

Freundlich constants

(8)

ΔG = −RT ln Kc

(9)

ln Kc = ΔS /R − ΔH /RT

sample

kJ·mol

Au(III)

2.56

−1

−1

J·mol ·K 12.08

278 K

298 K

318 K

−0.67

−1.31

−1.12

endothermic process, it is expected that increasing the solution temperature would result in an increased uptake of Au(III) from an aqueous solution. The positive values of ΔS suggest an increase in randomness at the solid−solution interface during the adsorption process.31 3.7. Effect of Cl− on the Adsorption of Au(III) onto GB400. Previous studies reported that the chemical form of Au(III) was affected by the concentration of chloride ion ([Cl−]);3,24,25 the [Cl−] affected the adsorption mechanism of Au(III) onto GB400. The effect of the [Cl−] for adsorption of Au(III) onto GB400 is shown in Figure 9. The amount

useful adsorbent for adsorption of Au(III) from aqueous solution. 3.6. Thermodynamic Analysis. From the kinetic adsorption experiments, thermodynamic parameters, such as ΔG, ΔH, and ΔS were obtained from the following equations:31

Kc = Cs/Ce

ΔG (kJ·mol−1) at temperatures

ΔS −1

(10) −3

−1

where R is the gas constant (8.314·10 kJ·mol·K ), Kc is the equilibrium constant, Cs is the number of milligrams of adsorbate in the adsorbent after adsorption equilibrium per liter of solution in contact with the adsorbent surface (mg·L−1), Ce is the equilibrium concentration in the solution (mg·L−1), and T is the absolute temperature (K). ΔG, ΔH, and ΔS are expressed in units of kJ·mol−1, kJ·mol−1, and J·mol−1·K−1, respectively. The values of the thermodynamic parameters studied are listed in Table 3. The negative value of ΔG at all studied temperatures for Au(III) adsorption on GB400 indicates that the adsorption process is spontaneous. The increase in ΔG with temperature shows that the adsorption is endothermic and more favorable at higher temperatures. The positive values of ΔH also indicate that Au(III) adsorption on GB400 is endothermic. This finding is consistent with the abovementioned case that shows the adsorption capacities of Au(III) increased with increasing temperature. Since diffusion is an

Figure 9. Effect of the chloride ion for the adsorption of Au(III) onto GB400. Initial concentration: 10 mg·L−1, sample volume: 50 mL, adsorbent: 0.02 g, contact time: 24 h, temperature: (5 to 45) °C, solution pH: 5.2, 100 rpm.

adsorbed decreased with increasing [Cl−] (correlation coefficient = 0.984). The solution pH after adsorption was 6.3 to 6.5, indicating that the [AuCl2(OH)2]− mainly exists in

Figure 8. Freundlich or Langmuir isotherms of GB400 for Au(III) at different temperatures: ●, 5 °C; ○, 25 °C; ◆, 45 °C. 416

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solution. Overall, the findings suggest that GB400 would be useful for the adsorption of Au(III) from aqueous solutions.

aqueous solution. The equilibrium relationship of Au(III) in solution with Cl− is described as follows: [AuCl4]− + nOH− ⇌ [AuCl4 − n(OH)n ]− + nCl

(11)

4. CONCLUSIONS Calcined GB was prepared at temperatures ranging from (200 to 1000) °C. The specific surface area and the number of hydroxyl groups on GB400 was the highest compared to other GBs prepared in the above-mentioned temperature range. GB400 had a boehmite structure. The correlation coefficient between the amount adsorbed and the specific surface area was 0.897 and that between the amount adsorbed and the number of hydroxyl groups was 0.946. The adsorption mechanism of Au(III) using calcined GB related to the specific surface area and the number of hydroxyl groups. The optimal pH for the adsorption of Au(III) onto GB400 was approximately 6.0, which indicated that the most suitable chemical form was [AuCl2(OH)2]−. Equilibrium adsorption was reached within 24 h and the data obtained in this study fit to the pseudo-secondorder model. The amount of Au(III) adsorbed increased with increasing temperature. The adsorption isotherm data was better fit to the Langmuir model (0.965 to 0.992) compared to the Freundlich model (0.898 to 0.918). Moreover, Cl− affected the adsorption of Au(III) from aqueous solution. The increase in ΔG with temperature showed that the adsorption was endothermic and more favorable at high temperature. The positive values of ΔH indicated that Au(III) adsorption onto GB400 was endothermic. The positive values of ΔS suggest an increase in randomness at the solid−solution interface during the adsorption process. GB400 could be used for at least three Au(III) adsorption/desorption cycles. These results suggest that GB400 would be useful for the adsorption of Au(III) from aqueous solution.

Increasing the chloride ion concentration shifted the equilibrium from [AuCl4−n(OH)n]− toward [AuCl4]−. Therefore, the amount adsorbed decreased with increasing Cl− concentration because the most suitable chemical form for the adsorption of Au(III), that is, [AuCl2(OH)2]−, was not available in solution. Moreover, increasing the [OH−] after adsorption also increased the pH in solution (pHfinal = 6.3 to 6.5; pHinitial = 5.2).23,31,32 3.8. Adsorption/Desorption Capability of Au(III) onto GB400. The amount of Au(III) adsorbed or desorbed using GB400 is shown in Figure 10, and the adsorption/desorption

Figure 10. Amount of Au(III) adsorbed or desorbed using GB400. Initial concentration: 30 mg·L−1, sample volume: 300 mL, contact time: 24 h, temperature: 25 °C, solution pH: 5.2, 100 rpm; ■, adsorption; □, desorption.

■

AUTHOR INFORMATION

Corresponding Author

*Tel.: +81-6-6730-5880 ext. 5556. Fax: +81-6-6721-2505. Email: [email protected].

Table 4. Adsorption/Desorption Percentage of Au(III) Using GB400 −1

1 mmol·L

NaOH

−1

10 mmol·L

Notes

The authors declare no competing financial interest.

■

NaOH

cycles (time)

adsorption percentage (%)

desorption percentage (%)

adsorption percentage (%)

desorption percentage (%)

1 2 3

59.0 24.6 36.9

40.3 80.1 74.5

55.4 33.4 34.7

54.9 103.0 73.7

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percentage of Au(III) using GB400 is shown in Table 4. We find that GB400 can be used for the adsorption/desorption of Au(III) at least three times. After the second use, the amount of Au(III) adsorbed/desorbed using 10.0 mmol·L−1 of NaOH was greater than the amount using 1.0 mmol·L−1 of NaOH, since the number of hydroxyl groups in GB400 was regenerated by the higher concentration of NaOH. Desorption percentage using 10.0 mmol·L−1 of NaOH ((54.9 to 103.0) %) was greater than that using 1.0 mmol·L−1 of NaOH ((40.3 to 80.1) %). These results suggested that the Au(III) amount remaining from previous step using 1.0 mmol·L−1 of NaOH was greater than that using 10.0 mmol·L−1 of NaOH. Therefore, regeneration of the number of hydroxyl groups in GB400 was easily occurred using 10.0 mmol·L−1 of NaOH. In this study, the number of hydroxyl groups present in GB400 was related to the adsorption mechanism of Au(III) from an aqueous 417

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dx.doi.org/10.1021/je400888r | J. Chem. Eng. Data 2014, 59, 412−418