Abstract:
Cobalt-doped alumina catalyst calcined at 500 °C (CoA-500) was investigated in the degradation of anionic textile dye Orange G in the presence of Oxone®. Different reaction parameters were altered in order to study their influence on Orange G degradation. The increase of the Oxone® dosage, mass of the catalyst and temperature was beneficial for the dye degradation rate. The best catalytic performance was obtained in the range of the initial solution pH = 6-8. Simultaneous degradation of both Orange G and cationic textile dye Basic blue 41, was also tested. The degradation of the Basic blue 41 did not occur while Orange G was present in the system. CoA-500 was found to be efficient catalyst in the Oxone® induced catalytic degradation of textile dyes.
Keywords: Cobalt-doped alumina catalyst; Peroxymonosulfate; Catalytic oxidation process; Orange G textile dye; Simultaneous dye degradation.
Сажетак: Кобалтом допирани катализатор Ha бази алумине je калцинисан на 500 °C (CoA-500) и ucnumuean у deepadayuju anjoncxe текстилне 6oje Orange G y присуству Okcoha (Oxone®). Испитиван je ymuyaj различитих реакционих параметара на деградаци]у Orange G боге. Повейаъе mace Оксона, mace катализатора и температуре je noитивно утицало на брзину oeepadayuje боге. Науболе каталитичко dejemeo je оставрено у области рН почетног раствора измейу 6 и 8. Taxohe je ucnumana симултана деградаци/а Orange С и kamjoncre Ooje Basic blue 41. Уочено je да ce dezpadayuja Hoje Basic blue 41 не дешава све док je 6oja Orange С присутна у систему. 3ak;byчено je da ce CoA-500 може користити као ефикасан катализатор y итичко} deepadayuju текстилних 6oja y присуству Оксона.
Къучне peuu: - Кобалтом donupanu - катализатор na - бази - алумине; Пероксимоносулфат; Каталитички оксидациони процес; Orange G текстилна бо/а; Симултана деградаци/а
(ProQuest: ... denotes formula omitted.)
1. Introduction
Metal oxides have a vast number of applications and many of them are associated with the surface activity that most of the metal oxides exhibit. The applications related to surface-activity include adsorption, sensing, and catalysis. Aluminum (III) oxide is a surfaceactive ceramic material that exists in a number of crystalline phases (polymorphs), more often referred to as "alumina". Aluminas are characterized by a high resistance to wear at both low and high temperatures, good mechanical properties, impact resistance, chemical resistance, abrasion resistance, and high-temperature properties [1, 2].
The application of alumina is mainly in catalytic processes and adsorption technologies. In the field of catalysis, alumina is largely used as a support of catalysts because it is inexpensive, reasonably stable, and can provide a wide range of surface areas and porosities, through its different phases [3]. By adding different metals or metal oxides properties of alumina can be altered [4] In metal-doped alumina, small amounts of metal are added in situ (during the synthesis of alumina), allowing the doping agent to be uniformly dispersed and closely associated with the aluminum matrix [5].
Advanced oxidation processes involve the generation of highly reactive intermediate radicals (dominantly hydroxyl radicals) which are powerful oxidants that can be applied to degrade organic compounds in wastewater treatments [6]. Sulfate anion radicals (SO14") were proven to be more powerful, selective and effective for the degradation of persistent organic pollutants than hydroxyl radicals [7-8]. Peroxymonosulfate (PMS) as an active component in mixed salt Oxone® (2KHSOsxKHSOsxK>SO4) can be used as a source of sulfate anion radicals. It is relatively stable, easily stored and transported, environmentally friendly, and cost-effective material [9-10].
Self-decomposition of PMS is a very slow process, so it should be activated externally [11]. PMS activation using metal-based heterogeneous catalysts is a promising strategy for reducing the release of metal cations into the environment and increasing the catalytic activity. Cobalt has shown the best performance of all transition metals in PMS activation [12]. To avoid the potential problems of using homogeneous solutions of soluble cobalt, heterogeneous cobalt-based catalysts have been developed [9, 13]. To the best of our knowledge, this group of researchers was the first to investigate cobalt-doped alumina in the PMS activation process applied in the oxidative degradation of tartrazine azo dye [14].
Environmental pollution affects the health of people and all life on Earth, so worldwide efforts are being made to reduce it [15]. Synthetic dyes are toxic and mutagenic organic compounds that cannot be biodegraded [16]. The release of these chemicals into natural waters would create a huge ecological problem that would affect the natural ecosystem and could influence human health [17]. For this reason, industrial wastewater must be treated before discharge into natural waters. Orange G (OG) is a synthetic, textile, anionic, mono-azo dye soluble in water and stable at any pH. It is the disodium salt of 7-hydroxy-8[(E)-phenyldiazenyl] naphthalene-1,3-disulfonic acid (C:6H10N2Na2z07S2) [18]. This dye has a hazardous and harmful effect on aquatic species and the entire water environment. It's toxic, carcinogenic, and teratogenic effects on living organisms have been attributed to the azo group in its chemical structure [19]. Basic blue 41(Cy0H26N4O6S>) is also synthetic, textile, mono-azo dye, but in contrast to OG, Basic blue 41 is a cationic. Even 1ppm of this dye in water can be hazardous to aquatic life [20].
The investigation of the simultaneous degradation of two or more contaminants in water is justified, since wastewaters usually contain more than one pollutant. The interaction of these pollutants in water medium can change kinetics of degradation reactions, comparing to degradation of the single pollutant [21].
In our previous paper [14], cobalt-doped alumina catalysts, calcined at different temperatures were investigated as catalysts in Oxone® induced degradation of food dye tartrazine. Under investigated conditions catalyst calcined at 500 °C (CoA-500) showed the best performance. In this follow-up study, CoA-500 was investigated in Oxone® activated oxidative degradation of textile dye Orange G. The influence of different reaction parameters on Orange С degradation: Oxone® dosage, Orange G concentration, mass of the catalyst, initial solution pH and temperature was followed. Apart from these experiments simultaneous degradation of two textile dyes Orange G and Basic Blue 41 was followed
2. Materials and Experimental Procedures
2.1 Materials and synthesis
Oxone® (monopersulfate compound, KHSOs-0.5-KHSO4-0.5-K3SO4) and textile dyes Orange G (OG) and Basic blue 41 (BB) were supplied by Sigma Aldrich and were used as received.
CoA-500 was prepared by the sol-gel method using aluminum isopropoxide as a precursor The sol-gel transformation was carried out by drying according to a specific regime and then the gel was heated from room temperature to the final temperature of 500 °C, with the heating rate of 2 °C min" and kept at the final temperature for 5 h in the CARBOLITE STF 15/75/400 horizontal tube furnace, with the aim of formation of y-ALO;, as the most suitable alumina phase for the catalytic support. At this temperature, the dehydration and dehydroxilation of the boehmite surface takes place by a sintering process, e.g., neck formation between crystallites, via surface diffusion, leaving behind a large number of new active centers and vacancies in tetrahedral positions. This is followed by the migration of the remaining vacancies protons and Al(IIT) cations and lasts until the system recrystallizes from boehmite into a new tetragonally deformed cubic y-spinel. In this way, the porous structure of the product was developed.
The synthesis was presented in details in our previous article together with the characterization of the synthesized material [14]. Synthesized material was characterized by X-ray powder diffractometry (XRPD), temperature programmed reduction (Hz TPR) and lowtemperature N physisorption. In order to correlate the catalytic efficiency and structural, phase, and textural properties of the catalyst, the characterization results are summarized and presented in Table S1 of the S1. part of the Supplementary material.
In addition to previous characterization, CoA-500 morphology was examined by Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM-EDS). SEM-EDS measurements were performed under the following conditions: tungsten filament, resolution - 3.5 nm at 30 kV, accelerating voltage - 200 V - 30 kV, EDX detector - BRUKER-Quantax 200, spectroscopic resolution at Mn-Ka and 1 kcps 126 eV.
2.2 Catalytic tests
Catalytic tests were conducted according to the procedure described in S2. part of the Supplementary material.
The experimentally obtained data were tested in the most common kinetic models in order to check which model fits best. The pseudo-first-order kinetic model was found to be the most suitable for all the experimental conditions. The obtained kinetic parameters are presented in column charts alongside the results of catalytic tests in order to facilitate the monitoring of the degradation process.
3. Results and Discussion
The XRPD together with H,-TPR confirmed the presence of two main phases in CoA-500: Co-spinel (Co304, CoALOs, C0,A104) and y-Al>03. Also, the synthetized material showed developed surface area and the high total pore volume (Table S1). Additional characterization was performed using SEM-EDS.
The SEM analysis of CoA-500 reveals existence of the wide particle size distribution. At higher magnification (Fig. 1b) white smaller particles of cobalt are noticeable. This is in agreement with H>-TPR where Co304 was identified as the dominant Co-phase. Additionally, the elemental mapping EDS pictures reveals homogeneous microstructure and uniformly distributed Co and Al (Fig. 1). Surface composition of CoA-500 is presented in Table S2 of Supplementary material.
3.1. The effect of Oxone® dosage on OG degradation
The mass of Oxone® was varied from 10 mg to 80 mg (Fig. 2a). Positive effect of the increase of Oxone® dosage on OG degradation was observed only after 60 min. Small differences in degradation efficiency were obtained in the first reaction hour. It was noticeable that degradation rate was the lowest for the highest Oxone® mass in first 30 min of the reaction, and it gradually increased as the reaction went on. The mass of 40 mg of Oxone® was optimal until the end of the reaction, when higher degradation was obtained for 80 mg of Oxone®. A possible explanation for this behavior lies in the fact that by that moment the content of radicals in the system was reduced due to their consumption in the reaction.
The highest square of coefficients of correlation values (R? > 0.984) was obtained for the pseudo-first-order kinetic model for all investigated masses of Oxone® (Fig. 2b). The pseudofirst-order rate constant (k) is a measure of the speed of a chemical reaction. The determination of k is of importance for comparison how different reaction parameters affect the reaction rate. The pseudo-first order rate is expected since Oxone® is used in excess compared to OG. k is almost doubled when mass of Oxone® increased from 10 mg to 80 mg, while its value was similar for 20 mg, 40 mg and 80 mg.
3.2. Influence of OG concentration
The influence of the OG concentration (Co oc) was followed in the range 20-50 mg dm? (Fig. 3a). The decrease of the degree of degradation with OG concentration increase was observed. For the Co,oo = 20 mg dm? the reaction was much faster than for other concentrations, even for small reaction times, where other concentrations show similar behavior. For this Cog almost 100% of degradation was obtained after 120 min. For other three Cog degradation degree was between 60 and 80% for the investigated reaction time.
With the decrease of the OG concentration from 50 mg dm· to 20 mg dm? the pseudo-firstorder rate constant increased almost 3 times. The biggest increase in k values for two consecutive Co,oo was obtained for the decrease from 30 mg dm? to 20 mg dm? and it was about 1.7 times. In other cases, the increase of k was about 1.3 times.
3.3. Influence of mass of catalyst
The influence of the mass of the catalyst (ca) Was investigated for CoA-500 in the mass range from 10 mg to 100 mg. Degradation reactions were carried out maintaining equal experimental conditions (Fig. 4a). With the increase of the mass of the catalyst the degree of degradation increased. For the mass of 100 mg a plateau, related to nearly 100% of degradation, was reached after 20 min. On the other hand, for the 10 mg of the catalyst, 60% of degradation was observed within the investigated time (120 min).
The obtained results showed that CoA-500 is a highly active catalyst because even a small mass of CoA-500 (10 mg) was sufficient to activate PMS, which further led to OG degradation. The pseudo-first-order kinetic model was found to be applicable for all investigated masses of the catalyst (Fig. 4b). The pseudo-first-order rate constant (k) increased with increasing mass of the catalyst, with the square of coefficients of correlation R· > 0.981. The pseudo-first-order rate constant (k) increased 2.6; 6.4 and 19.1 times when mass of catalyst increased from 10 mg to 25 mg, 50 mg and 100 mg, respectively. This confirmed that a higher CoA-500 mass accelerated OG degradation by facilitating production of sulfate anion radicals from PMS in the presence of more active sites.
For further investigations, a 10 mg of catalyst was chosen so the monitoring of the kinetic of the investigated reaction could be possible.
3.4. Influence of temperature
The influence of temperature was investigated in the range from 30 to 60 °C. The temperature increase was beneficial for the OG degradation rate (Fig. 5a). The degradation was almost complete after 120 min for temperatures over 40 °C.
The pseudo-first-order rate kinetic model was found to be the most appropriate for all investigated temperatures, with the square of the coefficient of correlation R? > 0.982. As shown in Fig. 5b, the pseudo-first-order rate constants (k) increased with increasing reaction temperature. The pseudo-first-order rate constant increases from 1.5 to 3 times with each 10 °C increase in temperature. The pseudo-first-order rate constant for 60 °C was 25 times higher than for 30 °C.
In order to calculate activation energy (Ea), the Arrhenius equation (1) was applied using obtained kinetic data:
... (1)
k- pseudo-first-order rate constant, A - constant related to the geometry, Eq - activation energy (J mol), and T - thermodynamic temperature (К) and К - universal gas constant (8.314 Jmol1 K1)
The obtained results are presented in Fig. 6.
The slope of the Arrhenius plot may be used to calculate the activation energy. The following activation energies are obtained: E, = 80.18 kJ mol'. The obtained value is in line with those obtained in similar systems [22, 23]. Relatively low activation energy indicates that the reaction can be easily performed.
3.5. Influence of initial pH
The initial pH of an aqueous solution (pH;) is another parameter that has a significant impact on the degradation of the organic contaminants. The influence of pH; of dye solution on the degradation process was investigated in the pH range from 2 to 9. The results were presented in Fig. 7a. The unadjusted initial pH value of pH; = 3.7 was included in these graphs.
It could be observed that the optimum performance appeared for pH; = 6-8, which was consistent with the previous studies on Co-based catalysts [14, 24]. Degradation of OG in the pH; = 6-9 was almost the same and was = 100% after 120 min of the reaction.
In Fig. 7b pseudo-first-order rate constants for different pH; was presented. The Æ values in pHi range from 6 to 9 were similar. The highest value was obtained for pH; = 7. Comparing to pHi = 2, k at pH; = 7 was 7.5 times higher. The obtained results confirmed that the CoA-500 catalyst is applicable with high efficiency in the wide range of initial pH values.
3.6. Simultaneous degradation of two textile dyes Orange G and Basic blue 41
Basic blue 41 (BB), cationic textile dye with characteristic peak in UV-Vis spectrum at Amax = 609 nm, was also tested in Oxone® induced degradation in the presence of the investigated catalyst. Apart from single component solution degradation test, simultaneous degradation of BB and OG was investigated. It was possible to follow the simultaneous degradation of OG and BB using UV-Vis spectroscopy since their characteristic peaks did not overlap. The degree of degradation of investigated dyes was calculated by comparing the absorbance at the characteristic peaks at predefined reaction times with the initial absorbance values. Co, no Was 20 mg dm? in all the tests. For comparison's sake the results obtained for degradation of single component solution under the same experimental conditions were presented together with degradation efficiencies obtained in a mixture of two dyes in Fig. 8a.
It was found that degradation of the BB in single component solution occurred but it was slower than for the same concentration of OG.
In the first simultaneous degradation test Co, oc was 50 mg dm? (Fig. 8a). In the mixture of two dyes, degradation of BB did not occur for the investigated time. On the other hand, OG degradation in mixture was similar, and even slightly higher than for OG as a single component solution.
In order to check what happens when characteristic peak for OG disappears completely, in the second simultaneous test Co,oc was lowered to 20 mg dm" (Fig. 8b). This concentration was chosen because in the single component solution test complete degradation at Amax = 478 nm was obtained.
It is clear that BB degradation did not start while OG was present in the reaction mixture, but from the moment when characteristic peak for OG disappeared, the decrease of the peak at at Amax = 609 nm was noticed. The reaction time was extended to 240 minutes so the degradation of BB could be followed.
This phenomenon can probably be attributed to the difference in the molecular structure of the dyes, which makes BB more difficult to degrade than OG [11]. During the simultaneous degradation reaction of two dyes, the effect of the electrostatic interaction of the catalyst surface and the dye molecule charge was probably also important. OG is an anionic and BB is a cationic dye, so probably OG occupies most of the active sites on the catalyst, thus preventing the degradation of BB [21].
4. Conclusion
Cobalt-doped alumina catalyst previously found to have the best performance in Oxone® induced tartrazine degradation was tested in Orange G (OG) textile dye degradation in the in the presence of Oxone®, as a source of SO, anion radicals. The degradation of the OG solution was monitored using the UV-Vis spectroscopy, as a decrease of the intensity of a chromophore related absorption peak at Amax = 478 nm. The degradation of OG was insignificant without the catalyst due to the slow Oxone® self-decomposition. Also, the adsorption of the dye on the investigated materials was less than 3%. The influence of the Oxone® dosage, OG concentration, mass of the catalyst, temperature and initial pH of the solution on the reaction efficacy was investigated. The increase of the Oxone® dosage, mass of the catalyst and temperature was led to increase of the degradation rate. On the other hand, with the increase of the OG concentration the degree of the OG degradation decreased. The optimum catalytic performance was found in the range pH; = 6-8. The pseudo-first-order kinetic model was found to be applicable for all investigated conditions.
Apart from experiments with anionic dye OG, degradation of cationic dye Basic blue 41 (BB) was also tested, as well as simultaneous degradation of two dyes OG and BB. It was found that the BB degradation did not occur during simultaneous reaction as long as OG was present in the system, while OG degradation rate was similar to the degradation of the single component solution. On the other hand, Oxone® induced degradation of the BB was achieved in a single component solution, but it was slower than for OG.
According to the obtained results cobalt-doped alumina catalyst was found to be efficient catalyst in the catalytic oxidative degradation of textile dyes in the presence of Oxone®.
Acknowledgments
This research was financially supported by the Ministry of Science, Technological Development and Innovation of Republic of Serbia (Contract No: 451-03-47/2023-01/200026).
ORCID numbers:
Sanja Marinovié, https://orcid.org/0000-0002-2214-0157
Tihana Mudrinic, https://orcid.org/0000-0001-7467-8330
Marija Ajdukovié, https://orcid.org/0000-0003-4219-6737
Natasa Jovic-Jovicic, https://orcid.org/0000-0001-9940-9508
Dimitrinka Nikolova, https://orcid.org/0000-0003-1778-6778
Predrag Bankovié https://orcid.org/0000-0002-9732-7370
Tatjana Novakovic, https://orcid.org/0000-0002-6407-9833
© 2025 Authors. Published by association for ETRAN Society. This article is an open access article distributed under the terms and conditions of the Creative Commons - Attribution 4.0 International license (https://creativecommons.org/licenses/by/4.0/).
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Abstract
Cobalt-doped alumina catalyst calcined at 500 °C (CoA-500) was investigated in the degradation of anionic textile dye Orange G in the presence of Oxone®. Different reaction parameters were altered in order to study their influence on Orange G degradation. The increase of the Oxone® dosage, mass of the catalyst and temperature was beneficial for the dye degradation rate. The best catalytic performance was obtained in the range of the initial solution pH = 6-8. Simultaneous degradation of both Orange G and cationic textile dye Basic blue 41, was also tested. The degradation of the Basic blue 41 did not occur while Orange G was present in the system. CoA-500 was found to be efficient catalyst in the Oxone® induced catalytic degradation of textile dyes.