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Article

Photocatalytic Degradation of Four Organic Dyes Present in Water Using ZnO Nanoparticles Synthesized with Green Synthesis Using Ambrosia ambrosioides Leaf and Root Extract

by
Martin Medina-Acosta
1,
Manuel J. Chinchillas-Chinchillas
2,*,
Horacio E. Garrafa-Gálvez
3,
Caree A. Garcia-Maro
3,
Carlos A. Rosas-Casarez
2,
Eder Lugo-Medina
1,
Priscy A. Luque-Morales
4 and
Carlos A. Soto-Robles
1,*
1
Departamento de Ingeniería Química y Bioquímica, Tecnológico Nacional de México-IT de Los Mochis, Los Mochis C.P. 81259, Sinaloa, Mexico
2
Departamento de Ingeniería y Tecnología, Universidad Autónoma de Occidente, Los Mochis C.P. 81223, Sinaloa, Mexico
3
Facultad de Ingeniería Mochis, Universidad Autónoma de Sinaloa, Los Mochis C.P. 81223, Sinaloa, Mexico
4
Facultad de Ingeniería, Arquitectura y Diseño, Universidad Autónoma de Baja California, Ensenada C.P. 22860, Baja California, Mexico
*
Authors to whom correspondence should be addressed.
Processes 2024, 12(11), 2456; https://doi.org/10.3390/pr12112456
Submission received: 8 October 2024 / Revised: 22 October 2024 / Accepted: 30 October 2024 / Published: 6 November 2024
(This article belongs to the Special Issue Advances in the Photocatalysis and Photodegradation of Various Contaminants Present in Water)
Browse Figures
Figure 1
<p>FT-IR spectra of nanoparticles synthesized with <span class="html-italic">Ambrosia ambrosioides</span>.</p> "> Figure 2
<p>XRD spectra of ZnO nanoparticles synthesized with <span class="html-italic">Ambrosia ambrosioides</span> using: (<b>a</b>) root and (<b>b</b>) sheet.</p> "> Figure 3
<p>UV–Vis analysis of ZnO nanoparticles synthesized with <span class="html-italic">Ambrosia ambrosioides</span>: (<b>a</b>,<b>c</b>) absorbance of ZnO nanoparticles synthesized with root and leaf, respectively, and (<b>b</b>,<b>d</b>) bandgap calculation of ZnO nanoparticles synthesized with root and leaf, respectively.</p> "> Figure 4
<p>SEM morphology study of ZnO nanoparticles synthesized with <span class="html-italic">Ambrosia ambrosioides:</span> (<b>a</b>,<b>b</b>) Morphology of AA_R_ZnO nanoparticles, (<b>c</b>) size distribution of AA_R_ZnO, (<b>d</b>,<b>e</b>) Morphology of AA_S_ZnO nanoparticles and (<b>f</b>) size distribution of AA_S_ZnO.</p> "> Figure 5
<p>TEM morphology study of ZnO nanoparticles synthesized with <span class="html-italic">Ambrosia ambrosioides</span> extracts. (<b>a</b>,<b>b</b>) Morphology of AA_R_ZnO nanoparticles, (<b>c</b>) SAED of AA_R_ZnO, (<b>d</b>,<b>e</b>) Morphology of AA_S_ZnO nanoparticles and (<b>f</b>) SAED of AA_S_ZnO.</p> "> Figure 6
<p>TGA/DSC of the nanoparticles synthesized using <span class="html-italic">Ambrosia ambrosioides</span> extracts.</p> "> Figure 7
<p>Photocatalytic degradations of (<b>a</b>) MB, (<b>b</b>) MO, (<b>c</b>) CR and (<b>d</b>) MR using ZnO nanoparticles synthesized with <span class="html-italic">Ambrosia ambrosioides</span> extracts.</p> "> Figure 8
<p>Mechanism of photocatalytic degradation proposed by this research.</p> "> Figure 9
<p>Green synthesis process of ZnO nanoparticles using <span class="html-italic">Ambrosia ambrosioides</span>.</p> ">
Versions Notes

Abstract

:
Currently, several organic dyes found in wastewater cause severe contamination problems for flora, fauna, and people in direct contact with them. This research proposes an alternative for the degradation of polluting dyes using ZnO nanoparticles (NPs) synthesized by an ecological route using leaf and root extracts of Ambrosia ambrosioides as a reducing agent (with a weight/volume ratio = 4%). Scanning Electron Microscopy (SEM) was used to determine the morphology, showing an agglomeration of cluster-shaped NPs. Using Transmission Electron Microscopy (TEM), different sizes of NPs ranging from 5 to 56 nm were observed for both synthesized NPs. The composition and structure of the nanomaterial were analyzed by infrared spectroscopy (FT-IR) and X-ray diffraction (XRD), showing as a result that the NPs have a wurtzite-like crystalline structure with crystallite sizes around 32–37 nm for both samples. Additionally, the bandgap of the NPs was calculated using Ultraviolet Visible Spectroscopy (UV–Vis), determining values of 2.82 and 2.70 eV for the NPs synthesized with leaf and root, respectively. Finally, thermogravimetric analysis demonstrated that the nanoparticles contained an organic part after the green synthesis process, with high thermal stability for both samples. Photocatalytic analysis showed that these nanomaterials can degrade four dyes under UV irradiation, reaching 90% degradation for methylene blue (MB), methyl orange (MO) and Congo red (CR) at 60, 100 and 60 min, respectively, while for methyl red (MR) almost 90% degradation was achieved at 140 min of UV irradiation. These results demonstrate that it is effective to use Ambrosia ambrosioides root and leaf extracts as a reducing agent for the formation of ZnO NPs, also evidencing their favorable application in the photocatalytic degradation of these four organic dyes.

1. Introduction

Global water use has increased almost sixfold over the past 100 years [1]. In every human activity, water usage is essential, as it can result in wastewater and contamination. The textile industry requires large volumes of water in its production processes, typically using between 100 and 200 L to produce one kilogram of textile products [2]. Wastewater from this industry contains significant amounts of pollutants, various dyes, and different chemical compounds [3]. Dyes are generally organic compounds that impart color to other substances. Today, there are approximately 10,000 dyes on the market, with up to 700,000 tons of these synthetic compounds produced annually [4,5,6]. Currently, different methods are used for wastewater treatment, generally classified into physical, chemical, and biological methods [7]. The technologies that have been emphasized include coagulation, membrane treatment, advanced oxidation processes, biological treatment, and adsorption. Unfortunately, many of these processes are costly, generate environmentally harmful by-products, and are complex [8].
Due to their performance, characteristics, and advantages, one of the most widely used methods for treating these effluents is advanced oxidation processes (AOPs) [9], among which we find photocatalysis. Photocatalysis has proven to be a highly efficient, cost-effective, and straightforward procedure. It has attracted significant research interest due to its successful results in degrading organic pollutants, including industrial dyes. Among the organic dyes that cause high contamination rates are methylene blue (MB), methyl orange (MO), Congo red (CR) and methyl red (MR) [10,11,12,13]. For the photocatalysis process to work, a material is needed to perform the function of a photocatalyst [14]. It has been reported through research that nanoparticles have this characteristic, because photocatalysis involves the generation of highly reactive radicals, such as hydroxyl radicals and superoxide anions. They result from the interaction of photons with a semiconductor material in the presence of an aqueous solution or oxygen. For this reason, semiconducting nanoparticles have been used as photocatalysts due to their characteristic electronic structure. These semiconductor nanomaterials have two bands: the valence band (VB), which is the last orbital or energy level of the atoms occupied by electrons, and the conduction band (CB), formed by empty orbitals. The energy gap between the VB and CB is known as the bandgap. When stimulated by a photon of equal or higher energy than the forbidden bandgap, the VB absorbs the photon and an electron passes from the CB to the VB, generating excess positive charge in the VB of the nanomaterial called a ‘hole’. These photogenerated charges are called the electron–hole pair and are the interaction that migrates to the surface of the semiconducting material producing the radicals necessary for photocatalysis [15]. Therefore, the use of nanoparticles of semiconductor materials has been implemented in photocatalytic processes due to their high stability, adequate mechanical strength, high capacity for electron volume movement, and high area/volume ratio [16]. One of the semiconductors with the best photoelectric properties is ZnO, an n-type material with a bandgap of 3.37 eV and a binding energy of 60 meV, making it suitable for photocatalysis [17]. To synthesize nanoparticles, there are various methods such as physical, chemical and biological methods [18,19,20]. Green synthesis is a biological process and works by using biological organisms such as bacteria, actinobacteria, yeasts, molds, algae, microorganisms or plants. Plant extracts contain various organic molecules in their structure such as proteins, enzymes, phenolic compounds, amines, alkaloids and pigments. These organic molecules help to reduce the metal salt (precursor of semiconductor nanoparticles), which is the basic principle for the green synthesis process [21]. Worldwide, a wide variety of plants and fruits are available, and some have been used in green synthesis to obtain nanoparticles. Other authors have explored the green synthesis of ZnO nanoparticles using extracts from Myrtus Communis [22], Salvia fruticosa Mill. [23], Nauclea latifolia [24] and Platanus orientalis [25].
The use of Chicura (Ambrosia ambrosioides) in the green synthesis of nanoparticles with application to the degradation of water pollutants has not been reported. This plant is a shrubby ragweed widespread in the deserts of northern Mexico and can be found in areas such as roadsides, riverbanks, and sandy soil, and sometimes in hollows in the rocks themselves. Its main uses are for medicinal purposes, and it has been reported to have been used as a phytoremediator of contaminated soils [26]. Some studies have shown that Ambrosia ambrosioides has the characteristic of being a hyperaccumulator of heavy metals, with an essential content of flavonoids in different species and with the presence of organic compounds such as damsine and franserine [26,27]. This plant contains a variety of organic compounds that can act as reducing agents, with a good number of available groups in its structure capable of performing reduction. The aqueous extract was found to contain various compounds, including tannins, sugars, and carbohydrates (specifically ketoses) [27]. These compounds have functional groups with high reducing capacity, collectively contributing to the synthesis of ZnO nanoparticles. Therefore, it is an excellent candidate for use in the green synthesis of semiconductor nanoparticles.
In this research, ZnO nanoparticles were synthesized by green synthesis using Ambrosia ambrosioides leaf and root extracts at a concentration of 4% relative to the aqueous solution. The synthesized material was characterized using FT-IR, XRD, SEM, TEM/SAED and UV–Vis techniques to determine their bandgap. Furthermore, these synthesized ZnO nanoparticles were employed in the degradation of four organic dyes—MB, MO, CR and MR—through photocatalysis analysis.

2. Results and Discussion

2.1. FT-IR Analysis of the ZnO Nanoparticles

The analysis of the infrared spectrum revealed very important information about the samples because it helps to know the biological molecular fingerprint of the samples and to identify the functional groups in the infrared electromagnetic region found in the samples [28]. Figure 1 shows the results of the molecular vibrations of the nanoparticles synthesized with Ambrosia ambrosioides. It should be noted that no significant effect is observed between the two infrared spectra of the samples. Three zones represented by blue, green and black colors are observed. In the first zone, identified with blue, a slight peak is observed at 3751 cm−1, attributed to the vibrations of the O-H groups, which can be associated with the adsorption of the water molecules present in the analyzed samples [29,30]. The green-colored zone represents the vibration of the organic molecules present in the natural extract used in the green synthesis. Research has reported that after the synthesis of the nanoparticles, the organic molecules of the natural extract are retained in the surface area of the nanomaterial, bringing about better material stability and influencing the size [31]. The two nanoparticle samples present a vibrational band at 1380 cm−1, which is associated with the product of the bending of the C-H bonds of organic molecules present in the phytochemicals of the Ambrosia ambrosioides natural extract, such as flavonoids or phenolic compounds [32]. In the study by MuthuKathija et al., signals of carboxylic groups, carbonyl groups, amides, amines, and aromatic rings were found after the synthesis process, originating from the Pisonia alba extract used for the synthesis of ZnO nanoparticles [33]. Given that both samples have a concentration of 4% of the extract, it is observed that the AA_S_ZnO sample probably contains a slightly higher number of organic molecules as it presents a wider and more extensive band. Finally, the vibration peak present at 400 cm−1 corresponds to metallic bonds such as Zn-O [34,35]. This value is very similar to that reported by Karthik et al. in 2022 [36]. These results present the characteristic molecular vibrations of the green synthesis of ZnO nanoparticles using Ambrosia ambrosioides. Furthermore, it shows relative purity as it does not show absorption peaks in uncharacteristic regions.

2.2. XRD Analysis of the ZnO Nanoparticle

The X-ray diffraction study is shown in Figure 2, where the Miller indices denoting the crystalline phase of the ZnO nanoparticles synthesized with Ambrosia ambrosioides can be observed. The most intense diffraction peaks are found at 28.29°, 31.68°, 34.37°, 36.21°, 40.47°, 47.54°, 56.64°, 62.89° and 67.97°. These peaks correspond to the following Miller indices: (200), (100), (002), (101), (220), (102), (110), (103) and (112), respectively [37]. Analyzing the International Centre for Sample Preparation Methods cards of powder X-ray diffraction data (JCPDS), these indices correspond to a hexagonal wurtzite-type structure of ZnO [38]. It is worth noting that both diffractograms (AA_R_ZnO and AA_S_ZnO) present a similarity in the diffracted peaks, unlike the peaks shown at 28.29° and 40.47°. These two peaks, shown in the ZnO nanoparticles with Ambrosia ambrosioides root, can be attributed to the presence of organic substances coating the surface of ZnO-NPs [39]. This is because, as mentioned by Maathuis, F. J., and Sanders in 1996, based on studies carried out where it was concluded that the plant under study was a hyperaccumulator of metals [26], ZnO could be absorbed by the root of the plant [40]. On the other hand, the average crystallite size of the nanoparticles was obtained using Scherrer’s formula, analyzing the average of the three most intense peaks of the diffractograms using Equation (1) [41].
D = K λ B C o s θ
where D corresponds to the average physical size of the crystallite in the diffraction peaks, B refers to the bandwidth of the three most intense peaks, θ is the diffraction angle at each peak considered, λ is the wavelength of the X-ray source and K is a dimensionless constant. The results show that the AA_R_ZnO and AA_S_ZnO nanoparticles had sizes of 36.7 nm and 32.5 nm, respectively. The size difference that exists between the two analysis samples can be attributed to the number of photochemical agents in the root and leaf [42].

2.3. UV–Vis Analysis and Bandgap Calculation

Figure 3 shows the bandgap value obtained for the AA_S_ZnO and AA_R_ZnO nanoparticles. It is very important to know the value of the energy required for an electron to pass from the valence band to the conduction band [43]. The calculation of these values was determined using the TAUC model following Equation (2) and analyzing the UV–Vis spectra of the ZnO nanoparticles.
α v h v = K h v − E g n
where α v corresponds to the absorption coefficient (Lambert–Beer), h v is the incident photon energy, K is a band tail constant, E g is the bandgap energy and n = corresponds to the allowed direct transition for semiconductors [44,45]. The calculated bandgap values were 2.82 and 2.70 eV, which correspond to the AA_R_ZnO and AA_S_ZnO samples, respectively. As can be seen, the bandgap of the AA_S_ZnO sample is lower than the AA_R_ZnO sample; this indicates that the sample synthesized with Ambrosia ambrosioides leaf needs less energy to cause electron hopping (from the valence layer to the conduction layer) compared to commercial ZnO nanoparticles, which would help to increase the photocatalytic properties. This aligns with Mousa et al., who determined that this occurs due to the interaction of the organic contents with the ZnO nanoparticles, causing defects such as interstitial vacancies and anionic or cationic vacancies [46].
It has been reported in the literature that ZnO nanoparticles in their pure state have bandgap values of around 3.3 eV [47]. It can be determined that there is a difference between the bandgap energy of the study samples and the nanoparticles in their pure state, demonstrating that the natural extracts of Ambrosia ambrosioides were able to modify the electronic properties of the nanomaterial. This is attributed to the effect of the organic molecules in the extract, which are functionalized on the surface of the material, affecting the energy required to achieve electron stimulation. Sai Kumar Tammin in 2017 reported that the organic molecules of the natural extracts used in green synthesis act as photosensitizers [48].

2.4. Morphological Analysis by SEM and TEM/SAED

To determine the morphology of the ZnO nanoparticles synthesized with Ambrosia ambrosioides, SEM analysis was used, which is presented in Figure 4. The morphology of the sample AA_R_ZnO is observed, showing some agglomerations. Enlarging the image (Figure 4b), uniform zones with hemispherical clusters on a micrometric scale around 5 µm can be seen. A size distribution was performed using 100 measurements with ImageJ software (version 1.53e), finding that the nanoparticle clusters have average sizes of 841 nm (Figure 4c). On the other hand, the AA_S_ZnO sample showed a morphology with non-uniform shapes, with some agglomerations and very different sizes of nanoparticle clusters (Figure 4d,e). The average size of the clusters was 863 nm (Figure 4f). The extracts used in this investigation had significant effects on the shape of the synthesized nanomaterial. The morphology presented in the two samples of the study shows a grouping of a large amount of nanoparticles, called agglomerated nanoparticles, based on what is reported in other research such as that of F. Davar in 2015 [49]. On the other hand, to perform a more detailed analysis of the shape and sizes of the nanoparticles synthesized in this study with Ambrosia ambrosioides, TEM/SAED analysis was performed, which is presented in Figure 5. In this analysis, it can be observed that the study nanoparticles have different sizes and shapes. The samples synthesized with Ambrosia ambrosioides root (AA_R_ZnO) showed some irregular shapes, and others were in crystal shapes (Figure 5a). Moreover, in Figure 5a,b, sizes smaller than 10 nm and up to 56 nm are observed. On the other hand, the nanoparticles synthesized with Ambrosia ambrosioides (AA_S_ZnO) leaf showed mostly quasi-spherical shapes (Figure 5d) and sizes smaller than 10 nm and up to 51 nm (Figure 5d,e).
To identify and explore the crystalline nature of the synthesized ZnO nanoparticles, selected area electron diffraction (SAED) analysis was performed and is shown in Figure 5c,f, corresponding to the sample of AA_R_ZnO and AA_S_ZnO, respectively. The halos presented in the SAED pattern reflect the polycrystalline nature of the nanoparticles and the (100), (002), (101), (102) and (110) reflections, which correspond to the wurtzite structure and agree with the XRD analysis presented in Figure 2 [50]. These results demonstrate the obtaining of particles that are in the nanometric scale and indicate that the leaf and root extracts do not show significant differences in the formation of the size and shape of the ZnO nanoparticles synthesized with Ambrosia ambrosioides.

2.5. Thermogravimetric Analysis (TGA/DSC)

The thermal behavior of ZnO nanoparticles synthesized using 4% of Ambrosia ambrosioides leaf and root is shown in Figure 6. It can be observed that the thermal behavior of both samples is similar. Both nanoparticles samples showed a loss between 120 and 200 °C, which corresponds to the absorbed water or the water molecules chemically bound to the natural extract [51]. The weight loss in this zone was 5% for the AA_R_ZnO sample and 7% for AA_S_ZnO. Increasing the temperature in the analysis zone from 250 to 450 °C resulted in a very significant weight loss for both samples. AA_R_ZnO showed a loss of 27%, and the AA_S_ZnO nanoparticles showed a loss of approximately 23%. Some authors have reported that the loss in this zone is attributed to the degradation of the organic molecules that are functionalized in the nanoparticles after the green synthesis process and to the calcination of free Zn+2 species that did not react [52]. After this zone, the weight loss in both samples is slow. Using this technique, it was possible to identify that the organic molecules used in the green synthesis process are part of the ZnO nanoparticles through possible functionalization.

2.6. Photocatalytic Degradations

The study of the photocatalytic activity of the nanoparticles synthesized with Ambrosia ambrosioides in the degradation of four organic dyes (MB, MO, CR and MR) is shown in Figure 7. This process was carried out under UV radiation, and subsequently, the absorbance and/or concentration of the pollutant was analyzed with UV–Vis spectroscopy equipment. For all study samples, the adsorption–desorption equilibrium was evaluated by stirring the solutions in the dark for 30 min.
Figure 7a corresponds to the degradation of MB, and the two samples (AA_S_ZnO and AA_R_ZnO) were analyzed at the absorption peak at 661 nm [10]. The degradations of the two samples showed very similar results. The adsorption percentage was 11% for sample AA_S_ZnO and 5% for sample AA_R_ZnO. The nanoparticles showed an efficient degradation of the dye during the first hour of exposure (60 min), where a degradation of 90% was achieved. After this time interval, the photocatalytic process was slower, achieving a complete degradation at approximately 120 min for both study samples. On the other hand, the analysis of the photocatalytic degradation of MO can be observed in Figure 7b, where the absorption band at the wavelength of 460 nm characteristic of this dye was identified [11,53]. For both study samples, a low adsorption–desorption percentage of approximately 0.5% was observed. Analyzing the degradation of the pollutant as a function of irradiation time, it can be observed that the ZnO nanoparticles had a significant effect on the degradation of the dye. The first 60 min of exposure caused a high decrease in the dye concentration (83% for AA_R_ZnO and 75% for AA_S_ZnO). Degradation above 90% was achieved after 100 min for both samples.
The results of the photocatalytic degradation of CR are presented in Figure 7c. The absorption of this dye was presented at 494 nm and was used as a reference to determine the degradation of the dye [12]. ZnO nanoparticles synthesized with Ambrosia ambrosioides showed a high decrease in dye concentration upon stirring in the dark. This indicates that the dye is adsorbed on the surface of the nanoparticles. The results showed an adsorption in the dark of 34% for the AA_R_ZnO sample and 49% for the AA_S_ZnO nanoparticles. This is attributed to the nature of the dye, which, being an anionic dye, generates a high electrostatic interaction with the nanomaterial, as well as the physical interaction between the oxygen groups of the ZnO and the functional groups of the dye [31,54] . Degradation results above 90% were achieved at 60 min of exposure for the AA_R_ZnO sample and at 20 min for the AA_S_ZnO nanoparticles.
For the MR dye, degradation was determined based on the peak present at 424.5 nm of the dye [55]. Figure 7d shows that the adsorption of both nanoparticle samples is low, with a percentage of 3.74% and 5.60% for AA_R_ZnO and AA_S_ZnO, respectively. The degradation of MR as a function of exposure time presented degradation percentages of 63.24% and 39.85% at 60 min using the AA_S_ZnO and AA_R_ZnO samples, respectively. The final degradation of the study for this dye presented a degradation percentage higher than 90% at 140 min for the AA_S_ZnO sample and 93% at 200 min with the AA_R_ZnO sample. The results of the photocatalytic activity in the degradation of the four organic dyes present in this research can be seen in Table 1, in addition to the results of other research reported in the literature.

2.7. Reaction Mechanism

The photocatalytic degradation of the four dyes presented in this work is depicted in Figure 8. This model describes in detail the degradation process of the organic dyes with photocatalysis processes. The degradation starts when the contaminated solution is irradiated with solar or UV energy. In this research, UV energy was used by means of the polaroid reactors described in the methodology section. This irradiated energy has wavelengths longer than the bandgap energy of the study samples: 2.82 eV for sample AA_R_ZnO and 2.70 eV for sample AA_S_ZnO (result observable in Figure 3). When the UV energy interacts with the ZnO nanoparticles dispersed in the contaminated solution, an excited state occurs in the nanoparticles (photon absorption Equation (3)), allowing the electrons in the valence layer to migrate to the conduction layer [68]. This process produces an electron ( e c b − ) hole ( h v b + ) , which tends to recombine to achieve its basal state. If this does not occur (recombination), these species ( e c b − y h v b + ) cause redox reactions in the medium in which they are found ( H 2 O ) [69]. The h v b + oxidizes water, producing hydroxyl radicals ( O H * ), and the e c b − reduces oxygen-generating superoxide radicals ( O 2 − * ). This process is observed in Equation (4). The •OH− and O2•− interact with the bonds of the organic dye molecules, mineralizing them until H2O and CO2 are obtained as residues (Equations (5) and (6)) [70].
Z n O + h v   →   h v b + + e c b −   ( Z n O )
h v b + + O H −   →   O H *   a n d   e c b − + O 2   → O 2 − *
D y e + O H * →   I n t e r m e d i a t e   m o l e c u l e s →   m i n e r a l i z a t i o n   ( H 2 O ,   C O 2 ,   e t c . )
D y e + H + →   I n t e r m e d i a t e   m o l e c u l e s →   m i n e r a l i z a t i o n   ( H 2 O ,   C O 2 ,   e t c . )

3. Materials and Methods

3.1. Materials

For the green synthesis of ZnO nanoparticles, root extracts and totally dried leaves of Ambrosia ambrosioides obtained from a local market in Los Mochis, Sinaloa, Mexico, were used as reducing agents. Zinc nitrate [Zn(NO3)2 × 6H2O] from Sigma Aldrich (Toluca, México) was used as a precursor agent, and distilled water obtained from FagaLab in Los Mochis, Sinaloa, Mexico, was used as a solvent. The dyes used in this research were obtained from Sigma Aldrich. The amounts of dyes were as follows: MB of 373.9 g/mol, MO of 327.34 g/mol, RC of 696.66 g/mol and RM of 269.30 g/mol.

3.2. Obtaining the Extract

Two extracts were prepared, one from the root of Ambrosia ambrosioides and one from the leaf of Ambrosia ambrosioides. For this preparation, the roots and leaves were dried in a food dryer for 12 h and then pulverized using a six-blade domestic blender. Then, 2 g of each material was weighed and placed together with 50 mL of distilled water (weight/volume ratio = 4%). The solutions were magnetically stirred for 2 h at room temperature (medium temperature = 30 °C). Once the stirring time was over, the solutions were placed in a water bath at 60 °C for one hour, and finally, each solution was filtered with Whatman #4 filter paper (Sigma Aldrich, Toluca, México) to remove organic material from the solutions, leaving extracts free of organic matter and solid impurities.

3.3. Green Synthesis of ZnO Nanoparticles

For the synthesis of ZnO nanoparticles, the methodology reviewed by Jun Xu et al. in 2021 [71] was followed. It was necessary to weigh two grams of the metallic Zn precursor and place this material in 50 mL of the extracts obtained from the previous process (4% extracts of root and leaf). The solution was stirred for one hour and then placed in a water bath for 14 h until a pasty (viscous) consistency of the solutions was obtained. The product obtained was then placed in porcelain capsules, distributing it as well as possible with a spatula over the entire inner surface of the capsules. The porcelain capsules were then placed in a heat treatment in a flask at 350 °C for 150 min. Finally, the material resulting from the heat treatment was manually crushed and stored. The samples were identified as AA_S_ZnO, corresponding to the ZnO nanoparticles obtained with the leaf extract (AA = Ambrosia ambrosioides and S = Sheet), and AA_R_ZnO for the nanoparticles obtained with a root extract of Ambrosia ambrosioides (R = Root). The process described can be seen in Figure 9.

3.4. Characterization of the Nanoparticles

The nanoparticles obtained were characterized using various characterization techniques. PerkinElmer FT-IR equipment (Brand equipment, Waltham, MA, USA) with a resolution of 0.5 cm−1 was used, and compressed powders of ZnO nanoparticles were used to form a tablet. An XRD diffractometer with Bruker-D2 Phase equipment (Billerica, MA, USA) was employed at 30 kV and 10 mA using 200 mg of ZnO nanoparticles powders. For the UV–Vis spectrophotometry study, a PerkinElmer Lambda 365 model instrument was used at a resolution of 600 nm/min; a solution of 5 mg of ZnO nanoparticles was made in deionized water and dispersed using ultrasound for 3 min. These three analyses were carried out at the Autonomous University of Baja California, Ensenada Campus. Morphology was analyzed using SEM analysis with a JEOL instrument (model JSM-6310LV of Tokyo, Japan) at a working distance of 10 mm. TEM analysis was performed with JEOL equipment (model JEM-2100) at an acceleration of 120 kV, and the ZnO nanoparticles were deposited on a copper grid to be observed.

3.5. Photocatalytic Test

The photocatalytic activity of ZnO nanoparticles synthesized with Ambrosia ambrosioides extracts was performed with the following methodology. As a first step, it was necessary to prepare different pollutants found in wastewater from the textile industry. Four different dyes (MB, MO, CR and RM) were prepared in 50 mL of deionized water, with a concentration of 15 ppm. Next, 50 mg of ZnO nanoparticles synthesized with Ambrosia ambrosioides was added to each of the contaminated solutions. The solutions were shaken in the dark for 30 min (adsorption–desorption equilibrium) at room temperature (medium temperature = 30 °C) and a neutral pH. Afterwards, the photocatalytic activity was recorded under UV radiation using Polaris UV-2C reactors with a 14 W lamp. Once the process was started, samples were taken at intervals every 20 min, and measurements were stopped once colorless samples were visually observed. Subsequently, the absorbance was evaluated by a UV–Vis spectrophotometer with a maximum absorbance of 664 nm for MB, 460 nm for MO, 496 nm for CR and 428 nm for MR to determine the degradation percentages of the contaminated solutions (following the Equation (7)).
D e g r a d a t i o n   e f f i c i e n c y % = ( C 0 − C f C 0 ) × 100

4. Conclusions

The results showed that the use of Ambrosia ambrosioides extracts as a reducing agent for the green synthesis of ZnO nanoparticles was successful, and the organic composition present in the nanoparticles synthesized with root and leaf extracts showed a high similarity. A similar morphology, size and structure were determined, as well as bandgaps of 2.82 and 2.70 eV for the nanoparticles synthesized with root and leaf extracts, respectively. With these results, the excellent photocatalytic degradation of four different organic dyes was obtained, thus contributing to the need to broaden the range of applications for these nanomaterials, which are obtained by innovative techniques that are environmentally friendly and energy-efficient. This addresses an important problem for our society today: water pollution. This research serves as a foundation for continuing to experiment in the laboratory with various variables, processes, and more specific tests, as well as for scalability analysis studies, with the aim that this technology can be applied directly in the field on an industrial scale in a short period of time.

Author Contributions

M.M.-A.: Methodology, formal analysis and writing—original draft; M.J.C.-C.: Conceptualization, investigation and resources and writing—review and editing; H.E.G.-G.: visualization, validation and formal analysis and data curation; C.A.G.-M.: investigation, visualization and software; C.A.R.-C.: Conceptualization, data curation and Methodology; E.L.-M.: software, investigation and resources; P.A.L.-M.: investigation and resources, supervision and project administration; and C.A.S.-R.: visualization, project administration and funding acquisition. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Data Availability Statement

Data are contained within the article.

Acknowledgments

The authors thank M. Castro-Sandoval for their support in the development of this research. May they rest in peace. The authors would like to thank the Universidad Autónoma de Occidente, Unidad Regional Los Mochis, and the PIFIP 2024 Project. They would also like to thank the Universidad Autónoma de Baja California (Ensenada), the Universidad Autónoma de Sinaloa (Mochis), and the Tecnológico Nacional de México (Mochis) for their support in the development of this research.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. FT-IR spectra of nanoparticles synthesized with Ambrosia ambrosioides.
Figure 1. FT-IR spectra of nanoparticles synthesized with Ambrosia ambrosioides.
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Figure 2. XRD spectra of ZnO nanoparticles synthesized with Ambrosia ambrosioides using: (a) root and (b) sheet.
Figure 2. XRD spectra of ZnO nanoparticles synthesized with Ambrosia ambrosioides using: (a) root and (b) sheet.
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Figure 3. UV–Vis analysis of ZnO nanoparticles synthesized with Ambrosia ambrosioides: (a,c) absorbance of ZnO nanoparticles synthesized with root and leaf, respectively, and (b,d) bandgap calculation of ZnO nanoparticles synthesized with root and leaf, respectively.
Figure 3. UV–Vis analysis of ZnO nanoparticles synthesized with Ambrosia ambrosioides: (a,c) absorbance of ZnO nanoparticles synthesized with root and leaf, respectively, and (b,d) bandgap calculation of ZnO nanoparticles synthesized with root and leaf, respectively.
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Figure 4. SEM morphology study of ZnO nanoparticles synthesized with Ambrosia ambrosioides: (a,b) Morphology of AA_R_ZnO nanoparticles, (c) size distribution of AA_R_ZnO, (d,e) Morphology of AA_S_ZnO nanoparticles and (f) size distribution of AA_S_ZnO.
Figure 4. SEM morphology study of ZnO nanoparticles synthesized with Ambrosia ambrosioides: (a,b) Morphology of AA_R_ZnO nanoparticles, (c) size distribution of AA_R_ZnO, (d,e) Morphology of AA_S_ZnO nanoparticles and (f) size distribution of AA_S_ZnO.
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Figure 5. TEM morphology study of ZnO nanoparticles synthesized with Ambrosia ambrosioides extracts. (a,b) Morphology of AA_R_ZnO nanoparticles, (c) SAED of AA_R_ZnO, (d,e) Morphology of AA_S_ZnO nanoparticles and (f) SAED of AA_S_ZnO.
Figure 5. TEM morphology study of ZnO nanoparticles synthesized with Ambrosia ambrosioides extracts. (a,b) Morphology of AA_R_ZnO nanoparticles, (c) SAED of AA_R_ZnO, (d,e) Morphology of AA_S_ZnO nanoparticles and (f) SAED of AA_S_ZnO.
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Figure 6. TGA/DSC of the nanoparticles synthesized using Ambrosia ambrosioides extracts.
Figure 6. TGA/DSC of the nanoparticles synthesized using Ambrosia ambrosioides extracts.
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Figure 7. Photocatalytic degradations of (a) MB, (b) MO, (c) CR and (d) MR using ZnO nanoparticles synthesized with Ambrosia ambrosioides extracts.
Figure 7. Photocatalytic degradations of (a) MB, (b) MO, (c) CR and (d) MR using ZnO nanoparticles synthesized with Ambrosia ambrosioides extracts.
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Figure 8. Mechanism of photocatalytic degradation proposed by this research.
Figure 8. Mechanism of photocatalytic degradation proposed by this research.
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Figure 9. Green synthesis process of ZnO nanoparticles using Ambrosia ambrosioides.
Figure 9. Green synthesis process of ZnO nanoparticles using Ambrosia ambrosioides.
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Table 1. Reports on the degradation of MB, MO, CR, and MR using ZnO.
Table 1. Reports on the degradation of MB, MO, CR, and MR using ZnO.
YearExtractNanoparticleDegraded DyePercentage Degradation (%)Time (min)Reference
2024Ambrosia ambrosoidesZnOMB9060This work
2024Ambrosia ambrosoidesZnOMO92100This work
2024Ambrosia ambrosoidesZnOCR9060This work
2024Ambrosia ambrosoidesZnOMR90140This work
2023Citrus jambhiri lushiZnOMB100120[56]
2024Vachellia niloticaZnOMO8090[57]
2024Gum arabicZnOCR9930[58]
2024Zingiber officinaleZnOMR88120[59]
2024Rosa rubiginosaZnOMB99240[60]
2023Cystoseira criniteZnOMO88200[61]
2024Epipremnum aureumZnOCR69100[62]
2023Kaolin clayZnOMR9910[63]
2022Thymus vulgarisZnOMB10020[64]
2022Wild oliveZnOMO9290[65]
2023Carica papayaZnOCR10080[66]
2023Borreria hispidaZnOMR9440[67]
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MDPI and ACS Style

Medina-Acosta, M.; Chinchillas-Chinchillas, M.J.; Garrafa-Gálvez, H.E.; Garcia-Maro, C.A.; Rosas-Casarez, C.A.; Lugo-Medina, E.; Luque-Morales, P.A.; Soto-Robles, C.A. Photocatalytic Degradation of Four Organic Dyes Present in Water Using ZnO Nanoparticles Synthesized with Green Synthesis Using Ambrosia ambrosioides Leaf and Root Extract. Processes 2024, 12, 2456. https://doi.org/10.3390/pr12112456

AMA Style

Medina-Acosta M, Chinchillas-Chinchillas MJ, Garrafa-Gálvez HE, Garcia-Maro CA, Rosas-Casarez CA, Lugo-Medina E, Luque-Morales PA, Soto-Robles CA. Photocatalytic Degradation of Four Organic Dyes Present in Water Using ZnO Nanoparticles Synthesized with Green Synthesis Using Ambrosia ambrosioides Leaf and Root Extract. Processes. 2024; 12(11):2456. https://doi.org/10.3390/pr12112456

Chicago/Turabian Style

Medina-Acosta, Martin, Manuel J. Chinchillas-Chinchillas, Horacio E. Garrafa-Gálvez, Caree A. Garcia-Maro, Carlos A. Rosas-Casarez, Eder Lugo-Medina, Priscy A. Luque-Morales, and Carlos A. Soto-Robles. 2024. "Photocatalytic Degradation of Four Organic Dyes Present in Water Using ZnO Nanoparticles Synthesized with Green Synthesis Using Ambrosia ambrosioides Leaf and Root Extract" Processes 12, no. 11: 2456. https://doi.org/10.3390/pr12112456

APA Style

Medina-Acosta, M., Chinchillas-Chinchillas, M. J., Garrafa-Gálvez, H. E., Garcia-Maro, C. A., Rosas-Casarez, C. A., Lugo-Medina, E., Luque-Morales, P. A., & Soto-Robles, C. A. (2024). Photocatalytic Degradation of Four Organic Dyes Present in Water Using ZnO Nanoparticles Synthesized with Green Synthesis Using Ambrosia ambrosioides Leaf and Root Extract. Processes, 12(11), 2456. https://doi.org/10.3390/pr12112456

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