Adsorptive and Photocatalytic Degradation of Imidacloprid Pesticide from Wastewater via the ZrP/NiSe 2 nanocomposite

doi:10.21203/rs.3.rs-4933424/v1

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Adsorptive and Photocatalytic Degradation of Imidacloprid Pesticide from Wastewater via the ZrP/NiSe 2 nanocomposite

https://doi.org/10.21203/rs.3.rs-4933424/v1

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In this study, ZrP/NiSe₂ nanocomposite was constructed for the first time. Characterizations were carried out by FT-IR, XRD, EDX mapping and FESEM, confirming the nanocomposite formation. The resulting sustainable ZrP/NiSe₂ nanocomposite exhibit improved photocatalytic activity in the visible area to remove imidacloprid from water compared to pure ZrP and NiSe₂ nanoparticles. Improving the performance of this nanocomposite can be the result of the integration of ZrP and NiSe₂ at the nanoscale and the synergistic enhancement of their activity. Furthermore, ZrP/NiSe₂ and ZrP can remove significant percentages of imidacloprid from aqueous solutions through adsorption. This result can be explained by the high adsorption affinity of ZrP toward organic pollutants with protonable groups.

Physical sciences/Chemistry

Physical sciences/Nanoscience and technology

Photocatalytic degradation

Imidacloprid

Zirconium phosphate

Nickel selenide

nanocomposite

Pesticides are used to control the harmful pests and thus improve agricultural production. Therefore, pesticides are an important component of the agricultural industry. However, the use of pesticides brings various adverse environmental impacts. Imidacloprid (Fig. 1), a potent neonicotinoid insecticide, is one of the most widely used pesticides, which is commonly used in seed treatment to control the insects. This insecticide is highly toxic having good solubility and stability in water and its widespread application has caused significant environmental concerns.(1, 2)

In recent decades, the scientific community has devoted a significant deal of effort to developing innovative and functional materials that can be applied in water and wastewater treatment, which has further accelerated the development of photocatalytic technology.(3, 4)

Due to their outstanding physical and chemical properties, α-zirconium phosphate (α-ZrP) and its derivatives have been widely investigated in adsorption processes for the removal and degradation of pollutants from wastewater,(5, 6) medical field, namely in the drug delivery,(7, 8) ion-exchange processes (9, 10), photocatalysis processes (11, 12), anti-corrosion technology (13, 14) and composite material preparation to allow their application in various fields (15, 16).

α-ZrP has been extensively investigated as catalysts and catalyst supports for a wide variety of applications due to its superior properties.(17–24) However, α-ZrP do not show satisfactory visible-light photocatalytic activity, due to a broad band gap.(11) Combination of α-ZrP with semiconductor has been proposed as an impactful solution to improve photocatalytic performance of the α-ZrP for the degradation of organic pollutants.(12)

Nickel selenide (NiSe₂) is an inorganic compound exhibiting wide range of applications including fields of electrocatalysis, high-temperature superconductors, energy storage gadgets, photocatalyst and electrocatalysts.(25, 26) NiSe₂ also offers several advantages including excellent electronic properties, chemical stability, having the appropriate band gap energy to absorb visible light (1.98 eV), low cost, low toxicity, and bio-compatibility.(27–29) As mentioned earlier, NiSe₂ has an adequate band gap to absorb visible light, however, due to the electron-hole pair recombination, its photocatalytic performance is not as efficient as expected. Literature on photocatalysis applications of NiSe₂ highlights the employment of a pronged strategy for enhancing the photocatalytic performance of activity of NiSe₂, namely; forming composites.(29)

The photocatalytic activity of NiSe₂-based composites on photodegradation of various organic pollutants in aqueous medium has been studied recently. Zhong et al.(25) reported that 9 mol% NiSe₂ composited BiVO₄ exhibited high photocatalytic performance for photodegradation Rhodamine B (RhB) under visible light compared to pure BiVO₄. Coupling NiSe₂ with TiO₂ exhibited improved photocatalytic efficiency in the photodegradation of RhB compared to pure ones.(26) Recently, Waseem Luo et al.(29) have been studied the photocatalytic activity of NiSe₂/Ag₃PO₄ nanocomposite for the photodegradation of RhB and Bisphenol A (BPA) pollutants. The 20% NiSe₂/Ag₃PO₄ nanocomposite as a promising photocatalyst effectively degraded 10 ppm RhB in 20 min and 20 ppm BPA in 30 min under visible light. Reduced graphene oxide (rGO) incorporated NiSe₂ nanocomposite has been synthesized and its photocatalytic performance was investigated via the degradation of RhB. The as-prepared nanocomposite showed 98.8% degradation of RhB after 120 min under visible light irradiation.(30)

Herein, we prepared a nanocomposite by combining NiSe₂ with ZrP and successfully used it for the removal of Imidacloprid pesticide in aqueous solution. In view of the photocatalytic and adsorption potential of NiSe₂ and ZrP nanoparticles, we speculate that ZrP/NiSe₂ nanocomposite should be effective to eliminate water organic pollutants.

Materials and apparatus

All chemicals and solvents were purchased from Merck (Germany) or Fluka (Switzerland). The Fourier-transform infrared (FT-IR) spectra of the samples were recorded with the KBr pellet method on a PerkinElmer PE-1600-FTIR spectrometer. The field emission scanning electron microscope (FESEM) images were recorded using a TESCAN VEGA 3, Czech microscope. X-ray diffraction (XRD) spectra were recorded using an X-ray diffractometer (PANalytical X'Pert PRO, Netherlands) with Cu Kα radiation (λ = 1.54 Å).

Synthesis of NiSe₂ nanoparticles

Initially, 6.6 mmol selenium powder was added into 2 mL of hydrazine hydrate. After a few minutes of sonication, 3.3 mmol Ni(NO₃)₂•6H₂O was added with ultra-sonication to form a homogeneous solution. The mixture was then transferred to a 50 mL Teflon-lined autoclave which was maintained at 180°C for 24 h. The autoclave was then cooled to room temperature and the NiSe₂ particles were collected by filtration. Subsequently, the obtained particles were washed with deionized water until pH = 7 and were dried for 24 h in a vacuum oven at 60°C.(31)

Synthesis of ZrP nanoparticles

To synthesize ZrP, 3.22 g Zirconium oxychloride (ZrOCl₂•8H₂O) was dissolved in deionized water and slowly dropped into the 40 mL diluted phosphoric acid solution (11 mol.L^− 1) under continuous stirring. After refluxing in an oil bath100°C for 24, the product was filtered and rinsed with deionized water several times to remove unreacted phosphoric acid and other impurities until the pH of the filtrate was neutral. Eventually, the sample was dried overnight in a vacuum oven at 60°C to obtain the ZrP powder.(32)

Synthesis of ZrP/NiSe₂ nanocomposite

We have used a straightforward surface soaking method to prepare ZrP/NiSe₂ nanocomposite. First, ZrP powder (0.1 g) was dispersed in deionized water (10 mL) by centrifuging for 30 min. After adding NiSe₂ nanoparticles (0.05 g), the suspension was sonicated for 30 min and stirred at room temperature for 24 hours. Eventually, the ZrP/NiSe₂ powder was collected by centrifugation, washed three times with distilled water, and dried overnight at 50°C.

Photocatalytic degradation of imidacloprid

Photocatalytic degradation experiments of imidacloprid (10 mL of 20 ppm) were conducted under visible light irradiation (LED lamp). The lamp was placed at a distance of 30 cm from the surface of the test solution. The temperature of the system was simply controlled by using a water bath. The irradiated solution was sampled every 15 min. The concentration of imidacloprid was quantified by UV–Vis spectrophotometry (Shimadzu, CPS-240A).

Characterization of the photocatalysts

A set of characterization techniques, such as FT-IR and, XRD, EDX mapping and FESEM, was used to get better insight into the structural properties of the prepared ZrP, NiSe₂ and ZrP/NiSe₂ samples.

XRD patterns of the synthesized ZrP, NiSe₂ and ZrP/NiSe₂ samples are illustrated in Fig. 2. Figure 2 represents the XRD pattern of cubic NiSe₂, which exhibits the characteristic peaks at 2θ values of 30.01, 33.64, 36.96, 42.94, 50.82, 53.26, 55.59, 57.89, 62.30, 72.66, and 74.65° in lattice planes (200), (210), (211), (220), (311), (222), (023), (321), (400), (421), and (332), respectively.(33)

Figure 2 also shows the XRD pattern of ZrP sample. The XRD pattern shows diffraction peaks at 2θ values of 11.84, 20.04, 25.14 and 34.13° respectively assigned to the (002), (110), (112), (020) planes, respectively, indicating the crystalline nature of the as-prepared ZrP.(34, 35) The typical reflection observed at 2θ values of 11.8°, due to the (002) crystallographic planes, indicates the interlayer distance of ZrP crystals. The interlayer distance of ZrP calculated by Bragg Eq. (2d sin θ = n λ) was 7.47 Å.(11)

The XRD pattern of Zrp/NiSe₂ nanocomposite (Fig. 2) demonstrates the presence of ZrP as well as NiSe₂ peaks. The NiSe₂ characteristic peaks were obtained at 2θ values of 30.02, 33.67, 37.00, 42.98, 50.82, 53.13, 55.66, 57.91, 72.75, and 74.76° and ZrP characteristic peaks were obtained at 2θ values of 11.73, 19.98, 24.79, and 34.50°. The interlayer distance of the ZrP in ZrP/NiSe₂ composite calculated according to Bragg equation was 7.53 Å.

Figure 3 presents the FTIR spectra of ZrP and NiSe₂ and ZrP/NiSe₂ nanocomposite. For the pure NiSe₂ nanoparticles, a broad band observed around 3300 − 3600 cm^− 1 and a peak at 1622 cm^− 1 could be attributed to the stretching and bending vibrations of the water’s hydroxyl groups adsorbed at the surface of NiSe₂, respectively. The stretching vibrations of Ni–Se bonds were characterized by a broad peak in the region of 500 to 800 cm^− 1.(28, 36)

For the pure α-ZrP nanoparticles, the sharp band located at 1041 cm^− 1 can be assigned to the symmetrical stretching vibration peak of PO₄³⁻ groups. The characteristic peak at 594 cm^− 1 can be ascribed to Zr − O bonds.(12)

FT-IR spectra recorded for ZrP/NiSe₂ nanocomposite exhibits all of the characteristic peaks of ZrP and of NiSe₂, indicating the presence of both nanoparticles in the nanocomposite composition. These results are in agreement with XRD results shown in Fig. 2.

As expected, the EDX spectrum of the ZrP/NiSe₂ nanocomposite (Fig. 3) clearly shows the presence of zirconium, phosphorus, nickel and selenium atoms in the composite combination. Furthermore, as can be seen in the EDX mapping (Fig. 4), the zirconium, phosphorus, nickel and selenium elements are homogeneously dispersed on the surface of the ZrP/NiSe₂ nanocomposite.

The surface morphologies of the synthesized NiSe₂, ZrP and ZrP/NiSe₂ samples was investigated using FESEM (Fig. 5). The NiSe₂ sample well exhibit a cubic-like morphology, as shown in Figs. 5A and 5B. The morphology of the ZrP was vividly shown in Figs. 5C and 5D at various magnifications (500 nm and 200 nm). The as-prepared ZrP particles formed disk shapes, as seen in Fig. 5C and 5D. It is clear that the ZrP disks have good uniformity. When the ZrP/NiSe₂ nanocomposite is formed using a straightforward surface soaking method, SEM images are obtained and shown in Fig. 5E and 5F. It can be seen that the particles of NiSe₂ were attached to the ZrP in the ZrP/NiSe₂ nanocomposite.

Consequently the results of the FT-IR, XRD, EDX mapping and FESEM characterization techniques confirm the successful preparation of ZrP, NiSe₂ and ZrP/NiSe₂ samples.

Photocatalytic degradation studies

The catalytic activity evaluation of the as-synthesized ZrP, NiSe₂ and ZrP/NiSe₂ samples was done on the removal of imidacloprid from the aqueous solution. The results of the study of imidacloprid removal are summarized in Fig. 6 and Table 1.

Preliminary tests on the catalytic activity of ZrP and NiSe₂ samples as well as ZrP/NiSe₂ for removal of imidacloprid displayed that ZrP and NiSe₂ samples were less active and the ZrP/NiSe₂ nanocomposite showed the highest photocatalytic activity in removal of imidacloprid than that of the pure ZrP and NiSe₂ photocatalysts (Fig. 6A). It seems that the combination and synergistic effect of NiSe₂ and ZrP play an important role for improvement of the photocatalytic activity of ZrP/NiSe₂ nanocomposite. In contrast, only small percentage of the pesticide (8.25%) was degraded in the absence of a photocatalyst, after 90 min of irradiation.

Furthermore, ZrP/NiSe₂ and ZrP can remove significant percentages of imidacloprid from aqueous solutions through adsorption (43.26% and 43.69%, respectively) under dark conditions (Fig. 6B). These results were predicted because the high adsorption affinity of ZrP toward organic pollutants with protonable groups has already been described.(6)

The effect of irradiation time on removal of imidacloprid in the presence of ZrP/NiSe₂ was also monitored. As expected, the imidacloprid concentration decreases by increasing the irradiation time (Fig. 6C). Nevertheless, when the irradiation time increases from 90 min to 105 min, there was no significant change in the concentration of imidacloprid (Fig. 6C).

The dosage of photocatalyst is a key factor that influence the percent removal of the pollutant. Therefore, the impact of ZrP/NiSe₂ dose on removal of the pesticide was also investigated. The increase in ZrP/NiSe₂ dose from 0.03 g to 0.05 g resulted in corresponding increase in percentage of imidacloprid removal (Table 1, Entry 7). However, further increasing ZrP/NiSe₂ dose to 0.07 g would only lead to a slight increase in the percentage of imidacloprid removal (Table 1, Entry 8).

The percent removal of the pesticide is affected by the initial concentration. As a result, the percentage removal of imidacloprid decreased with an increase in initial concentration from 10 to 20 ppm (Table 1, Entry 9).

In order to indicate the main active specie in the photodegradation of imidacloprid pesticide, the effects were evaluated when using isopropyl alcohol (IPA) as a hydroxyl radical scavenger, and p-benzoquinone (BQ) as a superoxide radical scavenger and EDTA as a hole scavenger. As shown in Fig. 6D, after the addition of IPA, an efficiency decrease in catalytic performance of ZrP/NiSe₂ was observed, indicating that the hydroxyl radicals play a vital role in the degradation of imidacloprid. Although, the addition of p-benzoquinone and EDTA did not affect imidacloprid removal significantly (Fig. 6D).

Table 1

Summary of the removal of imidacloprid in photocatalytic and photochemical systems within 90 min.
Entry	Photocatalyst	Catalyst dose (g)	Light source	Initial imidacloprid conc. (ppm)	Imidacloprid Removal [%]
1	ZrP/NiSe₂	0.05	Vis.	20	70.67
2	ZrP	0.05	Vis.	20	51.52
3	NiSe₂	0.05	Vis.	20	47.50
4	-	-	Vis.	20	8.25
5	ZrP/NiSe₂	0.05	-	20	43.26
6	ZrP	0.05	-	20	43.69
7	ZrP/NiSe₂	0.03	Vis.	20	49.28
8	ZrP/NiSe₂	0.07	Vis.	20	77.51
9	ZrP/NiSe₂	0.05	Vis.	10	79.63

The ZrP/NiSe₂ nanocomposite was recyclable without much loss of activity. After each, the ZrP/NiSe₂ nanocomposite separated from the reaction medium by centrifugation. The used catalyst was washed several times with water, dried at 50°C and further reused consecutively for 3 times. The ZrP/NiSe₂ nanocomposite showed 61.19% imidacloprid removal at 3th cycle (Fig. 7).

The ZrP/NiSe₂ nanocomposite was prepared with the purpose of creating recyclable catalytic system for removal of Imidacloprid pesticide from water. Detailed characterization results indicate the successful preparation of ZrP/NiSe₂ nanocomposite. Our results suggested the improved photocatalytic performance of ZrP/NiSe₂ nanocomposite. Furthermore, the ZrP/NiSe₂ nanocomposite can keep the good performance after three times of recycle.

Author Contribution

K.B. conceived the original idea and supervised the project. M.I. carried out the experiment. H.T helped supervise the project. M.I. and H.T. wrote the main manuscript text. All authors reviewed the manuscript.

Data Availability Statements

All data generated or analyzed during this study are included in this published article.

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No competing interests reported.

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You are reading this latest preprint version

Adsorptive and Photocatalytic Degradation of Imidacloprid Pesticide from Wastewater via the ZrP/NiSe 2 nanocomposite

Status:

Version 1

Abstract

Figures

Introduction

Experimental

Materials and apparatus

Synthesis of NiSe₂ nanoparticles

Synthesis of ZrP nanoparticles

Synthesis of ZrP/NiSe₂ nanocomposite

Photocatalytic degradation of imidacloprid

Results and discussion

Characterization of the photocatalysts

Photocatalytic degradation studies

Conclusion

Declarations

Author Contribution

Data Availability Statements

References

Additional Declarations

Status:

Version 1

Adsorptive and Photocatalytic Degradation of Imidacloprid Pesticide from Wastewater via the ZrP/NiSe 2 nanocomposite

Status:

Version 1

Abstract

Figures

Introduction

Experimental

Materials and apparatus

Synthesis of NiSe2 nanoparticles

Synthesis of ZrP nanoparticles

Synthesis of ZrP/NiSe2 nanocomposite

Photocatalytic degradation of imidacloprid

Results and discussion

Characterization of the photocatalysts

Photocatalytic degradation studies

Conclusion

Declarations

Author Contribution

Data Availability Statements

References

Additional Declarations

Status:

Version 1

Synthesis of NiSe₂ nanoparticles

Synthesis of ZrP/NiSe₂ nanocomposite