Multifunctional Zn0.3Al0.4O4.5 crystals: An efficient photocatalyst for formaldehyde degradation and EBT adsorption

Umesh Fegade; Ganesh Jethave; Wei-Gang Hong; Imran Khan; Hadi M. Marwani; Inamuddin; Ren-Jang Wu; Rajesh Dhake

doi:10.1016/j.arabjc.2020.04.002

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Original article

13 (

); 8262-8270

doi:

10.1016/j.arabjc.2020.04.002

Multifunctional Zn_0.3Al_0.4O_4.5 crystals: An efficient photocatalyst for formaldehyde degradation and EBT adsorption

Umesh Fegade^{^a,⁎}, Ganesh Jethave^{^b}, Wei-Gang Hong^{^c}, Imran Khan^{^d}, Hadi M. Marwani^{^e}, Inamuddin^{^e,⁎}, Ren-Jang Wu^{^c,⁎⁎}, Rajesh Dhake^{^f}

a Department of Chemistry, Bhusawal Arts, Science and P.O. Nahata Commerce College, Bhusawal, Jalgaon 425201 (M.H.), India

b School of Environmental and Earth Sciences, Kavayitri Bahinabai Chaudhari North Maharashtra University, Jalgaon 425001 (M.H.), India

c Department of Applied Chemistry, Providence University, Shalu, Taichung 433, Taiwan

d Applied Science Section, Faculty of Engineering and Technology, Aligarh Muslim University, Aligarh 202 002, India

e Chemistry Department, Faculty of Science, King Abdulaziz University, Jeddah 21589, Saudi Arabia

f Department of Chemistry, D. D. N. Bhole College, Bhusawal, Jalgaon 25201 (M.H.), India

⁎Corresponding authors. umeshfegade@gmail.com (Umesh Fegade), inamuddin@zhcet.ac.in (Inamuddin),

⁎⁎Corresponding author. rjwu@pu.edu.tw (Ren-Jang Wu)

Received: 2020-3-10, Accepted: 2020-4-2, Published: 2020-11-01

Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Peer review under responsibility of King Saud University.

Abstract

The Zn_0.3Al_0.4O_4.5 nanoparticles (ZnAlONPs) with size of 70–90 nm are used as an efficient photocatalyst for formaldehyde (HCHO) degradation and effective adsorbent for the removal of eriochrome black-T (EBT) dye from synthetic aqueous solution. Degradation of HCHO reactions were studied using TiO₂ (homemade), TiO₂ (P-25) and ZnAlONPs by irradiating under 18 W daylight lamp source for photocatalytic degradation. The HCHO degradation rate is about 67, 76 and 89% for TiO₂ (homemade), TiO₂ (P25) and ZnAlONPs during 2 h reaction, respectively at initial formaldehyde gas concentration of 20 ppm. Maximum adsorption capacity was optimized by changing the parameters such as pH, EBT concentration and adsorbent dosage. A 200 mg of ZnAlONPs are useable for quick removal of EBT (>95%). Langmuir isotherm model showed a maximum adsorption capacity of 90.90 mgg⁻¹. The ZnAlONPs could be successfully reused upto 5^th adsorption/desorption cycle for EBT dye removal from water samples.

Keywords

ZnAlONPs

HCHO degradation

Eriochrome black T

Pseudo second order model

Langmuir isotherm

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1 Introduction

Environmental pollution originated by HCHO, is becoming a severe problem in front of scientists and researchers. Among the many chemical contaminants usually found in polluted indoor air, formaldehyde (HCHO) is one of the major species (Zhang et al., 2016). Long term exposure of lower concentration of formaldehyde could cause eye and throat irritation and chest tightness (Tasbihi et al., 2015). Various studies (Ai et al., 2010; Kim et al., 2011; Sekiguchi et al., 2011; Fan et al., 2011; Wan et al., 2011 ) have presented high conversions of formaldehyde degradation as catalytic oxidation (Kim et al., 2011), high-frequency ultrasound combination with photocatalytic way (Sekiguchi et al., 2011), plasma-catalytic removal method (Fan et al., 2011) and direct circuit corona discharge plasma method (Wan et al., 2011). The photo degradation of HCHO, commonly uses TiO₂photocatalytic material in industry. There are several advantages of TiO₂ material towards photocatalytic HCHO degradation (Liu et al., 2008); for example high resistant to photo-corrosion, environmentally clean and known to completely oxidize HCHO into CO₂ and H₂O (Liang et al., 2012; Wang et al., 2012; Fu et al., 2011; Zhu and Wu, 2015 ).

Dyes have adverse effects on human body as well as aquatic life. These are readily used in textile, printing, dyeing, and related industries which discharge the huge amount of dye-containing wastewater into the environment and generates hazards for human health (Iram et al., 2010; Zhu et al., 2012; Fisli et al., 2014 ). Very small amount of dye in huge water reduces the photosynthesis efficiency for aquatic life. Dyes are generally thermo and photo stable and possess high resistance to chemical; these qualities increase the serious concern of scientist toward the removal of dyes from the wastewater (Girgis et al., 2015). The various techniques have been applied for removal of dyes from wastewaters (flocculation, coagulation, precipitation, membrane filtration, and adsorption techniques). Among these adsorption method associated with nanoadsorbent widely useful for dyes removal (Kong and Gan, 2012; Deng et al., 2013; Zhang et al., 2014; Zhou et al., 2015; Afkhami et al., 2010 ). There are some examples about the adsorption application using various adsorbents in recent studies (Van Tran et al., 2019a, 2019b, 2018c, 2019d, 2019e, 2019f, 2019g, 2020 ). The conventional activated carbon and zeolites have poor adsorption capacity and low dye removal efficiency (Sharma and Lee, 2015, 2017a, 2017b, 2014; Sharma et al., 2010 ). Thus, improvement of novel nanomaterials having high adsorption ability is still crucial task for scientist (Dehghanian et al., 2016). Sodium 1-[1-hydroxynaothylazo]-6-nitro-2-napthol-4-sulfonate i.e. Eriochrome black T (EBT) is anionic azo dye. It is hazardous (carcinogenic) in case of skin contact and irritant on eye contact. EBT is used in complexometric titrations and for dyeing silk (Dutta et al., 2014; Jethave et al., 2018a, 2018b ). In previous years our research group reported the receptor for sensing of ions from wastewater (Fegade et al., 2014a, 2014b, 2014c, 2014d, 2014e, 2015; Jethave and Fegade, 2018; Kondalkar et al., 2018 ). The current study explored the application of ZnAlONPs for photo-degradation of formaldehyde as well as adsorption of EBT.

2 Experimental

2.1

2.1 Materials and instrumentation

All the chemicals used in this work were of analytical grade and purchased from Merck, Germany. The MiliQ water (A Grade) was used in every stage of the study. The characterization done by FE-SEM (Bruker S-4800 at 15.0 kV), EDX (500 × 375 Magnitude: 40,000 × HV:15.0 kV), FTIR (Model: FT-IR Bruker) in the range of 500–4000 cm⁻¹ and UV–Visible spectrophotometer (Shimadzu UV-1800) at 25 °C.

2.2

2.2 Formaldehyde degradation system

During this study, 200 mg of ZnAlONPs was positioned in reactor with volume of 0.7L. HCHO gas was passed from reactor to test the photo catalytic activity of ZnAlONPs in 18 W daylight lamp of intensity 8.8 mWcm⁻² and the remaining concentration of HCHO is calculated after fixed interval (Supplementary Fig. S1). The HCHO degradation rate was determined by Eq. (1):

(1)

H C H O d e g r a d a t i o n r a t e (%) = (C_{0} - C_{e}) / C_{0} \times 100 %

where C₀ and C_e are the initial and final concentration of HCHO gas, respectively.

2.3

2.3 Batch adsorption experiment for EBT dye removal

Adsorption behavior of EBT was performed by varying experimental parameters. Optimization of adsorption method is done by varying doses (50–200 mg) of ZnAlONPs into the 50 ml solution of different doses of EBT (50–200 mg) in a 100 ml conical flask. The solution was shaken for 90 min on rotary shaker at 200 rpm. The adsorption of dye is calculated, the aliquot taken at time interval centrifuged at 2000 rpm for 3 min and the supernant solution is used for the measurement of concentration of EBT using spectrophotometer at 489 nm. The concentration of EBT decreased with time due to its adsorption on ZnAlONPs. The adsorption capacity (q_e) of nanoparticles for EBT dye was calculated by Eq. (2).

(2)

q_{e} = (C i - C e) V / m

where Ci = initial concentrations, Ce = equilibrium concentrations (mg/L), m = mass of the adsorbent (g) and V = volume (L).

2.4

2.4 Kinetic models, adsorption isotherms, separation factor and thermodynamic parameters equations

The pseudo–II–order kinetic model formula

(3)

t / q_{t} = 1 / {k_{a d} q_{e}}^{2} + t / q_{e}

The general form of the Langmuir isotherm is:

(4)

q_{e} α_{L} / K_{L} = K_{L} C_{e} / (1 + K_{L} C_{e})

After linearization of the Langmuir isotherm, Eq. (4), we obtain

(5)

C_{e} / q_{e} = C_{e} α_{L} / K_{L} + 1 / K_{L}

The adsorbed EBT (mg/g) was calculated based on a mass balance equation:

(6)

q_{e} = V (C_{o} - C_{e}) / m

The Freundlich isotherm can be expressed as:

(7)

q_{e} = {K_{f} C_{e}}^{1 / n}

where Ce = equilibrium concentration (mg/L), qe = amount adsorbed at equilibrium (mg/g), and K_f and 1/n = Freundlich constants

The linearized form of the Freundlich adsorption isotherm equation is as follows

(8)

l n q_{e} = l n K_{f} + l n C_{e} / n

A separation factor as described by Fegade et al. (2014e) (R_L), is defined as:

(9)

R_{L} = 1 / (1 + α_{L} C_{o})

where α_L = Langmuir coefficient and C₀ = initial dye concentration.

Thermodynamic parameters equation

(10)

Δ G = - R T l n K_{L}

where R = (8.314 J mol⁻¹ K⁻¹), T = Temperature and K_L = Langmuir constant (L mol⁻¹).

3 Results and discussion

3.1

3.1 Fabrication of ZnAlONPs

ZnAlONPs were fabricated by co-precipitation method followed by heating with stirring (Jethave et al., 2017). Initially 0.75 mol of ZnCl₂ and 1.0 mol of AlCl₃ were poured into the 300 ml distilled water (DW). Then 50 ml of 1 M NaOH and 30 ml ammonia was added drop wise with constant stirring for two hr at 60 °C. The white precipitates were dried for 4 h and then crushed into powder and again heated in an oven at 400 °C for 4 hr for calcinations. Fig. 1 show FE-SEM images of ZnAlONPs. Fig. 1(a), shows that the synthesized material has nano flake character and image (b) shows the nano flake size upto 70–90 nm. EDX spectrum confirmed the presence of Zn, Al and O in nano flake having 20.81, 10.15 and 69.03%, respectively (Fig. 2). The chemical composition of ZnAlONPs was explored using FTIR analysis and the FTIR spectrum is shown in Fig. 3. The broad band at 3366 cm⁻¹ is assigned to the O—H stretching vibrations of free water (Zawrah and El Kheshen, 2002; Kurien, 2010). The band at 1358 cm⁻¹ corresponds to metal–alloy (Zn–Al) and bands at 774 and 687 cm⁻¹ are attributed to Zn—O bonds while bands at 545 and 511 cm⁻¹ show the presence of the Al—O vibration bands (Zawrah and El Kheshen, 2002; Kurien, 2010) (Fig. 3).

(a) Closed FE-SEM image, and (b) FE-SEM images of nano flake ZnAlONPs with size 70–90 nm.

3.2

3.2 Photo-degradation of formaldehyde

The photocatalytic HCHO degradation system and its working are given in supplementary Fig. S1. The photo-degradation of HCHO was investigated quantitatively using TiO₂ (homemade), TiO₂ (P25) and Zn_0.3Al_0.4O_4.5 under 18 W daylight lamp irradiation and the results are shown in Fig. 4. The degradation rate was found to be 67, 76 and 89% for TiO₂ (homemade), TiO₂ (P25) and Zn_0.3Al_0.4O_4.5 during 2 h reaction, respectively (Supplimentry information Table S1). The ZnAlONPs showed a maximum photo-degradation efficiency for HCHO than other catalysts because ZnAlONPs have wide range and strong absorption in visible light region than the TiO₂ (P25).

The photo-degradation of 20 ppm HCHO by various photo-catalysts (a) Homemade TiO2 (b) P-25 TiO2 (c) ZnAlONPs under photo radiation.

3.3

3.3 Possible mechanism of HCHO degradation

HCHO photo-degradation mechanism as proposed is shown in Fig. 5 and Eqs. (11)–(16). Eq. (11) described the electron excitation and hole formation using photoenergy. Under visible light irradiation of ZnAlONPs the electrons present in valence band are excited and transfer to conduction band and form electron-hole pairs. The Eq. (13) shows the generation of •OH radicals using photocatalyst and Eqs. (14)–(16) shows the degradation of HCHO through the •OH radicals which is previously generated by photocatalyst in equation (13).

(11)

Photocatalyst → e⁻ + h⁺

(12)

H₂O → H⁺ + OH⁻

(13)

h⁺ + OH⁻ → ^•OH

(14)

HCHO + ^•OH → HCO + H₂O

(15)

HCO + ^•OH → HCOOH

(16)

HCOOH + 2 h⁺ → CO₂ + 2H⁺

Schematic representation of possible mechanism of HCHO degradation.

3.4

3.4 Effect of pH, time and adsorbent variation

The effect of pH on dye adsorption using ZnAlONPs was evaluated at various pH ranges 3–10. Fig. 6 shows that percent adsorption enhance from 38 to 96% when the pH varies from 4 to 6. It is due to the protonation on ZnAlONPs. The dissociation constant pKa for EBT is 6.2 and 11.55, consequently EBT present as monovalent anions, at the equilibrium pH (Dehghanian et al., 2016). EBT was protonated and increases repulsion with ZnAlONPs due to similar charges and percent removal decreases at low pH. As demonstrated the experiment by varying the time from 0 to 120 min in supplementary Fig. S2, the maximum adsorption efficiency of EBT was achieved after 60 min and the phenomenon is explained based on that the great numbers of active sites if available but active sites required sufficient contact time for the chemical or physical interaction for adsorption. The influence of ZnAlONPs quantity on adsorption of EBT was examined in batch experiments by adding adsorbent in range of 50–200 mg in 50 mg L^-1 dye solution. The results showed that the ZnAlONPs amount is directly proportional to percent adsorption, until it reaches a saturation point. The enhancement in percent adsorption with ZnAlONPs can be attributed to increased surface area and more adsorption sites. Fig. 7 results showed that the adsorption efficiencies (%) increased from 58.51 to 97.75% by increasing adsorbent dose from 50 to 200 mg due to availability of more adsorption sites.

Effect of pH on adsorption of EBT (conditions, ZnAlONPs dose = 200 mg, EBT concentration = 50 mg/L, shaking time = 90 min). Inset shows the color of dye solution before and after treatment.

Variation in ZnAlONPs dose at constant EBT concentration (at 25 °C).

3.5

3.5 Kinetic models, adsorption isotherms, separation factor and thermodynamic parameters

To determine the controlling mechanism of dye adsorption from aqueous solution, the adsorption kinetics of EBT on ZnAlONPs was analyzed using kinetic models proposed by Ho and McKay (1999a, 1999b). The kinetic study confirmed the pseudo second-order (Fig. 8 and Table 1). The results obtained for adsorption of EBT were analyzed by the use of well known Langmuir (Dada, 2012; Langmuir, 1916, 1918 ) and Freundlich (Dada, 2012; Freundlich and Heller, 1939) models. The isotherms for EBT were obtained for ZnAlONPs at the solution pH of 5.5. The Figs. 9 and 10 represent the graph obtained by the adsorption isotherms and the calculated parameters are shown in Table 2. It is clear that the Langmuir is preeminent fitted than Freundlich of EBT adsorption. So, it is concluded that the above study may be a homogeneous monolayer adsorption. The separation factor (R_L) (Weber and Chakravorti, 1974) for EBT dye fall in between 0 and 1 which shows that dye adsorption on nano flake is a favorable adsorption process (Fig. 11). The study of temperature illustrated whether the process is exothermic or endothermic. The variation of dye EBT adsorbed on ZnAlONPs as function of solution temperature (Fegade et al., 2014a) is shown in Fig. 12. The ΔG determined is −7.08 kJ mol⁻¹. The negative ΔG specifies the spontaneous nature of process between adsorbent for the dyes (Banerjee and Chattopadhyaya, 2017; Deniz, 2013; Murcia-Salvador et al., 2019 ).

Kinetic plots of EBT onto ZnAlONPs at various primary EBT concentrations.

Table 1 Result obtained by Kinetic equation.

Parameters
Concentration (mg)	50	100	150	200
K_ad g mg^-1 min⁻¹	0.045	0.094	0.089	0.083
qe (mg/g)	62.5	83.33	100	111.11
R²	0.997	0.998	0.993	0.995

Linearization of the Langmuir isotherm. Conditions: pH 5.5, and 25 °C.

Freundlich plot for the adsorption of EBT onto ZnAlONPs at 25 °C and pH 5.5.

Table 2 Data calculated from Langmuir and Freundlich.

Langmuir		Freundlich
K_L	13.157	log K_f	1.347
q_max = K_L/α_L	90.909	1/n	0.328
R²	0.991	R²	0.98

RL of the adsorption of EBT onto ZnAlONPs at 25 °C. (C0 = initial EBT dye concentration).

Effect of temperature on qe of dye EBT using ZnAlONPs.

3.6

3.6 Reuse of ZnAlONPs by acidic cleaning

To explore the reuse ability of ZnAlONPs the dye adsorbed material converted in to desorbed material using HCl (0.1 M) and repeated upto five cycles. It is confirmed that the percent adsorption of ZnAlONPs is higher than 93% after the five reuse cycles (Fig. 13).

Effect of reuse of ZnAlONPs by acid clean on adsorption.

4 Conclusion

The ZnAlONPs showed the rapidest HCHO decomposition efficiency rate than TiO₂ catalysts. The ZnAlONPs synthesized by easy and economic way for EBT adsorption. The degradation of HCHO was studied on a variety of TiO₂ (home made), TiO₂ (P-25) and ZnAlONPs under photo irradiation. The HCHO degradation rate is about 67, 76 and 89% for TiO₂ (home made), TiO₂ (P25) and ZnAlONPs during 2 h reaction, respectively at 20 ppm initial formaldehyde concentration. The small amount 200 mg of the proposed ZnAlONPs is applicable for quick removal of EBT (>95%). From the above results we can say that the synthesized nano flake will be the effective candidate for the HCHO photocatalysis as well as for EBT adsorption.

Acknowledgement

This project was funded by the Deanship of Scientific Research (DSR) at King Abdulaziz University, Jeddah, under grant no. KEP-54-130-38. The authors, therefore, acknowledge with thanks DSR for technical and financial support.

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Appendix A

Supplementary material

Supplementary data to this article can be found online at https://doi.org/10.1016/j.arabjc.2020.04.002.

Appendix A

Supplementary material

The following are the Supplementary data to this article:

Supplementary data 1

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Multifunctional Zn0.3Al0.4O4.5 crystals: An efficient photocatalyst for formaldehyde degradation and EBT adsorption

Abstract

Keywords

ZnAlONPs

HCHO degradation

Eriochrome black T

Pseudo second order model

Langmuir isotherm

1 Introduction

2 Experimental

2.1 Materials and instrumentation

2.2 Formaldehyde degradation system

2.3 Batch adsorption experiment for EBT dye removal

2.4 Kinetic models, adsorption isotherms, separation factor and thermodynamic parameters equations

3 Results and discussion

3.1 Fabrication of ZnAlONPs

3.2 Photo-degradation of formaldehyde

3.3 Possible mechanism of HCHO degradation

3.4 Effect of pH, time and adsorbent variation

3.5 Kinetic models, adsorption isotherms, separation factor and thermodynamic parameters

3.6 Reuse of ZnAlONPs by acidic cleaning

4 Conclusion

Acknowledgement

References

Appendix A

Supplementary material

Appendix A

Supplementary material

Supplementary data 1

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Multifunctional Zn_0.3Al_0.4O_4.5 crystals: An efficient photocatalyst for formaldehyde degradation and EBT adsorption