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Article

Performance of CuTiO3 Photocatalytic Oxidation for Treating Organic Peroxide Production Wastewater Under Visible Light

by
Zichun Yan
1,2,3,*,
Hongfu Li
1,
Hao Yang
1,2,3 and
Shuo Li
1
1
School of Environmental and Municipal Engineering, Lanzhou Jiaotong University, Lanzhou 730070, China
2
Key Laboratory of Yellow River Water Environment of Gansu Province, Lanzhou 730070, China
3
Ministry of Education Engineering Research Center of Water Resource Comprehensive Utilization in Cold and Arid Regions, Lanzhou 730070, China
*
Author to whom correspondence should be addressed.
Sustainability 2026, 18(2), 983; https://doi.org/10.3390/su18020983
Submission received: 22 September 2025 / Revised: 13 January 2026 / Accepted: 16 January 2026 / Published: 18 January 2026
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Abstract

To investigate the treatment performance of a CuTiO3 photocatalytic system for organic peroxide production wastewater under visible light, CuTiO3 powder prepared through the hydrothermal method was used for this experiment. The light absorption properties of the CuTiO3 catalyst were analyzed using Uv-Vis diffuse reflectance spectroscopy (Uv-Vis DRS). The effects of the initial pH, photocatalyst dosage, light intensity, and reaction duration on the photocatalytic reaction were examined. Before and after the reaction, the changes in pollutant components in water were characterized via three-dimensional excitation–emission matrix fluorescence spectrometry (3D-EEM) and gas chromatography–mass spectrometry (GC-MS); the changes in the concentrations of some pollutants were analyzed via wavelength scanning. The results indicated that CuTiO3 has a good response to visible light. Under the optimized conditions (initial pH = 5, CuTiO3 dosage = 1.2 g/L, light intensity = 1300 W/m2, duration = 4 h), the COD removal rate reached 58%, and the B/C (BOD5/COD) ratio of wastewater increased from 0.112 to 0.221, demonstrating a good pretreatment effect. GC-MS analysis demonstrated significant degradation effects on amide and hydride substances. Radical capture experiments verified hydroxyl radicals as the dominant species in CuTiO3 photocatalysis. Visible-light photocatalysis using CuTiO3 provides an efficient pretreatment pathway for organic peroxide production wastewater.

1. Introduction

Organic peroxides are widely used as catalysts and initiators for free radical polymerization [1], with applications spanning polymer materials and the film, medical materials, textiles, paper, and daily chemical industries [2]. With the continuous expansion of industry, the demand for organic peroxides is steadily increasing [3]. However, the production of organic peroxides generates large volumes of wastewater containing specific contaminants like tert-butyl peroxide. These contaminants impart characteristics to the wastewater such as an irritating odor, high toxicity, high Chemical Oxygen Demand (COD) concentration, and low biodegradability [1,4]. This makes their subsequent treatment exceedingly challenging, and improper handling can lead to persistent hazards [5]. Meanwhile, these characteristics make such wastewater challenging to directly treat using conventional biological methods. Pretreatment is therefore essential for removing pollutants that are difficult to degrade and improving biodegradability [6,7,8]. Common pretreatment technologies for such wastewater include Fenton oxidation [9], catalytic ozonation [10], and iron–carbon micro-electrolysis [1]. Due to its ability to efficiently degrade pollutants and broad applicability, photocatalysis is emerging as a promising technology for environmental remediation [11,12,13,14]. For instance, Mahalingam et al. successfully synthesized a visible-light-responsive G-CuO-Co3O4 photocatalytic and demonstrated its efficacy in degrading dye wastewater via a visible-light photocatalyst, achieving excellent removal efficiency within 300 min [15]. Bukhari et al. utilized nickel-doped graphitic carbon nitride (x-NGCN) to degrade methylene blue dye under LED white light, confirming its superior photocatalytic activity [16]. Wu et al. employed natural sphalerite as a catalyst for the visible-light photocatalytic treatment of mineral processing wastewater, significantly reducing organic content [17]. Concurrently, the development of economical, reliable, and photocatalysts has been a research hotspot [18,19,20,21]. CuTiO3, as a typical bimetallic oxide, has attracted attention for visible-light photocatalysis due to its suitable electronic band structure, narrow bandgap, and excellent chemical stability [22,23]. Despite this progress, research specifically dedicated to visible-light photocatalytic oxidation technology for treating organic peroxide production wastewater remains lacking. Current pretreatment processes also face challenges like high costs [24] and limited effectiveness [1]. Developing cost-effective technologies is crucial for the effective purification of organic peroxide production wastewater. In order to prevent the severe harm to aquatic environments caused by the discharge of organic peroxide-production wastewater, this study employed a hydrothermal synthesis method to prepare a visible-light-responsive CuTiO3 photocatalyst. The photocatalytic efficiency of CuTiO3 for treating organic peroxide production wastewater under visible-light irradiation was investigated. This research represents the first application of visible-light photocatalysis for treating organic peroxide production wastewater, offering pioneering insights and approaches for utilizing CuTiO3 in remediation.

2. Materials and Methods

2.1. Chemicals and Wastewater

The chemicals used in the experiment, including Cu(NO3)2·3H2O, H2SO4, NaOH, and AgNO3, were supplied by Tianjin Damao Chemical Reagent Co., Ltd. (Tianjin, China). Ti(OC4H9)4, tert-butanol, EDTA-2Na, and chloroform were obtained from Zhiyuan Chemical Reagent Co., Ltd. (Tianjin, China). All chemicals were of analytical reagent (AR) grade.
The wastewater used for the experiment was obtained from an auxiliary agent plant in Lanzhou, China. The plant mainly produces organic peroxides, dispersing agents, initiators, surfactants, polymerization inhibitors, and other products. Raw materials primarily include tert-butyl hydroperoxide, sodium hydroxide, neopentyl alcohol, neodecanoic acid, chloroformates, etc. The wastewater contains raw materials, intermediate products, and final products, with specific pollutants such as tert-butyl hydroperoxide, along with various refractory organic compounds, including amines and heterocyclic substances. The wastewater during the experiment exhibited a COD concentration ranging from 9764.6 mg/L to 18,289.8 mg/L and a pH ranging from 4.47 to 6.26.

2.2. Preparation of CuTiO3

The procedure for CuTiO3 is as follows: 2.33 g Cu(NO3)2·3H2O was added to 40 mL of water and stirred (HJ-1, Changzhou Surui Instrument, Changzhou, China) for 20 min until completely dissolved. While continuing stirring, 3.4 mL Ti(OC4H9)4 and 0.4 g NaOH were added; the molar stoichiometric ratio of Cu:Ti:Na was maintained at 1:1:1 and stirring continued for 30 min until the solution was fully homogenized. The mixture was then transferred to a 50 mL polytetrafluoroethylene (PTFE) reactor and reacted at 200 °C for 24 h to obtain the precursor solution. After taking out the reactor, the solution was cooled to ambient temperature. The precursor solution was centrifuged, separated, and washed twice with a 95% ethanol solution. The washed precursor was dried at 60 °C for 10 h. Finally, the precursor was placed in a muffle furnace, heated to 600 °C, and allowed to cool naturally to indoor temperature. The product was thoroughly ground to obtain the desired sample [22,23]. The preparation procedure is illustrated in Figure 1.

2.3. Properties of Photocatalyst

The light absorption intensity and absorption range of the catalyst within the 200–800 nm wavelength region were characterized using a Uv-Vis diffuse reflectance spectrophotometer (UV-3600 Plus, Shimadzu, Kyoto, Japan) equipped with an integrating sphere to analyze its light absorption properties.
The surface morphology of the catalyst was observed using a scanning electron microscope (GeminiSEM 500, Carl Zeiss AG, Oberkochen, Germany). Prior to imaging, the catalyst was sputter-coated with gold to enhance surface conductivity, and an accelerating voltage of 12 kV was applied during observation.

2.4. Experimental Procedure for Photocatalytic Degradation of Organic Peroxide Production Wastewater

The performance of the prepared CuTiO3 was evaluated by the COD removal rate of organic peroxide production wastewater through visible-light photocatalysis. The experiment utilized a batch photoreactor (480 mL, short beaker with a diameter of 12 cm and a height of 6 cm) equipped with a magnetic stirrer as the reaction vessel. The experiment first needed CuTiO3 to reach adsorption saturation in a dark environment. Subsequently, different dosages of CuTiO3 were introduced into 200 mL wastewater samples, followed by controlled irradiation using a 300 W xenon lamp (H3, Cnlight, Foshan, China) positioned 15 cm above the liquid surface and equipped with a 420 nm cutoff filter to selectively transmit visible light (λ ≥ 420 nm) while eliminating ultraviolet components. Light intensity was measured with a solar power meter (sm206, Sanpometer, Shenzhen, China) and adjusted with a knob. After the reaction, photocatalyst particles were removed via centrifugation, and the Chemical Oxygen Demand (COD) of the treated wastewater was measured by the potassium dichromate colorimetric method [25].

2.5. Analytical Methods for Wastewater

The changes in the composition and concentration of pollutants in wastewater before and after the treatment reaction were detected using the following methods: three-dimensional fluorescence spectroscopy (F-7100 fluorescence spectrophotometer, Hitachi, Japan) [26]; gas chromatography–mass spectrometry analysis (GC-MS 7000C, Agilent Technologies, Santa Clara, CA, USA) [27]; and wavelength scanning (DR5000, Hach, Loveland, CO, USA) [28].
pH was measured using a pHs-25 pH meter. BOD (Biochemical Oxygen Demand) was determined via the dilution and seeding method [29]. COD (Chemical Oxygen Demand) was measured via the potassium dichromate method (DR5000, Hach, Loveland, CO, USA) [25].

3. Results and Discussion

3.1. Characterization of CuTiO3

3.1.1. Uv-Vis DRS Characterization of CuTiO3

Uv-Vis diffuse reflectance spectroscopy (Uv-Vis DRS) was employed to investigate the light absorption range and bandgap structure of the synthesized catalyst in the 200–800 nm wavelength region. As shown in Figure 2a, the CuTiO3 material exhibited a photoresponse within the 250–400 nm range (covering UVA, UVB, and part of the UVC region), enabling efficient absorption of most ultraviolet light. Furthermore, it maintained a favorable photoresponse in the 400–460 nm visible-light range, with its absorption edge located at 492 nm, thereby allowing for enhanced utilization of visible-light energy. The high and flat absorption (250–460 nm) rate indicates that CuTiO3 has a good absorption effect in this range. In the long-wavelength region (492–800 nm), a weak and flat absorption band can be observed; it cannot excite intrinsic interband electronic transitions, leading to a sharp decline in absorption, which is attributed to the intrinsic properties of the material, indicating negligible absorption of long-wavelength light by the catalyst. The optical bandgap energy was calculated using the Kubelka–Munk function:
( a h v ) 1 n = A h v − E g
where α is the absorption coefficient, h is Planck’s constant (6.63 × 10−34 J·s), ν is the light frequency, A is a proportionality constant, n is an index related to the semiconductor type (n = 1/2 for CuTiO3), and Eg is the bandgap energy. Using Equation (1), the material’s optical absorption coefficient (α) is plotted against photon energy (hν), yielding a linear functional relationship between absorption characteristics and photon energy (Figure 2b). The tangent line drawn to the linear ascending region intersects the hν axis at the material’s bandgap, with the CuTiO3 material exhibiting a bandgap of 2.52 eV. This value represents the transition capability of photogenerated carriers across the bandgap during photocatalysis reaction, facilitating the generation of electron–hole pairs that drive oxidation reactions [30].

3.1.2. SEM Characterization of CuTiO3

A scanning electron microscope (SEM) equipped with an EDS (Energy-Dispersive X-ray Spectroscopy) system (GeminiSEM 500) was used to observe the surface morphology of the samples, and the SEM image is shown in Figure 3.
The SEM image of the CuTiO3 material is presented in Figure 3, revealing its microstructure characteristics. The as-prepared CuTiO3 exhibits an agglomerated morphology with a rough texture, numerous surface cracks, and a stacked structure composed of small particles. This unique microstructure contributes to a larger specific surface area for the catalyst. This morphology offers advantages in catalytic and photocatalytic reactions, as it enables better contact with reactants and facilitates reaction progression. The hydrothermal synthesis method provides a rougher surface and more active sites, thereby enhancing the photocatalytic performance [31].

3.2. Performance of CuTiO3 Photocatalysis in Treating Organic Peroxide Production Wastewater

3.2.1. Control Experiment on Photocatalytic Treatment of Organic Peroxide Production Wastewater

To investigate the photocatalytic treatment efficiency of photocatalysts on organic peroxide production wastewater, a non-photocatalyst control group was established with the following parameters: light intensity = 1300 W/m2, initial pH = 5, initial COD concentration = 15,950 mg/L, and no catalyst addition.
Non-photocatalytic reaction over 4 h yielded a COD removal rate of 21%, as depicted in Figure 4. During illumination, the wastewater temperature progressively increased from 17 °C to 30 °C with subsequent stabilization. This temperature rise intensified odor emissions due to the volatilization of components in the wastewater. Notably, certain constituents may direct photolysis under irradiation [32]. All subsequent experiments exhibited volatilization and photolytic effects.

3.2.2. Effect of CuTiO3 Dosage

The pH for each photocatalytic reaction was at raw pH, with a wastewater volume of 200 mL and an influent COD concentration of 13,285 mg/L. The catalyst dosage was set at 0.6 g/L, 0.8 g/L, 1.0 g/L, 1.2 g/L, and 1.4 g/L.
The COD removal rate, as shown in Figure 5a, increased with a rising photocatalyst dosage within the range of 0.6 g/L to 1.2 g/L. This enhancement is attributable to the increased number of total active sites, generating more photogenerated electrons (e−) and holes (h+) on the catalyst surface, which thereby accelerated the generation rates of ·O2- (superoxide radical) and ·OH (hydroxyl radical) species, further improving the degradation efficiency of COD [33]. However, when the photocatalyst dosage reached 1.4 g/L, a decrease in removal efficiency was observed. The reason is that excessive photocatalyst impeded light penetration through the wastewater, consequently reducing the removal rate [34]. Therefore, a catalyst dosage of 1.2 g/L was identified as the optimum dosage.

3.2.3. Effect of pH

In this study, 200 mL of wastewater with an influent COD concentration of 12,588 mg/L was treated using a catalyst dosage of 1.2 g/L. The pH of the reaction system was adjusted to 2, 3, 4, 5, 6, 7, and 8 using dilute acids (H2SO4) and bases (NaOH).
As shown in Figure 5b, as the initial pH value increased, the removal efficiency of wastewater via photocatalysis first rose and then declined, reaching its peak at pH 5. This indicates that photocatalytic performance is better under weakly acidic conditions. Equations (2)–(5) demonstrate that the reaction of holes (h+) oxidizing water proceeds more readily, which promotes the generation of ·OH [35]. Furthermore, the acidic environment favors the suppression of the recombination of photogenerated electrons (e−) and holes (h+), allowing more holes to be utilized for the direct oxidation of pollutants or the formation of ·OH, thereby enhancing the quantum efficiency. The generation of hydroxyl radicals (·OH) is lower under alkaline conditions than under acidic conditions, which is the primary reason for the decrease in treatment efficiency as the pH increases. However, when the pH increased from pH 5, the COD removal rate did not continue to improve. This may be attributed to the corrosion of the catalyst under excessively acidic conditions, leading to a decline in the performance of the photocatalyst. CuTiO3 demonstrated higher degradation efficiency for organic peroxide production wastewater at pH 5.

3.2.4. Effect of Light Intensity

All reactions were conducted using 200 mL of wastewater at pH 5, with an influent COD concentration of 15,154 mg/L and a catalyst dosage of 1.2 g/L. Light intensity was systematically varied at 1100 W/m2, 1200 W/m2, 1300 W/m2, and 1400 W/m2.
As evidenced in Figure 6a, the COD removal rate exhibited a modest increase within the light intensity range of 1100–1300 W/m2, peaking at 1300 W/m2 before stabilizing. This trend is attributed to increased generation of electron–hole pairs at higher light intensities, with more active groups formed through combination, thereby improving photocatalytic degradation efficiency [36]. Beyond 1300 W/m2, no significant enhancement was observed, indicating the recombination rate of photogenerated carriers rises, leading the photocatalytic reaction into a state of light saturation. Once the photosaturation state is reached, further increasing the light intensity will not cause significant changes in the COD removal rate [37].

3.2.5. Effect of Reaction Duration

Holding constant the parameters (200 mL wastewater, pH 5, 12,956 mg/L influent COD, 1.2 g/L catalyst, 1300 W/m2 irradiance), the photocatalytic COD removal rate was recorded every hour over the reaction period of 1 to 6 h.
As illustrated in Figure 6b, with the extension of time, the COD removal rate increased, reached the maximum value after 4 h and then showed no significant improvement. This is due to the continuous degradation of organic pollutants via photocatalysis, but as the concentration of organic pollutants decreases, the reaction rate gradually decreases. Consequently, 4 h was identified as the optimal reaction duration for efficient photocatalytic treatment.

3.2.6. Performance of Photocatalysis on Wastewater Treatment Under Optimized Conditions

In this paper, under the optimized conditions of a 12,900 mg/L COD concentration, initial pH 5, CuTiO3 dosage of 1.2 g/L, light intensity of 1300 W/m2, and reaction duration of 4 h, the COD and BOD5 of the wastewater were measured to determine its B/C(BOD5/COD) ratio; the wastewater is considered more amenable to biological treatment methods when this ratio is higher, as it reflects greater biodegradability.
As shown in Figure 7, under optimal conditions, after adding the CuTiO3 photocatalyst, the COD removal rate of the system for wastewater increased from 18% to 58%. This indicates that the CuTiO3 photocatalytic system can effectively enhance the treatment effect on organic peroxide production wastewater. Photocatalysis achieved a marked improvement, showing a 61% higher efficiency compared to the 36% COD removal rate obtained from previous iron–carbon micro-electrolysis treatment of the same wastewater [1]. To date, there have been no reports on the utilization of visible-light photocatalysis for treating organic peroxide wastewater. Previous studies by Baygi et al. have demonstrated that an Al2O3 foam coated with a CuTiO3 layer achieved a photocatalytic degradation efficiency of approximately 70% for methylene blue [38]. Generally, organic peroxide wastewater exhibits a more complex composition and a higher COD concentration, leading to greater treatment challenges. Therefore, the results obtained in this study demonstrate positive significance.
After pretreatment via CuTiO3 visible-light photocatalysis, the B/C ratio of the wastewater increased from 0.112 to 0.221, indicating a significantly improved biodegradability. This result demonstrates that CuTiO3 visible-light photocatalysis can decompose macromolecular organic compounds into smaller molecules, which are more biodegradable by microorganisms. This transformation provides more favorable conditions for subsequent biological treatment processes.

3.3. Reusability of CuTiO3 Photocatalyst

Under the optimized conditions of 200 mL wastewater volume, 1300 W/m2 light intensity, pH 5.0, 1.2 g/L catalyst dosage, and influent COD concentration of 16,447 mg/L, five consecutive photocatalytic reactions were conducted to evaluate the reusability of CuTiO3. After each reaction, the catalyst was recovered by centrifugation at 2500 rpm, washed and dried, and reused in subsequent experiments.
As depicted in Figure 8a, the COD removal rate of CuTiO3 reached 59.24% during the initial cycle and declined modestly to 54.71% after five consecutive cycles. The experimental results show that CuTiO3 has stable chemical properties, and it can effectively maintain high catalytic performance in five cycles. The efficiency reduction is attributable to partial catalyst loss during recovery processes (Figure 8b). In conclusion, the excellent reusability proves that the prepared CuTiO3 is a photocatalyst with practical application prospects.

3.4. Transformation of Organic Compounds and Reaction Mechanism in Photocatalytic Treatment of Organic Peroxide Production Wastewater

3.4.1. Uv-Vis Analysis

Wavelength scanning analysis of the wastewater samples, both influent and effluent water, revealed significant changes in Uv-Vis absorption profiles. The corresponding spectra within the 190–350 nm range are presented in Figure 9.
After the reaction, the relative intensity of the absorption peak at 202 nm decreased from 3.66 to 2.35, indicating a significant weakening of the absorption peak. Absorption peaks within this spectral range are typically associated with compounds with unsaturated bonds (e.g., C=C) or heteroatomic functional groups (alcohols, phenols, aldehydes, ketones, amides, etc.) [1,39]. This indicates that after photocatalytic treatment, certain unsaturated and heteroatomic compounds in the wastewater were likely removed or transformed. The absence of any new peaks indicates that no intermediate by-products with significant UV absorption were generated during the treatment process, which implies the relatively thorough mineralization of pollutants into CO2 and H2O or their conversion into small, non-UV-absorbing molecules.

3.4.2. 3D-EEM Analysis

3D-EEM analysis was performed on the influent and effluent of organic peroxide production wastewater treated via photocatalytic pretreatment [40].
The color intensity of fluorescence peaks in 3D-EEM reflects the concentration and pollution level of organic contaminants in water bodies. Analysis was performed using the widely adopted Fluorescence Regional Integration (FRI) method [41]. Comparative analysis of influent and effluent 3D-EEM spectra (Figure 10a,b) revealed varying degrees of reduction in organic compounds across Regions I, II, and IV. This indicates that the photocatalytic reaction effectively degraded tyrosine-like and tryptophan-like substances in the wastewater. Specifically, the characteristic peak intensity of protein-like substances (Region IV) significantly weakened. Conversely, a slight increase in the weak characteristic peak of humic acid-like substances (Region V) was observed post-reaction. This phenomenon may be attributed to the partial conversion of macromolecular proteins into humic acid derivatives.

3.4.3. GC–MS Analysis

GC–MS analysis was performed on organic peroxide production wastewater before and after the photocatalytic reaction.
Comparative analysis of influent and effluent GC-MS spectra (Figure 11a,b) revealed significant removal of esters, amides, and anhydrides from the wastewater via photocatalytic treatment. Macromolecular nitrogen-containing compounds, such as caprolactam and N-benzyloxy-2,2-bis(trifluoromethyl)aziridine, were degraded, potentially generating ammonia and small-molecule compounds. Compounds such as methyl benzoate are degraded into benzoic acid. Furthermore, macromolecular organic compounds, including 2-chloroethyl benzoate, 1,3-benzenediol monobenzoate, 2-ethylhexoic acid, α, α-dimethyl benzenemethanol, and neopentane, were either removed or transformed during the reaction. The relative content of cyclohexane and .alpha.-methylstyrene significantly decreased. After the photocatalytic reaction, the diversity of organic contaminants in the wastewater markedly decreased. Conversely, as illustrated in Figure 11c, photocatalytic degradation exhibited limited efficacy against specific pollutants such as acetophenone and α-methylstyrene. Notably, new contaminants, including 3-heptanone and propane, 2-methoxy-2 methyl ether, were generated during the reaction. Although the decomposition of tert-butyl hydroperoxide (TBHP) under visible-light irradiation has been documented in previous studies [42,43], the GC-MS spectra from this experiment indicated that no decrease in TBHP content was observed. This discrepancy may be attributed to the formation of intermediates from alcohols containing weak C–H bonds during the photocatalytic reaction process, followed by their oxidation with reactive species under reaction conditions to generate TBHP [44].

3.4.4. The Mechanism of Degradation Pollutants in Organic Peroxide Production Wastewater

Under the conditions of 200 mL wastewater volume, 1300 W/m2 light intensity, pH 5.0, catalyst dosage of 1.2 g/L, and influent COD concentration of 14,253 mg/L, specific quenchers were selected to identify the contributions of different reactive species: tert-butanol (TBA) as a hydroxyl radical (·OH) quencher; AgNO3 as an electron (e−) quencher; EDTA-2Na as a hole (h+) quencher; and chloroform (CHCl3) as a superoxide radical (·O2−) quencher.
As shown in Figure 12, the COD removal rate of the blank group (without quenching agents) reached 59.24%. The addition of 0.5 mmol/L alcohol-based quenching agent (TBA) reduced the COD removal rate to 36.35%, while 0.5 mmol/L chloroform (CHCl3) quenching agent lowered it to 57.03%. For systems containing 0.5 mmol/L EDTA-2Na and AgNO3, COD removal rates decreased to 53.46% and 48.66%, respectively. The inhibitory effects of the four quenching agents from strong to weak were as follows: TBA > AgNO3 > EDTA-2Na > CHCl3, indicating that the contribution of reactive species to the reaction was ·OH > e− > h+ > ·O2−. Therefore, hydroxyl radicals (·OH) play the dominant role in CuTiO3 photocatalytic degradation of organic peroxide production wastewater.
The reaction occurring during the photocatalytic experiment is illustrated in Figure 13. Under visible-light irradiation, CuTiO3 is activated, generating electrons (e−) and holes (h+). Incident light with energy exceeding the semiconductor bandgap excites electrons to transition from the valence band (VB) to the conduction band (CB), leaving holes in the VB. The photogenerated electrons and holes are captured by O2 and H2O, generating reactive species including superoxide radicals (·O2−) and hydroxyl radicals (·OH) [45].
CuTiO3 + light → h+ + e−
h+ + OH− → ·OH
e− + O2 → ·O2-
The attack by hydroxyl radicals (·OH) on ester molecules primarily involves the cleavage of unsaturated bonds or the abstraction of active hydrogen atoms. This process generates radical intermediates (e.g., Alkyl radical and acyloxy radical), which propagate through chain reactions, leading to the degradation of esters into small molecular carboxylic acids and alcohols [46,47]. These primary products can be further mineralized into CO2 and H2O. Hydroxyl radicals attack anhydrides, causing the anhydride bonds to break and generating carboxylic acids and radical intermediates [48]. The proposed reaction pathways are outlined below:
R-CO-O-CO-R’ + ⋅OH → R-COOH + R’-COO⋅
R-COO-R’ + ·OH → R-COO· + R’-OH
R-COO· → R· + CO2 ↑
R· + ⋅OH → ROH
From Equations (5)–(8), it can be seen that photocatalytic oxidation mainly decomposes larger organic pollutants such as esters and anhydrides into smaller organic pollutants such as carboxylic acids and alcohols. Some of these carboxylic acids and alcohols may continue to participate in oxidation reactions and be completely mineralized into harmless CO2 and H2O. The other part terminates the reaction. As shown in Figure 10a,b the peak intensities of Benzenemethanol and Hexanoic acid, 3,5,5-trimethyl increased after the reaction, while Dimethyl phthalate at around 28 min was not detected after the reaction. This further confirms that carboxylic acids and alcohols are generated as reaction products, while esters are consumed.

4. Conclusions

This study successfully demonstrates the synthesis and application of a visible-light-responsive CuTiO3 photocatalyst for the efficient pretreatment of refractory organic peroxide production wastewater, addressing the research gap. The key findings are summarized as follows:
(1)
Under optimized conditions (initial pH = 5.0, catalyst dosage = 1.2 g/L, light intensity = 1300 W/m2, reaction time = 4 h), the CuTiO3 photocatalytic system achieved a COD removal rate of 58%. More importantly, the biodegradability (B/C ratio) of the wastewater was significantly enhanced, increasing from 0.112 to 0.221. This demonstrates that the process effectively converts recalcitrant organic compounds into more biodegradable forms, providing an excellent pretreatment strategy for subsequent biological treatment.
(2)
DRS characterization confirmed the strong visible-light response of CuTiO3, with an absorption edge at 492 nm and a bandgap of 2.52 eV, enabling efficient utilization of visible-light energy. The catalyst also exhibited robust stability and reusability, maintaining a high COD removal efficiency of 54.71% after five consecutive reaction cycles, indicating its potential for long-term practical application. A multi-method analytical approach (3D-EEM, Uv-Vis, and GC-MS) revealed the effective degradation and transformation of diverse refractory organic pollutants. 3D-EEM showed a significant reduction in tyrosine-like and tryptophan-like substances. GC-MS analysis confirmed the effective removal or transformation of esters, amides, and anhydrides (e.g., caprolactam). Radical quenching experiments unequivocally identified the hydroxyl radical (OH) as the primary active species responsible for the degradation, elucidating the underlying reaction mechanisms.

Author Contributions

Conceptualization, Z.Y. and H.L.; methodology, H.L.; validation, H.L.; formal analysis, H.L.; investigation, H.L.; resources, Z.Y.; data curation, H.L.; writing—original draft preparation, H.L.; writing—review and editing, Z.Y. and H.L.; visualization, H.L. and S.L.; supervision, Z.Y.; project administration, Z.Y.; funding acquisition, H.Y. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the Gansu Province Ecological Civilisation Construction Key R&D Special Project (25YFFA014), the National Natural Science Foundation of China (51568034), the Department of Education of Gansu Province: Major Cultivation Project of Scientific Research Innovation Platform at Universities (2024CXPT-14), and the Open Foundation of the Key Laboratory of Yellow River Water Environment in Gansu Province (20JR2RA0002).

Data Availability Statement

All data generated or analyzed during this study are included in this article. The data used in this study are available on request.

Acknowledgments

The authors acknowledge/thank the heads of the funding project.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. Flow chart of CuTiO3 preparation.
Figure 1. Flow chart of CuTiO3 preparation.
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Figure 2. (a) UV–visible spectrum; (b) Diffuse reflection spectrum of CuTiO3.
Figure 2. (a) UV–visible spectrum; (b) Diffuse reflection spectrum of CuTiO3.
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Figure 3. SEM image of CuTiO3 photocatalyst: (a) ×50 KX, (b) ×200 KX.
Figure 3. SEM image of CuTiO3 photocatalyst: (a) ×50 KX, (b) ×200 KX.
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Figure 4. Blank control group of the CuTiO3 photocatalytic system.
Figure 4. Blank control group of the CuTiO3 photocatalytic system.
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Figure 5. Factors affecting photocatalytic organic peroxide production wastewater degradation: (a) photocatalytic dosage and (b) pH.
Figure 5. Factors affecting photocatalytic organic peroxide production wastewater degradation: (a) photocatalytic dosage and (b) pH.
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Figure 6. Factors affecting photocatalytic organic peroxide production wastewater degradation: (a) light intensity; (b) reaction duration.
Figure 6. Factors affecting photocatalytic organic peroxide production wastewater degradation: (a) light intensity; (b) reaction duration.
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Figure 7. The removal rate of wastewater treated via photocatalysis under optimized conditions.
Figure 7. The removal rate of wastewater treated via photocatalysis under optimized conditions.
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Figure 8. (a) CuTiO3 photocatalytic repeat reaction removal rate, (b) recycle dose after reaction.
Figure 8. (a) CuTiO3 photocatalytic repeat reaction removal rate, (b) recycle dose after reaction.
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Figure 9. Uv-Vis absorption profiles of influent and effluent water.
Figure 9. Uv-Vis absorption profiles of influent and effluent water.
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Figure 10. 3D-EEM of (a) influent and (b) effluent water.
Figure 10. 3D-EEM of (a) influent and (b) effluent water.
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Figure 11. GC-MS spectra of (a) influent and (b) effluent; (c) compound composition.
Figure 11. GC-MS spectra of (a) influent and (b) effluent; (c) compound composition.
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Figure 12. Experiment on capture of active species.
Figure 12. Experiment on capture of active species.
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Figure 13. Mechanism of photolysis and photosensitization.
Figure 13. Mechanism of photolysis and photosensitization.
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MDPI and ACS Style

Yan, Z.; Li, H.; Yang, H.; Li, S. Performance of CuTiO3 Photocatalytic Oxidation for Treating Organic Peroxide Production Wastewater Under Visible Light. Sustainability 2026, 18, 983. https://doi.org/10.3390/su18020983

AMA Style

Yan Z, Li H, Yang H, Li S. Performance of CuTiO3 Photocatalytic Oxidation for Treating Organic Peroxide Production Wastewater Under Visible Light. Sustainability. 2026; 18(2):983. https://doi.org/10.3390/su18020983

Chicago/Turabian Style

Yan, Zichun, Hongfu Li, Hao Yang, and Shuo Li. 2026. "Performance of CuTiO3 Photocatalytic Oxidation for Treating Organic Peroxide Production Wastewater Under Visible Light" Sustainability 18, no. 2: 983. https://doi.org/10.3390/su18020983

APA Style

Yan, Z., Li, H., Yang, H., & Li, S. (2026). Performance of CuTiO3 Photocatalytic Oxidation for Treating Organic Peroxide Production Wastewater Under Visible Light. Sustainability, 18(2), 983. https://doi.org/10.3390/su18020983

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