Halloysite@polydopamine/ZIF-8 Nanocomposites for Efficient Removal of Heavy Metal Ions

Jiao, Linhong; Feng, Huixia; Chen, Nali

doi:https://doi.org/10.1155/2023/7182712

Journal of Chemistry

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Abstract Introduction Materials and Methods Results and Discussion Conclusions Data Availability Conflicts of Interest Acknowledgments References Copyright Related Articles

Research Article | Open Access

Volume 2023 | Article ID 7182712 | https://doi.org/10.1155/2023/7182712

Halloysite@polydopamine/ZIF-8 Nanocomposites for Efficient Removal of Heavy Metal Ions

Linhong Jiao,¹Huixia Feng,¹and Nali Chen¹

Academic Editor: Ahmad M. Mohammad

Received30 Mar 2023

Revised24 May 2023

Accepted27 May 2023

Published22 Jun 2023

Abstract

In this study, polymeric nanocomposites of zeolitic imidazolate frameworks (ZIFs) were synthesized by assembly of a biomimetic polymer-polydopamine (PDA)onto halloysite nanotubes (HNTs@PDA), followed by the in situ growth of zeolitic imidazolate framework-8 (ZIF-8) on the surface of HNTs@PDA. The obtained nanocomposites (HNTs@PDA/ZIF-8) prevented agglomeration of ZIFs and increased the number of active sites derived from PDA. The factors influencing heavy metal ions (Pb²⁺, Cd²⁺, Cu²⁺, and Ni²⁺) adsorption by HNTs@PDA/ZIF-8 were discussed. The Langmuir model was able to well describe the adsorption, and the maximum adsorption capacity of HNTs@PDA/ZIF-8 was calculated to be 285.00 mg/g for Cu²⁺, 515.00 mg/g for Pb²⁺, 185 mg/g for Cd²⁺ and 112.5 mg/g for Ni²⁺. Thermodynamic parameters confirmed that the adsorption was exothermic and spontaneous. Moreover, HNTs@PDA/ZIF-8 has good regenerability, which is very important in practical applications. The adsorption mechanism study showed that electrostatic attraction, coordination reactions and ion-exchange were the main mechanisms between the adsorbents and heavy metal ions. Hence, HNTs@PDA/ZIF-8 is a promising candidate for removing heavy metal ions from wastewater.

1. Introduction

The heavy metal ions in wastewater from industry are extremely toxic and readily cause metabolic disorders as well as other harmful effects. Heavy metal ions in water cannot be degraded, and enriched in organisms. Thus, human health is threatened [1–3]. New and efficient heavy metal removal techniques are urgently needed. To date, various methods have been used to remove heavy metal ions, including chemical precipitation, adsorption, ion-exchange, filtration, and coagulation. Among all mentioned methods, adsorption is one of the most widely applied technologies owing to its high removal efficiency, simplicity, and low cost [4]. Furthermore, a variety of adsorption materials are available for removing heavy metal ions. For example, metal-organic frameworks (MOFs) are nanomaterials that have useful features such as high surface area and porosity, adjustable pore size, easy surface functionalization, good thermal stability, as well as abundant active sites [5]. Therefore, they are widely applied in adsorption [6], storage [7], separation [8], catalysis [9], biosensing [10], as well as drug-loaded diagnosis and treatment [11]. As one of MOFs, zeolitic imidazolate framework-8 (ZIF-8) not only inherits the advantages of MOFs, but also overcomes the poor thermal and chemical stability [12] and exhibits substantial potential for environmental remediation [13]. However, MOFs are prone to disperse in water [14], making it difficult to separate and regenerate in water treatment. Therefore, it is necessary to design and develop suitable support materials to ensure efficient loading and avoid agglomeration of MOFs, by means of synergy between the MOFs and support material [15, 16].

Halloysite nanotubes (HNTs) possess high surface area and well porous structure and have a great potential applications for nanoscale supports or functionalized nanomaterials due to its low toxicity, widespread natural existence, lower price, and strong adsorption [17, 18]. Thus, HNTs can be used as suitable carriers for MOFs, which enable efficient loading and avoid agglomeration. To date, there are no reports on HNTs-loaded ZIF-8 for adsorption of heavy metal ions in water.

In this work, HNTs were first functionalized by polydopamine (PDA) then combined with ZIF-8 by the in situ growth method. Polydopamine (PDA) containing a large amount of catechol groups and amino groups which have good adsorption affinity for heavy metal ions is the main component of adhesion proteins secreted by marine mussels. The introduction of polydopamine (PDA) contributes to the continuous growth of ZIF-8 on HNTs. Then, the morphology and structure of nanocomposites were investigated by Scanning electron microscopy (SEM), Fourier-transformed infrared spectroscopy (FTIR), and X-ray powder diffraction (XRD). In addition, the adsorption performance and adsorption mechanisms of heavy metal ions (Cd(II), Cu(II), Pb(II), and Ni(II)) by nanocomposites were proposed and discussed.

2. Materials and Methods

2.1. Chemicals

All chemicals and reagents were commercially available in analytical grade and were used without further purification. Dopamine hydrochloride (AR, 99%), 2-methylimidazole (MIM; AR, 99%), and methanol (AR, 99%) were obtained from Sigma-Aldrich. HNTs (>99% purity) were purchased from Minchuangda Biotechnology Co., Ltd. Stock solutions of Pb(II), Cd(II), Cu(II), and Ni(II) (1000 mg/L each) were prepared by dissolving corresponding nitrates (AR, 99%, Sigma-Aldrich) into deionized water and were then diluted to 30–400 mg/L for batch experiments.

2.2. Synthesis of HNTs@PDA

HNTs (1.0 g) were added into 200 mL distilled water and sonicated for 30 min to form a suspension. Dopamine hydrochloride (0.7 g) was dissolved in Tris-HCl (50 mL, 0.01 M), then added into HNTs suspension and stirred for 12 h at 30°C, and the pH was adjusted to 8.5. The obtained product was separated from the black suspension by centrifugation at 10,000 rpm (21532 × ) and washed with distilled water and dried at 60°C under vacuum overnight.

2.3. In Situ Growth of ZIF-8 onto HNTs@PDA

HNTs@PDA/ZIF-8 was synthesized by a typical solvothermal method. HNTs@PDA (0.6 g) was first added into methanol. Zn(NO₃)₂∙6H₂O (8 mmol) was dissolved in methanol (30 mL). A certain quantity of HNTs@PDA was added into the abovementioned solution, followed by sonication (30 min) and agitation (30 min) to form a homogeneous dispersion, denoted as solution A. Next, 2 mmol MIM was dissolved in methanol (30 mL), denoted as solution B. The mixture containing solution A and B was transferred into a Teflon-lined stainless autoclave and maintained at 90°C for 6 h. The obtained black precipitate was washed with methanol and dried at 60°C for 8 h to collect the final product, denoted as HNTs@PDA/ZIF-8 (Figure 1).

2.4. Characterization

The surface functional groups were identified by Fourier transform infrared (FT-IR) spectrometer (Thermo Nicolet IS10) in the range of 400–4000 cm⁻¹. The morphology was observed by the scanning electron microscope (SEM; FEI QUANTA FEG 450). X-ray diffraction (XRD) patterns were recorded on a Bruker D8 Advance X-ray diffractometer with Cu Kα radiation from 5° to 85°. The chemical bonding states of the adsorbent were analyzed by X-ray photoelectron spectroscopy (XPS, ESCALAB250Xi).

2.4.1. Batch Adsorption Experiments

All batch adsorption experiments were carried out at a constant temperature (25°C) with a platform shaker (HZP-25-S, oscillation incubator) at 150 rpm. The adsorbent (0.01 g) was added into 50 mL solution of heavy metal ions, and then suspensions were shaken at 150 rpm. The collected solution was filtered through a 0.22 µm membrane and centrifuged at 10,000 rpm (21532 × ) for 10 min. The heavy metal ions concentration of supernatant was determined by inductively coupled plasma spectrometer (ICP/IRIS Advantage, Thermo). The effect of the solution pH on adsorption was determined within the range of 2.0–7.0 using HNO₃ and NaOH solutions.

Four cycles of desorption/adsorption experiments were conducted to try and predict the regeneration of adsorbent. After the adsorption of heavy metal ions, the adsorbent was collected and added into 50 ml 0.01 M EDTA-2Na solution as desorption agents and stirred for 3 h at 30°C. The regenerated adsorbent was used in the next cycle of adsorption-desorption experiment.

The adsorption capacity was calculated in accordance with the following equation:where q_e is the adsorption capacity (mg/g) at equilibrium, q_t is the adsorption capacity (mg/g) at time t, C₀ is the initial concentration (mg/L), C_e is the equilibrium concentration, C_t is the concentration (mg/L) at time t, V is the volume of the solution (L), and m is the adsorbent mass (mg).

3. Results and Discussion

3.1. Characterization

3.1.1. FTIR

FTIR spectroscopy of HNTs, HNTs@PDA, and HNTs@PDA/ZIF-8 are shown in Figure 2. The peaks at 3612 cm⁻¹ and 3693 cm⁻¹ could be ascribed to –OH stretching vibration inside the tube wall and the –OH stretching vibrations between the silicon-oxygen tetrahedron and the aluminum-oxygen tetrahedron, respectively [20]. The peak at 1640 cm⁻¹ was attributed to the bending vibration of –OH. The peaks at 1029, 909, 542, and 470 cm⁻¹ were attributed to bending vibrations of Si–O–Si, Al–OH, Al–O–Si, and Si–O–Si, respectively. The peak at 755 cm⁻¹ was due to the vertical stretching vibration of Si–O [21]. After modification by PDA, a new peak was evident at 1490 cm⁻¹, corresponding to the catechol O–H bending vibrations in PDA [22]. Accordingly, PDA was synthesized on the surface of the HNTs rod.

The contrast between FTIR spectra of ZIF-8 and HNTs@PDA/ZIF-8 showed that the peak at 2929.6 cm⁻¹ corresponded to the stretching vibrations of C–H [15]; the peaks at 3131 and 1581 cm⁻¹ corresponded to the stretching vibrations of C–N and C=N, respectively [23]. The peak at 1311 cm⁻¹ was due to the bending vibrations of the imidazole ring [24]. The peak at 1424.7 cm⁻¹ was attributed to the stretching vibrations of the imidazole ring [25]. In addition, the intensity of the peak at 424.53 cm⁻¹ which was attributed to the stretching vibrations of Zn-N decreased, indicated that the Zn atom was coordinated with the O atom in PDA [26]. Hence, The above analysis confirmed that HNTs@PDA/ZIF-8 was effectively synthesized.

3.1.2. SEM

Figure 3 manifests the SEM of HNTs, ZIF-8, HNTs@PDA/ZIF-8, and Cu-HNTs@PDA/ZIF-8. It could be seen that the tubular HNTs (Figure 3(b)) with typical slender rod-like structure (length: 0.5–1 µm) facilitated the growth of ZIF-8 [27]. The synthesized ZIF-8 crystals with an average size of 100–150 nm have grown on the surface of HNTs@PDA rod, formed a uniform and compact ZIF-8 layer, and prevented agglomeration of ZIF-8 (Figure 3(c)). Elemental mapping images of the adsorbent demonstrated the uniform distribution of Zn elements on the entire surface of the material (Figure 3(d)), which further confirmed that the uniform distribution of ZIF-8 nanoparticles.

3.1.3. XRD

The XRD patterns of HNTs, HNTs@PDA, and HNTs@PDA/ZIF-8 are shown in Figure 4. As can be seen from the figure, the diffraction peaks of HNTs at 9°, 20.1°, 26.7°, and 35.2° corresponded to (001), (020), (002), and (130) crystal planes [28]. After modification by PDA, characteristic peaks of HNTs are well maintained at similar positions, indicating that self-polymerization of dopamine did not destroy the HNTs structure. The characteristic peaks of HNTs@PDA/ZIF-8 at 7.22°, 10.24°, 12.64°, and 16.39° correspond to (011), (002), (112), and (013) crystal planes were in good agreement with that of ZIF-8 [29], which showed the successful growth of the ZIF-8 crystals on HNTs@PDA.

(a)

(b)

The peak intensity of HNTs@PDA/ZIF-8 was obviously decreased after the combination of HNTs@PDA and ZIF-8, because the amount of ZIF-8 and HNTs is significantly reduced [30].

After the adsorption of Cu²⁺(Figure 4(b)), characteristic diffraction peak positions of Cu-HNTs@PDA/ZIF-8 were in good agreement with that of ZIF-8, but the intensity of peaks decreased, indicating that the structure of partial ZIF-8 was destroyed. This is probably due to the ion-exchange effect.

3.2. Adsorption Performance

3.2.1. Effect of Initial pH on Adsorption

The pH of the solution is a substantial factor, because the pH of the solution not only affects the protonation of functional groups but also affects the chemical properties of adsorbent as well as the state of the heavy metal ions in the solution [31]. Thus, the effect of pH on the adsorption by HNTs@PDA/ZIF-8 was investigated in the pH range of 2.0–7.0 (Figure 5(a)).

(a)

(b)

The results shows that when the pH was 2.0–3.0, HNTs@PDA/ZIF-8 adsorbed few heavy metal ions, possibly because the amino functional groups in the HNTs@PDA/ZIF-8 were protonated under acidic conditions [32] and the ZIF-8 of HNTs@PDA/ZIF-8 under strong acidic conditions was unstable [33]. However, when the pH was in the range of 3.0–7.0, the uptake capacity of HNTs@PDA/ZIF-8 gradually increased. This might be because the degree of protonation of the amino group decreased in this pH range [34], and the stability of HNTs@PDA/ZIF-8 in this pH range was enhanced. This was in accordance with the literature [35].

As shown in Figure 5(b), the zeta potentials of HNTs@PDA and HNTs@PDA/ZIF-8 decreased with the increase of the pH value. The isoelectric point of HNTs@PDA is 4.5, while the isoelectric point of HNTs@PDA/ZIF-8 decreased to 2.69 after the in situ growth of ZIF-8, indicating that ZIF-8 loaded on the surface increased the negative charge, leading to increased electrostatic attraction force [36].

3.2.2. Adsorption Kinetics

The relationship between adsorption quantity of heavy metal ions and contact time is shown in Figure 6. The adsorption capacity increased rapidly at the beginning. The uptake of heavy metal ions by HNTs@PDA/ZIF-8 took 100−150 min to reach adsorption equilibrium. This rapid adsorption in the beginning was attributed to insufficient internal diffusion resistance and the availability of large adsorption sites.

To further study the adsorption behaviour and the potential rate-limiting steps, experimental data were fitted with pseudo-first-order (equation (2)) and pseudo-second-order (equation (3)) kinetic models [37].where k₁ and k₂ denote the pseudo-first-order (min⁻¹) and pseudo-second-order (g⋅mg⁻¹⋅min⁻¹) rate constants, respectively, and Q_e and Q_t denote the heavy metal adsorption capacity (mg/g) at equilibrium and time t (min), respectively.

The fitting curves are shown in Figure 7. The adsorption parameters are summarized in Table 1. It can be seen from Figure 7 and Table 1. The correlation coefficient of the pseudo-second-order kinetics model is higher than that of the pseudofirst-order kinetics model. The Q_ecal from the pseudo-second-order kinetics model matched well with the experimental data Q_eexp, indicating that the process of heavy metal adsorption by HNTs@PDA/ZIF-8 is more described by pseudo-second-order kinetics. Hence, the adsorption was dominated by chemical adsorption [38]. This is in agreement with the available literature [39].

(a)

(b)

3.2.3. Adsorption Isotherms

The effect of the initial concentration on the adsorption capacity is shown in Figure 8. As the concentration increased, the uptake capacity initially increased rapidly. As it can be seen, the uptake capacity of Pb²⁺ by HNTs@PDA/ZIF-8 was stronger than that of the others, possibly because of the charge densities of various heavy metal ions.

The adsorption isotherm describes the relationship between the adsorbate concentration on the surface of the adsorbent and the concentration in the solution. Langmuir isotherm and Freundlich isotherm models were taken into account to evaluate the adsorption behavior.

The fitting curves are shown in Figure 9. The adsorption parameters are summarized in Table 2. The equations are given bywhere k_l and k_f are the Langmuir (L/mg) and Freundlich constants, respectively; C_e denotes the heavy metal concentration (mg/L) in the solution at equilibrium; Q_e and Q_max denote the heavy metal adsorption capacity (mg/g) at equilibrium and the maximum heavy metal adsorption capacity (mg/g), respectively.

(a)

(b)

As it can be seen from Table 2, the correlation coefficients (R²) by the Langmuir model is greater than that of the Freundlich model, so the adsorption by HNTs@PDA/ZIF-8 is more consistent with the Langmuir isotherm.

The adsorption process followed a single-layer adsorption type [40].

According to Langmuir isotherm, the calculated maximum adsorption capacity was 301.20 mg/g for Cu²⁺, 515.46 mg/g for Pb²⁺, 187.62 mg/g for Cd²⁺, and 116.41 mg/g for Ni²⁺. The adsorption capacity of HNTs@PDA/ZIF-8 was greater than that of the other reported ZIFs-based adsorbents (Table 3).

3.2.4. Adsorption Thermodynamics

Figure 10 shows the effect of temperature on the adsorption of heavy metal ions by HNTs@PDA/ZIF-8. As can be seen from the figure, as temperature increased, the adsorption capacity gradually decreased. Thermodynamic parameters (including the equilibrium constant (K_d), enthalpy change (∆H), entropy change (∆S), and Gibbs free energy (∆G)) were calculated by equations (5)–(7) and listed in Table 4.

The negative value of G indicates the uptake of heavy metal ions by HNTs@PDA/ZIF-8, which is a spontaneous process. In addition, G decreased as the temperature increased, indicating that a low temperature facilitated the adsorption. In addition, the value of ∆H is negative, indicating that the adsorption is an exothermic process. The negative S value reveals that the randomness at the solid/liquid boundary decreased [47, 48].

3.2.5. Desorption and Reusability

To evaluate the reusability of the adsorbent, the recycling experiments were carried out on HNTs@PDA/ZIF-8. The results are shown in Figure 11. It can be seen that HNTs@PDA/ZIF-8 underwent loss of adsorption capacity after 4 cycles of adsorption-desorption. The decrease of adsorption capacity might be ascribed to structure destruction of partial ZIF-8 caused by ion-exchange. However, even after four adsorption-regeneration cycles, the adsorption capacity was still higher than 50 mg/g. Hence, the synthesized adsorbent possesses good regeneration properties for the removal of heavy metal ions from water.

4. Adsorption Mechanism

4.1. Ion-Exchange

As shown in Figure 12, Zn ions appeared in the solution after adsorption, indicating that partial Zn atom of HNTs@PDA/ZIF-8 exchanges with heavy metal ions in the solution. Although the ion-exchange greatly increased the uptake capacity of heavy metal ions by HNTs@PDA/ZIF-8, it reduced the regeneration performance of the adsorbent.

4.2. XPS

To gain further insight into the adsorption mechanism, the adsorbent before and after adsorption were investigated by XPS. After adsorption, new peaks assigned to Cu 2p, Cd 3d, Pb 4f, and Ni 2p were observed (Figure 13), which indicates that the heavy metals were adsorbed on HNTs@PDA/ZIF-8. In addition, after adsorption of Cu²⁺ and Ni²⁺, peaks at 933.35 and 953.29 eV corresponding to Cu–O were observed, and peaks at 857.05 and 875.22 eV corresponding to Ni–O were observed. This might be due to the fact that Cu and Ni atoms in the solution replaced the Zn atoms of ZIF-8 by ion-exchange and then interacted with the O atoms in PDA in a manner that formed chemical bonds [49].

(a)

(b)

(c)

(d)

Figure 14 and Table 5 show the high-resolution spectra of the N 1s peaks of HNTs@PDA/ZIF-8 before and after the adsorption. Before adsorption, the binding energies of N 1s peaks were 398.68 and 399.22 eV, respectively, corresponding to –NH₂ and –NH, respectively [50]. The main peak at 400.81 eV was attributed to the C–N bonds of MIM in the ZIF-8 of HNTs@PDA/ZIF-8 (Table 5).

(a)

(b)

(c)

(d)

(e)

After adsorption, the N 1s peaks of –NH₂ and –NH slightly shifted to lower values except for Cd²⁺, indicating that the heavy metal ions interacted with –NH₂ and –NH in the adsorbent. Notably, after adsorption of Cu²⁺ and Ni²⁺, new peaks at 406.77 and 407.27 eV were evident. This might be due to the fact that Cu²⁺ and Ni²⁺ interacted with the N atoms of MIM in the ZIF-8 of HNTs@PDA/ZIF-8 [33].

In summary of the results discussed above, HNTs@PDA/ZIF-8 mainly removed heavy metal ions via electrostatic attraction, coordination reactions, and ion-exchange.

5. Conclusions

A highly efficient adsorbent HNTs@PDA/ZIF-8 was synthesized by the in situ growth of ZIF-8 onto HNTs@PDA. The addition of PDA induced the in situ growth of ZIF-8 nanoparticles. Hence, ZIF-8 nanoparticles were uniformly distributed on the tubular HNTs@PDA.

The obtained HNTs@PDA/ZIF-8 showed a high uptake capacity and well recyclability. The uptake capacity of HNTs@PDA/ZIF-8 was calculated to be 285.00 mg/g, 515.00 mg/g, 185 mg/g, and 112.5 mg/g for Cu²⁺, Pb²⁺, Cd²⁺, and Ni²⁺, respectively. The adsorption isotherm model was in accordance with the Langmuir model. The pseudo-second-order kinetic model can well describe the adsorption process. The mechanism of adsorption showed that the adsorption process was dominated by electrostatic attraction, coordination reactions, and ion-exchange. Therefore, HNTs@PDA/ZIF-8 is a potential candidate for the uptake of heavy metal ions in wastewater.

Data Availability

The data from this study are availabe, could be accessible by contacting the corresponding author.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Acknowledgments

This study was financially supported by National Natural Science Foundation of China, Grant numbers (21664009 and 51063003).

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Copyright © 2023 Linhong Jiao et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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