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Effect of SiO2 aerogels loading on photocatalytic degradation of nitrobenzene using composites with tetrapod-like ZnO

  • Zhigang Yi EMAIL logo , Tao Jiang , Ying Cheng and Qiong Tang EMAIL logo
Published/Copyright: October 23, 2020
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Nanotechnology Reviews
From the journal Nanotechnology Reviews Volume 9 Issue 1

Abstract

To study the effect of improved adsorption property of tetrapod-like ZnO (T-ZnO) on its photocatalytic performance, a new composite was prepared by loading silica aerogels (SiO2(AG)) on the surface of T-ZnO via the sol–gel method. Various characterization methods showed that SiO2(AG) was uniformly loaded on the surface of T-ZnO, and the morphology as well as structural characteristics of SiO2(AG) and T-ZnO were not changed. Nitrobenzene (NB) was selected as the model pollutant, and the adsorption and photocatalytic properties of T-ZnO and SiO2(AG)/T-ZnO for NB were studied. The photocatalytic degradation processes of NB using T-ZnO and SiO2(AG)/T-ZnO followed the first-order reaction. Considering the initial moment reaction kinetic, the photocatalytic kinetic of SiO2(AG)/T-ZnO and T-ZnO was consistent with the Langmuir–Hinshelwood kinetic model, and reaction rate constant k SiO 2 AG / T-ZnO ′ > k T-ZnO ′ , adsorption rate constant K ad SiO 2 ( AG ) / T-ZnO > K ad T-ZnO, which demonstrated that SiO2(AG) loading could increase T-ZnO adsorption to NB, then promoted its photocatalytic performance.

Keywords: silica aerogels; tetrapod-like zinc oxide; adsorption property; photocatalytic performance; nitrobenzene

1 Introduction

In recent years, large varieties of nanomaterials have become research hotspots in the fields of medicine [1,2,3,4], architecture [5,6,7], energy storage [8,9], and environmental protection [10,11,12,13,14] due to their many special properties such as good chemical stability, microwave absorption, high surface activity, and strong oxidation. Nanomaterials have been investigated in-depth for environmental pollutant treatment [15,16,17,18,19] because of the environmental problems caused by the discharge of persistent organic pollutants with rapid development of industry [20,21,22,23].

In the past few decades, more and more attention has been paid to nanomaterial photocatalytic technology, which uses natural/UV light as energy and semiconductor nanomaterials as photocatalysts to degrade organic contaminates via the photocatalytic process on the surface of nanomaterials [24,25,26]. Among the semiconductors employed, although TiO2 is generally regarded as the best photocatalyst, ZnO has frequently exhibited similar or higher photocatalytic activity compared to TiO2 [27,28,29,30,31,32]. In addition, ZnO has the advantages of low cost and easy preparation [33]. All of these make ZnO an ideal substitute for TiO2. Previous studies of our research group have found that the microsized tetrapod-like zinc oxide (T-ZnO) had better photocatalytic activity and dispersion than nanosized ZnO with other different morphologies, and was easier to separate from water for reusage [20]. Among different factors affecting the efficiency of photocatalytic degradation of organic matter, the adsorption behaviors of the contaminants onto the surface of photocatalyst were typically considered to play significant roles [34,35,36]. Plenty of studies have shown that adsorption behaviors were necessary for successful photocatalytic decomposition of organic compounds [37,38]. Thus, improving adsorption property of T-ZnO on the basis of keeping its morphology has been a major consideration to further improve the photocatalytic performance of T-ZnO.

In recent years, porous materials such as activated carbon, zeolites, and SiO2 were actively investigated as advanced sorbents [39]. Many of these porous materials have been used as support materials; loading of TiO2, ZnO, and other semiconductors in the porous materials has improved their adsorption and photocatalytic activity [40,41,42]. One of the promising porous materials, SiO2 aerogels (SiO2(AG)), is a three-dimensional and multiscaled porous nanomaterial formed by numerous fine particles and networks. The SiO2(AG) materials possess excellent adsorption efficiency owing to high porosity, high specific surface area (SSA), low density, etc. [39,43,44].

To study the effect of improved adsorption property of T-ZnO on its photocatalytic performance, we prepared SiO2(AG)/T-ZnO composites via the sol–gel method, and nitrobenzene (NB) was selected as the model pollutant. The absorption and photocatalytic properties of T-ZnO and SiO2(AG)/T-ZnO for NB were comparatively studied. The Langmuir–Hinshelwood kinetic model was used to calculate the photodegradation kinetic parameter.

2 Experimental

2.1 Reagents and materials

T-ZnO, received from Key Laboratory of Advanced technologies of Materials (Ministry of Education), Southwest Jiaotong University, was prepared by the gas-expanding method using metallic zinc as the raw material [45]. Tetraethyl orthosilicate, anhydrous ethanol (EtOH), trimethylchlorosilane, hexane, HCl, NH3·H2O, and NB were commercially purchased. All reagents were of analytical-grade quality and used without further purification. Deionized water was used in all experiments.

2.2 Preparation of SiO2(AG)/T-ZnO

The SiO2(AG) was synthesized by the solvent-exchanging procedure under ambient pressure as described in our earlier report [20]. The SiO2(AG) powders were dispersed with hexane under ultrasonic assistance to form a fluid sol dispersion [46]. The designated amounts of T-ZnO were mixed into the sol, and after stirring at 60°C for 2 h, the SiO2 gel was deposited onto the surface of T-ZnO. SiO2(AG)/T-ZnO composites were obtained after washing with EtOH and drying at 60°C for 24 h.

2.3 Material characterization

The FESEM (Inspect F; FEI, Holland, the Netherlands) and FETEM (JEM-2100F; JEOL, Japan) were used to investigate the microtopography of fabricated materials. The crystal structure of the materials was analyzed by X-ray diffraction (XRD DX-2500) with Cu Kα-ray generator (40 kV, 40 mA, λ = 0.15406 nm). The pore structure and the SSA of the prepared materials were determined by the automatic porosity and surface area analyzer (3H-2000PS4; Beishide Instrument Technology Co., Ltd, Beijing, China), respectively, and the detecting conditions of analyzer were as follows: nitrogen as adsorbate, degassing mode of heating vacuum, degassing temperature of 150°C, degassing time of 180 min, saturated steam pressure of 1.0434 bar, and ambient temperature of 14.0°C. UV-VIS diffuse reflectance spectra (UV-VIS DRS) were measured using a TU-1901 spectrophotometer (Purkinje General).

2.4 Research of adsorption performance

Isothermal adsorption experiments were conducted in NB solution with different concentrations (12, 24, 36, 48, and 60 mg/L). The dosage of adsorbent (T-ZnO and SiO2(AG)/T-ZnO) was 2.0 g/L. NB solution of different concentrations (100 mL) was placed in a 250 mL conical flask and shaken at 220 rpm for 24 h under 25°C. The adsorption amount of NB on adsorbent was reflected by measuring the change of concentration of NB in solution via the UV-VIS spectrophotometer (UV-2550; Shimadzu, Japan), which was calculated by:

(1) q = ( C 0 − C e ) × v w ,

where q is the adsorption amount of NB on adsorbent, mg/g; C 0 is the initial concentration of NB in solution, mg/L; C e is the equilibrium adsorption concentration of NB in solution after adsorption equilibrium, mg/L; v is the volume of solution, L; and w is the dosage of adsorbent, g.

2.5 Photocatalytic performance

NB solution with different concentrations (12, 24, 36, 48, and 60 mg/L) was used as simulated wastewater. The dosage of photocatalyst (T-ZnO and SiO2(AG)/T-ZnO) was 2 g/L, respectively. The suspension was stirred for 30 min at room temperature under dark condition, then irradiated under UV (EA-180, 8w; Spectronics Corporation, America). The sample was fetched at an interval of 30 min, then centrifuged (8,000 rpm, 5 min), and filtered (0.22 µm filter membrane). UV-VIS spectrophotometer was used to analyze the concentration change of NB during the photocatalytic degradation process. Formula of photocatalytic removal ratio of NB is as follows:

(2) η % = C 0 − C C 0 ,

where η% is the photocatalytic removal ratio of NB; C 0 is the initial concentration of NB (mg/L); and C is the concentration of NB after photocatalytic reaction (mg/L).

2.6 Photodegradation kinetics

Langmuir–Hinshelwood kinetic models are often used to calculate photodegradation kinetic parameters, which are as follows [47]:

(3) r = − d C d t = − K ad k ′ C 1 + K ad C ,

(4) 1 r = 1 K ad k ′ C + 1 k ′ ,

where r is the photodegradation reaction rate, k′ is the rate constant of NB photocatalytic degradation, mg/(L min−1); K ad is the adsorption equilibrium constant of NB on catalyst surface, L/mg; C is the concentration of NB in solution, mg/L; and t is the reaction time, min.

The process of photocatalytic degradation begins with the catalyst surface adsorbing organic mass. C e is the initial moment (t = 0) concentration of the solution while in adsorption equilibrium. The reaction time is calculated by the following equation:

(5) t = 1 K ad k ′ ln C e C + 1 k ′ ( C e − C ) .

Formulae (3) and (5) can be simplified to formulae (6) and (7), respectively, when the organic content is extremely low. Formula (6) is also used for inefficient adsorption of organic mass. In this case, the reactions are manifested as first-order reactions.

(6) r = − d C d t = K ad k ′ C = k C ,

(7) ln C e C = K ad k ′ t = k t ,

where k is the apparent rate constant, min−1.

3 Results and discussion

3.1 Microtopography of SiO2(AG)/T-ZnO

The microtopography of SiO2(AG) and SiO2(AG)/T-ZnO is demonstrated in Figure 1. As displayed in Figure 1a and c, SiO2(AG) powders were composed of numerous narrow-size-range nanoparticles and presented loose sponge-like porous shapes. The SEM image of SiO2(AG)/T-ZnO nanocomposites (Figure 1b) shows typical structures with four needles extending from the same center, ascribable to the T-ZnO [18] and SiO2(AG) particles uniformly loaded on the surface of these needles. Figure 1(d) shows that the morphology of SiO2(AG) loaded on the surface of T-ZnO has no obvious change.

Figure 1 Morphologies of SiO2(AG) and SiO2(AG)/T-ZnO samples. (a) SEM image of SiO2(AG); (b) SEM image of SiO2(AG)/T-ZnO; (c) TEM image of SiO2(AG); and (d) TEM image of SiO2(AG)/T-ZnO.
Figure 1

Morphologies of SiO2(AG) and SiO2(AG)/T-ZnO samples. (a) SEM image of SiO2(AG); (b) SEM image of SiO2(AG)/T-ZnO; (c) TEM image of SiO2(AG); and (d) TEM image of SiO2(AG)/T-ZnO.

3.2 Crystal structure of SiO2(AG)/T-ZnO

As shown in Figure 2, a bread-like dispersion peak was observed in 2θ = 20–25°, which is the characteristic peak of amorphous SiO2(AG) [48]. Other peaks corresponded with the characteristic peaks of the wurtzite ZnO structure [18]. The peaks of SiO2(AG)/T-ZnO further indicated that SiO2(AG) and T-ZnO still retained their crystal structural characteristics after forming SiO2(AG)/T-ZnO composites.

Figure 2 XRD pattern of SiO2(AG)/T-ZnO sample.
Figure 2

XRD pattern of SiO2(AG)/T-ZnO sample.

3.3 SSA and pore structure of SiO2(AG), T-ZnO, and SiO2(AG)/T-ZnO

SSA and pore structure of SiO2(AG), T-ZnO, and SiO2(AG)/T-ZnO were analyzed via the N2 adsorption–desorption method. As can be seen in Figure 3, N2 adsorption–desorption isotherms of SiO2 (AG), T-ZnO, and SiO2(AG)/T-ZnO were type IV, II, and IV adsorption isotherms, respectively. Figure 3(a) indicates that SiO2(AG) powders were porous materials, and the hole was a narrow tubular pore with open ends and wide mouth [49]. Figure 3(b) shows N2 adsorption behavior on T-ZnO is gas physical absorption, which indicated that T-ZnO was a nonporous material [47]. Figure 3(c) shows that the SiO2(AG) loaded on the surface of T-ZnO still maintained its original shape, and the adsorption of SiO2(AG)/T-ZnO was significantly increased compared with T-ZnO. The SSA, pore size, and pore volume of SiO2(AG), T-ZnO, and SiO2(AG)/T-ZnO are shown in Table 1. Compared to T-ZnO, the SSA, pore size distribution, and pore volume of SiO2(AG)/T-ZnO were significantly improved.

Figure 3 N2 adsorption–desorption isotherm ((a) SiO2(AG), (b) T-ZnO, and (c) SiO2(AG)/T-ZnO).
Figure 3

N2 adsorption–desorption isotherm ((a) SiO2(AG), (b) T-ZnO, and (c) SiO2(AG)/T-ZnO).

Table 1

SSA, pore size, and pore volume of SiO2(AG), T-ZnO, and SiO2(AG)/T-ZnO

Sample SiO2(AG) T-ZnO SiO2(AG)/T-ZnO
SSA (m2/g) 896 0.4310 86.8132
Pore size (nm) 8.93 — 7.08
Pore volume (mL/g) 2.0065 0.0006 0.1418

3.4 UV-VIS DRS analysis

SiO2(AG), T-ZnO, and SiO2(AG)/T-ZnO were characterized by UV-VIS DRS. As shown in Figure 4, SiO2(AG) had lower absorbance within the wavelength range between 200 and 800 nm. T-ZnO and SiO2(AG)/T-ZnO showed strong absorption between 200 and 400 nm. Within the limits of visible light, the absorption of SiO2(AG)/T-ZnO was enhanced slightly. The UV-VIS DRS of SiO2(AG)/T-ZnO was similar to that of T-ZnO.

Figure 4 UV-Visible diffuse reflectance spectra of SiO2(AG), T-ZnO, and SiO2(AG)/T-ZnO.
Figure 4

UV-Visible diffuse reflectance spectra of SiO2(AG), T-ZnO, and SiO2(AG)/T-ZnO.

3.5 Adsorption property of T-ZnO and SiO2(AG)/T-ZnO

Adsorption isotherms of T-ZnO and SiO2(AG)/T-ZnO for NB are demonstrated in Figure 5. In the range of the organic concentration of this experiment, the adsorption amount of SiO2(AG)/T-ZnO and T-ZnO to NB grew with the increase of the equilibrium concentration and equilibrium adsorption capacity up to 3.23 and 2.21 mg/g, respectively. T-ZnO had poor adsorption properties for NB because of small SSA of T-ZnO. The adsorption performance of SiO2(AG)/T-ZnO was better than T-ZnO, because the SiO2(AG) loaded on the surface of T-ZnO has good adsorption for NB [39].

Figure 5 Adsorption isotherms of NB by T-ZnO and SiO2(AG)/T-ZnO.
Figure 5

Adsorption isotherms of NB by T-ZnO and SiO2(AG)/T-ZnO.

3.6 Kinetic study of NB degradation by T-ZnO and SiO2(AG)/T-ZnO

The NB photocatalytic degradation curves of T-ZnO and SiO2(AG)/T-ZnO are shown in Figure 6. Compared to T-ZnO, SiO2(AG)/T-ZnO had better photocatalytic effect for NB with different initial concentrations. The degradation processes of different initial concentrations of NB were fitted by the pseudo first-order kinetic equation. Figure 7 obviously indicates that the degradation processes of NB by T-ZnO and SiO2(AG)/T-ZnO followed the first-order reaction.

Figure 6 Degradation curves of different initial concentrations of NB by SiO2(AG)/T-ZnO (a) and T-ZnO (b).
Figure 6

Degradation curves of different initial concentrations of NB by SiO2(AG)/T-ZnO (a) and T-ZnO (b).

Figure 7 Degradation-fitting curves of NB by SiO2(AG)/T-ZnO (a) and T-ZnO (b).
Figure 7

Degradation-fitting curves of NB by SiO2(AG)/T-ZnO (a) and T-ZnO (b).

Considering the initial moment reaction kinetic, the curves of 1/C e and 1/r 0 are displayed in Figure 8, and the relevant fitting equations are as follows:

SiO 2 ( AG ) /T-ZnO: 1 r 0 = 35.397 C 0 + 4.1307 R 2 = 0.976 ,

T-ZnO: 1 r 0 = 63.695 C 0 + 6.7816 R 2 = 0.9915 .

Figure 8 Curves of 1/C e and 1/r 0 of NB degradation.
Figure 8

Curves of 1/C e and 1/r 0 of NB degradation.

The degradation kinetics of SiO2(AG)/T-ZnO and T-ZnO were consistent with the Langmuir–Hinshelwood kinetic model. The degradation rate constant and adsorption constant of NB using SiO2(AG)/T-ZnO and T-ZnO could be calculated, which were k′ = 0.2421 mg/L min−1, K ad = 0.1167 L/mg and k′ = 0.1475 mg/L min−1, K ad = 0.1065 L/mg. The results indicated that k SiO 2 AG / T-ZnO ′ > k T-ZnO ′ , K ad SiO 2 ( AG ) / T-ZnO > K ad T-ZnO. According to the phenomenon, we concluded that the loading of SiO2(AG) could increase T-ZnO adsorption to NB, and then promoted photocatalysis.

4 Conclusion

SiO2(AG)/T-ZnO composites were prepared via a simple and controllable method. Various characterization methods showed that the morphology and structural characteristics of SiO2(AG) and T-ZnO were retained after SiO2(AG) loading on the surface of T-ZnO. The photocatalytic degradation processes of NB using T-ZnO and SiO2(AG)/T-ZnO followed the first-order reaction. SiO2(AG)/T-ZnO had better photocatalytic performance. Considering the initial moment reaction kinetic, the photocatalytic kinetic of SiO2(AG)/T-ZnO and T-ZnO was consistent with the Langmuir–Hinshelwood kinetic model, and reaction rate constant k SiO 2 AG / T-ZnO ′ > k T-ZnO ′ , adsorption rate constant K ad SiO 2 ( AG ) / T-ZnO > K adT-ZnO, which demonstrated SiO2(AG) loading could increase T-ZnO adsorption to NB, then promoted its photocatalytic performance. Compared with the conclusions of the important relevant papers of this study, loading SiO2(AG) on the surface of T-ZnO can retain the morphology and structural characteristics of T-ZnO and SiO2(AG) unchanged, and the photocatalysis of SiO2(AG)/T-ZnO composites for NB can be significantly improved. The improvement of the catalytic performance of the material by this method is better than that of other porous materials combined with semiconductor materials.

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Acknowledgments

This work was supported by the National Natural Science Foundation of China (No. 21507052), Project of Introduction of Teachers of Leshan Normal University, Sichuan Province, China (Grant No. Z1517), and Scientific Research Fund of Leshan Normal University, Sichuan Province, China (Grant No. 205190012).

  1. Author contributions: Zhigang Yi designed the experiments, contributed to characterization of materials, and led the drafting of the manuscript. Tao Jiang and Ying Cheng assisted in the analysis and testing work during the experiments. Qiong Tang designed and supervised the experiments.

  2. Conflict of interest: The authors declare no conflict of interest regarding the publication of this paper.

  3. Data accessibility: The authors conducted the experiment systematically and reported experimental procedure clearly in Section 2 and provided all necessary data in Section 3 of the manuscript.

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Received: 2020-04-20
Revised: 2020-10-01
Accepted: 2020-10-01
Published Online: 2020-10-23

© 2020 Zhigang Yi et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/ntrev-2020-0081
Keywords for this article
silica aerogels; tetrapod-like zinc oxide; adsorption property; photocatalytic performance; nitrobenzene
Creative Commons
BY 4.0

Articles in the same Issue

  1. Research Articles
  2. Generalized locally-exact homogenization theory for evaluation of electric conductivity and resistance of multiphase materials
  3. Enhancing ultra-early strength of sulphoaluminate cement-based materials by incorporating graphene oxide
  4. Characterization of mechanical properties of epoxy/nanohybrid composites by nanoindentation
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  81. Review articles
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  83. Review on the research progress of cement-based and geopolymer materials modified by graphene and graphene oxide
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  106. Theoretical calculation of a TiO2-based photocatalyst in the field of water splitting: A review
  107. Two-photon polymerization nanolithography technology for fabrication of stimulus-responsive micro/nano-structures for biomedical applications
  108. A review of passive methods in microchannel heat sink application through advanced geometric structure and nanofluids: Current advancements and challenges
  109. Stress effect on 3D culturing of MC3T3-E1 cells on microporous bovine bone slices
  110. Progress in magnetic Fe3O4 nanomaterials in magnetic resonance imaging
  111. Synthesis of graphene: Potential carbon precursors and approaches
  112. A comprehensive review of the influences of nanoparticles as a fuel additive in an internal combustion engine (ICE)
  113. Advances in layered double hydroxide-based ternary nanocomposites for photocatalysis of contaminants in water
  114. Analysis of functionally graded carbon nanotube-reinforced composite structures: A review
  115. Application of nanomaterials in ultra-high performance concrete: A review
  116. Therapeutic strategies and potential implications of silver nanoparticles in the management of skin cancer
  117. Advanced nickel nanoparticles technology: From synthesis to applications
  118. Cobalt magnetic nanoparticles as theranostics: Conceivable or forgettable?
  119. Progress in construction of bio-inspired physico-antimicrobial surfaces
  120. From materials to devices using fused deposition modeling: A state-of-art review
  121. A review for modified Li composite anode: Principle, preparation and challenge
  122. Naturally or artificially constructed nanocellulose architectures for epoxy composites: A review
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