Reusable titania-SBA-15 photocatalyst synthesized by different silica/titania ratios for enhancing methylene blue photodegradation

Reusable titania-SBA-15 photocatalyst synthesized by different silica/titania ratios for enhancing methylene blue photodegradation | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Reusable titania-SBA-15 photocatalyst synthesized by different silica/titania ratios for enhancing methylene blue photodegradation Sevgi Can Göl, Elif Akbay This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-1831676/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 13 Nov, 2023 Read the published version in ChemistrySelect → Version 1 posted You are reading this latest preprint version Abstract In this study, a series of TiO 2 /SBA-15 photocatalysts were synthesized with different Si/Ti ratios by a one-step hydrothermal method with TiO 2 nano-powder as a titanium source. These materials were characterized by XRD, SEM-EDX, N2 adsorption-desorption isotherms-desorption isotherms, XRF, and UV-DRS analysis. During the synthesis of TiO 2 /SBA-15s, the SBA-15 pore structure and channels did not deteriorate, and the Si/Ti molar ratios are close to the expected nominal ratios. SBA-15 and TiO 2 /SBA-15s exhibited a uniform- narrow pore size distribution, but TiO 2 /SBA-15s pore size shifted to a smaller range, and the BET area values of TiO 2 /SBA-15s materials are in the range of the 621–583 m2/g. TiO 2 nanocrystals into the SBA-15 mesopores walls wall up to the ratio of Si/Ti = 16. With high TiO2 loading of that value, clogging occurs in the SBA-15 pores. The optical band gap energies were significantly blue-shifted which is the quantization effects improving the photocatalytic activities Photocatalytic activities of TiO 2 /SBA-15s were evaluated by degradation of methylene blue under UV-light irradiation at constant TiO 2 content. The highest efficiency was obtained in the TiO 2 /SBA-15 (16) photocatalyst at 79.6%, and all efficiencies in synthesized photocatalyst are higher than bulk TiO 2 photocatalyst activity (27.52%) due to the poor dispersion of active phases. Reused photocatalyst has no activity losses for five runs and may be used for long periods without loss of activity. For the stability of the photocatalyst, a combination of XRD, SEM, and N2 adsorption-desorption isotherms was employed after the fifth run. These results demonstrate that the photocatalyst activity and stability are good, and photocatalytic activity was sustainable after reuse for several cycles. Mesoporous material TiO2/ SBA-15 Photocatalytic degradation Reusability Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 1. Introduction Industries utilizing dye which are dying, textile, cosmetics, plastics, pharmaceutical, photographic, and many others, used more than 700,000 tons of various colorings produced from around 100,000 kinds of commercial synthetic dyes (Nur et al., 2022 ). Dye pollution discharged from these industries is a serious environmental problem, such as the textile industry is utilized an amount of dyestuff at approximately 10 000 tons per year worldwide (Katheresan et al., 2018 ). Methods for the degradation of dyes in water by different techniques such as adsorption, absorption, ion exchange, photocatalysis, etc, have been developed (Ahmed et al., 2017 ; Sultana et al., 2022 ; Zhou et al., 2021 ). Among these methods, photocatalysis is an inexpensive, green, and environmentally friendly process that provides full degradation of dyes with no production of secondary pollution (Sirisha et al., 2022 ) Titanium dioxide (TiO 2 ) is an important semiconductor photocatalyst used for the treatment of dye pollution (Li et al., 2018 ). Titanium exists as different polymorphs with various physical properties such as brookite, anatase, and rutile phases (Besançon et al., 2016 ). Among them, the anatase phase of TiO 2 is the preferable semiconductor because of its long-term photostability, commercial availability, low toxicity, and excellent semiconductor which is a bandgap of 3.2 eV (Lachheb et al., 2011 ; Nur et al., 2022 ; Wei et al., 2018 ). However, photocatalytic efficiency is limited by several parameters such as low surface area, agglomeration of nanoparticles in aqueous media, and defective crystal structure (Mehta et al., 2016 ).Also, nano-TiO 2 particles have separation and recycling problems thus limiting their application on an industrial scale (Castanheira et al., 2022 ). One of the possible solutions to overcoming these limitations is the immobilization of TiO 2 in the mesoporous silica SBA-15 (Acosta-Silva et al., 2011 ; Araújo et al., 2016 ; Besançon et al., 2016 ; Calzada et al., 2019 ; Conceição et al., 2017 ; Liou et al., 2018 ; Mehta et al., 2016 ; Wei et al., 2018 ). SBA-15 is an ideal support material owing to uniform hexagonal pores with a high specific surface area, narrow size distribution, good thermal and chemical stability, tunable surface composition, low cost, and biodegradable template (Diagboya & Dikio, 2018 ; Li et al., 2018 ; Yuan et al., 2020 ). Different synthesizing methods have been employed to functionalize SBA-15 with TiO 2 reported by several authors in the literature, the comparing results of these methods are given in Table 1 . In most reports reviewed, the obtained TiO 2 nanoparticles in the synthesized materials were anatase phase, and TiO 2 /SBA-15 photocatalysts gave approximately seven times higher photocatalytic activity than commercial P25 Degussa or other synthesized nanoparticles form, verifying the advantage of incorporating the TiO2 in the SBA-15 matrix (Acosta-Silva et al., 2011 ; Sanches et al., 2018 ; Wei et al., 2018 ). As seen in Table 1 , TiO 2 /SBA-15photocatalysts have been prepared by the post-synthesis method and direct synthesis under hydrothermal conditions with different titanium sources and loading amounts (Acosta-Silva et al., 2011 ; Besançon et al., 2016 ; Conceição et al., 2017 ; Lachheb et al., 2011 ; Li et al., 2018 ; Liou et al., 2018 ; Wei et al., 2018 ). In the post-synthesis method, TiO 2 particles incorporated into the surface of the SBA-15 displayed high photocatalytic activity as TiO 2 particles were more accessible to the reactants. However, should TiO 2 loading increase too much, the activity decreases due to cluster formation. The optimum TiO2 loadings determined in these reports were given in Table 1 . On the other hand, direct synthesis method requires the simultaneous addition of the precursors of SBA-15 and TiO 2 . This method achieves the titania heteroatom partial substitute into the silica skeleton (Thunyaratchatanon et al., 2017 ), the easier to perform than the post-synthesis method (Qiang et al., 2019 ), and provides the uniform distribution of TiO 2 nanoparticles in the SBA-15 matrix keeping the mesostructure of the SBA-15 (Tomer et al., 2015 ). The amount of titanium oxide is of critical importance because it affects the mesoporous structure of the SBA-15 in this method, too. The low loadings of TiO 2 in SBA-15 could be achieved because titania clusters would dissolve under the acidic synthesis environment of SBA-15 (Lin et al., 2018 ). Also, this is observed that the obtained Si/Ti molar ratio is approximately two or three times lower than the theoretical value in some study in the literature (Araújo et al., 2016 ; Conceição et al., 2017 ; Tomer et al., 2015 ). These two methods tend to produce TiO 2 particle agglomeration at high loading and use expensive titanium alkoxides as the titania source as seen in Table 1 . The rapid hydrolysis of the organic titania source causes the production of non-homogeneously dispersion of particles, therefore unpractical for industrial production (Li et al., 2018 ; Lin et al., 2018 ). To eliminate the disadvantage of these methods, the use of inexpensive titanium sources such as TiO 2 nano-powder during the direct synthesis of Ti/SBA-15 can provide an opportunity to condensate TiO 2 nanoparticles as a unique and specific active site in the mesostructure. In this study, it has been used by a one-step hydrothermal method with TiO 2 nano-powder as a titanium source. The effect of the silica/titania ratio on photocatalytic activity has been studied. The synthesized photocatalysts have been characterized by kinds of different analytical methods; XRD, SEM-EDX, UV-DRS, and N2 adsorption-desorption isotherms. The photocatalytic efficiency of the synthesized TiO 2 /SBA-15 photocatalysts has been investigated by the degradation of methylene blue under UV irradiation. Also, the reusability and stability of TiO 2 /SBA-15 photocatalysts have been tested for five runs. After five runs, the reused photocatalysts have been characterized by XRD, SEM-EDX, and N2 adsorption-desorption isotherms to determine the structural deviation. Table 1 Recently reported photocatalytic systems for TiO 2 /SBA-15 synthesis by different methods TiO 2 Sources TiO 2 loading on SBA-15 Synthetic Methods Pollutants Reaction Conditions Catalytic Efficiency (%), Time (min) References Titanium Isopropoxide Ti/Si = 0.43 Sol–Gel Method Methylene Blue C MethyleneBlue = 50.0 µM, C Cat . = 1.75 g/L, pH 4.0, UV 100%, 180 (Liou et al., 2018 ) Titanium (IV) Oxide (Anatase) Ti/Si = 1.3 Sol–Gel Method Amicarbazone C Amicarbozone = 41.4 µM, C Cat = 0.5 g/L, pH = 5.0, UV 100%, 120 (Conceição et al., 2017 ) Titanium Isopropoxide Ti/Si = 8 Sol–Gel Method Methylene Blue C MethyleneBlue =30.0 mg/L C Cat . = 0.5 g/L, UV 98%, 210 (Lachheb et al., 2011 ) Titanium (IV) Isopropoxide 31 wt % Post-Synthesis Method Methylene Blue C MethyleneBlue =40.0 ppm, C Cat =0.3 g/L, mercury lamp, under air flow 90%, 255 (Acosta-Silva et al., 2011 ) Ilmenite 26 wt % Post-Synthesis Hydrolysis Dimethoate C Dimethoat e= 30 mg/L, C Cat = 1.67 g/L, pH = 12, UV 100%, 420 (Li et al., 2018 ) Tetrabutyl Titanate 41.5 wt % Modified Implantation Methylene Blue C MethyleneBlue =30.0 mg/L, C Cat =0.48 g/L, UV 85%, 150 (Wei et al., 2018 ) Titanium Isopropoxide 44 wt % Post-Synthesis Method Methyl Orange C methyl orange = 16 mg/L, C Cat = 0.5 g/L 100%, 90 (Besançon et al., 2016 ) Metatitanic Acid 17wt % Post-Synthesis Method Methyl Orange C methyl orange = 50 mg/L, C Cat = 1.33 g/L, Mercury Lamp 98%, 50 (Wang et al., 2013 ) Titanium Butoxide 5 wt% Microwave-Assisted Technique Alizarin Dye C Alizarin = 100 mg/L, C Cat = 1 g/L, UV 98%, 60 (Mehta et al., 2016 ) 2. Experimental Section 2.1. Chemicals Tetraethyl orthosilicate (TEOS), Pluronic-123 ((triblock poly(ethylene oxide)–poly(propylene oxide)–poly(ethylene oxide) were obtained from Sigma Aldrich. HCl (37%) were supply form Riedel-de Haen. TiO 2 nano-powder was bought from Merck, and its molecular weight of 79.90 g/mol. Methylene blue was obtained from Merck, and its molecular weight of 319.85 g/mol. 2.2. Synthesis SBA-15 synthesis method was described previously in the our previous work (Akbay & Ölmez, 2018 ). A series of TiO 2 /SBA-15 photocatalysts were prepared by modifying SBA-15 synthesis methods. In this method, 4 g of Pluronic-123 was mixed with 30 ml of distilled water in a magnetic stirrer at 35°C for 3 hours before adding 150 ml of 2 M HCl to the solution. In this step, the desired amount of TiO 2 nano-powder was added and stirring for 2 hours, then TEOS of 9 ml was added to the solution containing. The mixture was stirred for 20 h at 313 K and was permitted to react at 373 K during the overnight in Teflon containers. The solid product was filtered and washed with deionized water to extract excess HCl. Drying was carried out at 30°C for 45 h, and calcination was applied at 600°C under airflow for 5.5 hours. The products were designated as TiO 2 /SBA-15 ( R ), where R was the ratio of Si/Ti. The TiO 2 /SBA-15 catalyst synthesized with different amounts of TiO 2 is named according to the Si/Ti molar ratios as given are in Table S1. 2.3. Characterization Low and wide-angle X-ray diffraction (XRD) analyses were carried out by using an X-ray diffractometer (RigakuRind XRD MiniFlex 300/600) and Cu-Kα (1.54 Aº) radiation (40kV-15mA). The scanning was performed from 2ϴ=70° to 2ϴ=5° at a rate of 2° min − 1 . Additionally, the crystallite sizes of the photocatalysts were calculated by using Scherrer’s equation of D = kλ/βcosθ where D is crystallite diameter, λ is the radiation wavelength (1.5406Å), β is the peak full with that half maximum (FWHM), θ is the diffracting angle and k = 0.90 for spherical shape particle. To obtain information about the surface morphology of the catalysts, images were taken at various magnifications on the HITACHI TM 3030 Plus branded SEM device. Rigaku ZSX Primus II brand device was used for XRF analysis. The BET (Brunauer–Emmett–Taller) specific surface area was obtained from an N2 adsorption-desorption isotherms measured at 77 K in an automatic adsorption apparatus (Tristar II 3020 Operator Manual v3.02, Micrometric). Before measurement, photocatalysts were degassed at 250ºC for about 4 h. The pore size distributions of catalysts were calculated by Barrett–Joyner–Halenda (BJH) method. UV Diffuse Reflectance Spectra (DRS) were done from the range of 200 to 700 nm using a UV–vis spectrophotometer (Shimadzu UV-3600). 2.4. Photocatalytic runs Activities of synthesized photocatalysts was investigated by degradation of methylene blue. Photocatalytic experiments were carried out in a quartz reactor system with temperature controller. The reactor system included a thin layer of aluminum foil with a purity of 99%. The light source was four 8 W UV lamps (364nm) low-pressure mercury lamps. In a typical run, methylene blue of 150 ml with 20 ppm concentration at natural pH was prepared and then a known amount of catalyst (given in Table 2 S) whose TiO 2 content was equal to 6 mg, was added to the solution because only the semiconductor particles have the photocatalytic activity. For obtaining the adsorption-desorption equilibrium the reaction mixture was magnetically stirred in the dark for 1 h before the irradiation. By taken 2 ml of the reaction mixture, the catalyst was removed by centrifugation at 13000 rpm for 20 min. at given time intervals. The concentration of the samples was determined by using the spectrophotometric method (SHIMADZU UV-2600 UV Spectrophotometer device). The decrease in the intensity of the absorption band of the methylene blue spectra, typically at 664 nm, was used to follow the degradation of the methylene blue solution. The degradation efficiency of methylene blue was calculated by the following equation: where C 0 and C are the concentration of the initial and the concentration of methylene blue at a specific interval of time, respectively. 2.5. Reusability After complete photocatalytic experiments, the catalyst was recollected through centrifugation and reused five times to check the stability and reusability of the photocatalyst under the same experimental conditions. Before the next cycle, the catalyst was washed with ethanol and dried on filter paper to separate the methylene blue trapped in the photocatalyst. The catalyst was refreshed in two ways; the first is the direct use of the dried sample after filtration, and the second is the use of the photocatalyst after calcination. The calcination was carried out in an airflow oven at 400°C for 2 hours. 3. Results And Discussions To investigate the structural, textural and morphological change stimulated by the silica/titania ratio on the TiO 2 /SBA-15 photocatalyst, a combination of XRD, SEM-EDX, N2 adsorption-desorption isotherms, XRF, and UV-DRS were employed. The activity and stability of the synthesized TiO 2 /SBA-15 photocatalysts were investigated by the degradation of methylene blue under UV irradiation. Also, reused catalysts were characterized for the determination of the structural deviation. 3.1. Characterization Results The synthesized photocatalysts were characterized by using low-angle and wide-angle XRD patterns shown in Fig. 1 a and b. As seen in Fig. 1 a, the XRD patterns display a reflection peak the characteristic of mesoporous silica SBA-15 and is in agreement with the literature (Sanches et al., 2018 ). The main peak at 2Ɵ̴̴̴̴≅0.8° (100) is related to the cylindrical hexagonal geometric structure of SBA-15, and two broad diffraction peaks of low intensity 1.5° (110), 1.7° (200), and crystallographic planes, respectively. These peaks are the reflection of the p6mm space group, the ordered 2D hexagonal mesostructure (Tomer et al., 2015 ). These peaks, showing the characteristics of SBA-15 in the synthesized TiO 2 /SBA-15 catalysts, proved that the TiO 2 /SBA-15(R) synthesis was successful and the SBA-15 pore structure and channels did not deteriorate. The insertion of titania created the peak shift to higher 2Ɵ̴̴̴̴ angles on the reflection plane (100) and no decrease in all diffraction peaks. Therefore, no contradiction of lattice parameter (a 0 ) of photocatalyst, obtained from the d100 spacing included in Table 2 , was observed. All lattice parameters have small variations from the SBA-15, which may be caused by the incorporation of TiO 2 into the SBA-15 mesoporous walls (Nogueira et al., 2013 ). The crystallite size of TiO 2 in TiO 2 /SBA-15 was calculated according to the Scherrer formula; the results are shown in Table 2 . The catalyst crystallite size approximately has the similar value at all contents because of pore diameter restrictions. Also, the very weak peaks attributed to the (110) and (200) diffraction planes reveal that the pore properties of SBA-15 were slightly affected by the decreasing R ratios (Fig. 1 a), indicating that the titania particles incorporated into the silica framework prevent the collapse of the SBA-15 mesostructure. This assumption was also confirmed by SEM. Wide-angle XRD patterns of synthesized catalysts have confirmed the presence of any crystalline species in the mesoporous TiO 2 /SBA-15 (R) catalyst (Fig. 1 b). As seen in Fig. 1 b, TiO 2 /SBA-15(R) catalysts have patterns with a broad peak centered at 2θ ≅ 23° corresponding to the amorphous silica walls of the SBA-15(Acosta-Silva et al., 2011 ). The new diffraction peaks that appeared at ≅ 25°(101), 38° (004), 48° (200), 54° (105), 55° (211), and 63° (204) exhibit the crystal structure of anatase TiO 2 and no diffraction peaks were detected that confirmed the rutile TiO 2 phase whereas the pure-TiO 2 shows both anatase (JCPDS card no. 01-084-1285) and rutile phase (JCPDS card no. 01-088-1172), which indicates that the rutile phase was completely transformed into anatase phase during the synthesis of the photocatalyst. Also, the increase in peak intensity with decreasing R indicates the increment in TiO 2 loading in the mesoporous silica framework (Araújo et al., 2016 ; Calzada et al., 2019 ). To examine the morphological structure of synthesized SBA-15 and TiO 2 /SBA-15(R) photocatalysts, SEM images were taken at various magnifications at 15 kV, and the results are given in Fig. 2 . As seen in Fig. 2 a, the SBA-15 has agglomerated tubular-like morphology (Tamizhdurai et al., 2021 ). SEM images of TiO 2 /SBA-15(R) catalysts given in Fig. 2 b-e. SBA-15 retained the filamentous structure to prevent the collapse of the silica mesostructure after titania nanoparticles were inserted into the silica framework. It was observed that titanium particles were distributed evenly on the SBA-15 pore walls in TiO 2 /SBA-15 photocatalysts. SEM-EDX and XRF analyses were performed to detect the chemical composition of the photocatalysts (Table 1 ). As seen in Table 2 , the Si/Ti molar ratios are close to the expected nominal ratios, calculated values by SEM-EDX and XRF. The numerical difference between the SEM-EDX and XRF results is because SEM-EDX analysis is performed on the sample surface and the other on the bulk. The Si/Ti molar ratios obtained by XRF are very good compared to the study conducted by Araujo et al. (2016)(Araújo et al., 2016 ) found about two times lower than the expected value despite using the TiO 2 nano-powders as a titanium source. The textural properties of the SBA-15 and TiO 2 /SBA-15(R) samples were studied by the N2 adsorption-desorption isotherms method. N2 adsorption-desorption isotherms and the pore size distributions curves of synthesized SBA-15 and TiO 2 /SBA-15(R) were given by using the BJH model from the desorption branch, are displayed in Fig. 3 , and the related textual data of the synthesized photocatalyst are given in Table 2 . The synthesized SBA-15 and TiO 2 /SBA-15(R) exhibited type IV characteristic curves with type H1 hysteresis loop, according to the IUPAC classification (Acosta-Silva et al., 2011 ). The SBA-15 presented the hysteresis loop at high relative pressures (0.6 < p/p 0 < 0.8) in a range of representing the self-filling of mesopores due to capillary condensation and indicating the presence of uniform mesopores. The synthesized TiO 2 /SBA-15(R) photocatalysts (lower R values than 16) showed a hysteresis loop with a little bit low relative pressure ranges (0.5 < p/p 0 < 0.8) due to the reduction in mesopores size with some of the small TiO 2 particles dispersed in the pores of SBA-15 (Wei et al., 2018 ). In TiO 2 /SBA-15(R) photocatalysts, especially R = 16 and 64, the hysteresis loop is some open over the P/Po region of 0.8, displays that the SBA-15 pores are slightly clogged by TiO 2 nanoparticles (Devi et al., 2018 ). In Fig. 3 b, SBA-15 exhibited a uniform, narrow pore size distribution in the range of 65–85 Aͦ, which is the characteristic of mesoporous materials (Qiang et al., 2019 ). There appears to be a pore size peak shifted to a smaller range at high TiO 2 loading (lower R values than 16), whereas; the pore size peak has the same as SBA-15 at low TiO2 loading, indicating TiO 2 particles inserted into the mesostructure of SBA-15 in TiO2/SBA-15(R) photocatalyst (R values up to 16). Table 2 Structural, chemical, and textural properties of SBA-15 and TiO 2 /SBA-15 Catalyst Stoichiometric ratio Si/Ti Crystallite sizes of TiO 2 (nm) a Surface Area BET a (m 2 /g) Pore Volume b (cm 3 /g) Pore Diameter (nm) b Lattice parameter a 0 (nm) a Pore Wall Thickness nm d Band Gap energy (eV) f Theoretical ratio Determined by XRF Determined by SEM-EDX SBA-15 - - - - 732 0,89 5,95 13,33 7,38 2.37 TiO 2 /SBA-15 (R = 64) 64 68 54 11,27 621 0,83 5,84 13,01 7,26 3.30 TiO 2 /SBA-15 (R = 32) 32 34 41 11,61 616 0,81 5,64 13,41 7,77 3.31 TiO 2 /SBA-15 (R = 16) 16 15 13 11,23 609 0,76 5,45 12,97 7,52 3.31 TiO 2 /SBA-15 (R = 11) 11 13 7 11,23 593 0,76 5,41 12,97 7,56 3.31 TiO 2 /SBA-15 (R = 8) 8 10 6 10,98 541 0,64 5,16 12,68 7,52 3.32 TiO 2 /SBA-15 (R = 6) 6 7 8 11,09 583 0,67 5,21 12,81 7,60 3.32 a from XRD, a Multipoint BET method., b from BJH method., d Wall thickness (a 0 − pore diameter)., f fron UV-DRS As seen in Table 2, the surface area of SBA-15was found to be 732 m 2 /g, and falls within the range of high-quality SBA-15 as 500–1300 m 2 /g (Zhan et al., 2014). Although the surface area and pore volume decreased slightly after TiO 2 loading, the BET area values of TiO 2 /SBA-15(R) are still high as the range 621–583 m 2 /g. Additionally, the decrease in R values is ideal for promoting an increase in the wall thickness. These effects may be due to the presence of TiO 2 nanocrystals in the SBA-15 mesopores and is complied with the XRD and SEM results (Han et al., 2011; Malik et al., 2016). DRS analyses of synthesized TiO 2 /SBA-15(R) photocatalysts were performed and given in Figure 4. It was observed that all samples have an absorption band at wavelengths from 250 to 380 nm, and the large absorption drop around 380 nm, which is complied with the absorb on the bandgap of anatase TiO 2 (Chang et al., 2016; Wróblewska et al., 2018). The adsorption edges of TiO 2 /SBA-15(R) photocatalysts are slightly blue-shifted with increasing R ratios, indicating that the SBA-15 effectively suppresses the agglomerate of TiO 2 nanoparticles. Also, the strong adsorption peak at about 350–400 nm demonstrate the TiO 2 particle whose size is the larger than 5 nm (Acosta-Silva et al., 2011). These observations are in good agreement with XRD results. The bandgap energy (E g ) was found by using the modified plot of the Kubelka–Munk function given in Figure S1 and Table 2 (García et al., 2021 ). The calculated values of the optical band gap energies were considerably blue-shifted compared with that of TiO 2 anatase phase (3.2 eV) (García et al., 2021 ). The increment in the bandgap energies of TiO 2 /SBA-15s is indicative of quantization effects (Araújo et al., 2016 ), which improves the photocatalytic properties. 3.2. Photocatalytic activity Photocatalytic activities of TiO 2 /SBA-15(R) were evaluated by degradation of methylene blue under UV-light irradiation. To compare their catalytic efficiencies, the amount of active TiO 2 inserted in SBA-15, or TiO 2 nano powder is the same, which is 6 mg of TiO 2 .Results of photocatalyst efficiencies of TiO2/SBA-15(R) photocatalysts are given with and without adsorption in Figs. 5 a and b. As seen in Fig. 5 , blank tests were carried out in the absence of a photocatalyst no methylene blue degradation was observed (Fig. 5 b). The second test was made in the presence of SBA-15, the concentration of methylene blue, no changed after the light was turned on, indicating the SBA-15 reached the adsorption equilibrium of methylene blue (Fig. 5 a). It is obvious that SBA-15 has no photocatalytic activity due to having no radical groups in an amorphous silica structure (Araújo et al., 2016 ). Therefore, all catalyst in methylene blue solution were stirred for 1 h for adsorption equilibrium. TiO 2 nano powder have low photoactivity (27.52%) due to the poor dispersion of active phases. Its photocatalytic efficiency is increased as a result of high dispersion of TiO 2 into the SBA-15 in all synthesized photocatalyst. This result shows that the titanium incorporated into SBA-15 framework is enhanced the photoactivity of TiO 2 . As seen in Fig. 5 b, methylene blue degradation efficiencies are 57%, 67.5%, 61.7%, 79.6%, 70.9%, and 75.6% with increasing R ratios, respectively. Among them, TiO 2 /SBA-15 (R = 16) presented the best photocatalytic performance. Therefore, the improved photocatalytic activity should be attributed to the insert of the TiO 2 particles in the SBA-15 pore walls with an increase in Ti amount (R; 64, 32, and 16). At the lower R values than 16, decreasing efficiency in the photocatalytic activity may depend on clogging of TiO 2 particles in mesopore channels of SBA-15. Also, this phenomenon is seen in the pore distribution curve in Fig. 3 b. These results show that good TiO 2 dispersion into the SBA-15 reveals more active sites near the adsorbed dye molecules, resulting in an increase in degradation rates. 3.3. Reusability Catalyst reusability is one of the major factors in the photocatalytic degradation industries. The reusability studies were conducted on the TiO 2 /SBA-15 (R = 16) catalyst for five runs given in Fig. 6 . Each of run was examined by using the fresh dye solution in the presence of the same amount of the used catalyst, refreshed with and without calcination described in the Experimental Section. As seen in Fig. 6 , the activity of the reused catalyst with and without calcination in the fifth run was the same as that of the fresh catalyst. Therefore, photocatalyst could use for long periods without loss of activity. After the fifth run, the used catalyst was characterized by XRD, SEM-EDX, and N2 adsorption-desorption isotherms/desorption analyses, and results are given in Figures S2, S3, and S4 and Table S3. It is seen in Figure S2, reused catalyst retained the crystal structure of anatase TiO 2 and the hexagonal structure of SBA-15. The photocatalyst still had type IV characteristic curves with a type H1 hysteresis loop. Pore distribution curves show that some pore-clogging occurs without calcination due to the adsorption of methylene blue on the catalyst while the pore size changed slightly, from 5.45 to 4.75 nm during the calcination process. As seen in Table S3, the calcined catalyst BET surface area, pore-volume, and diameter values were higher than the fresh catalyst and reused catalyst without calcination because of the removal of the dye remaining in the pores during the calcination process performed in each of run. Photocatalyst activity and stability was maintained after reuse for several cycles. 4. Conclusions In this study, a series of TiO 2 /SBA-15 photocatalysts were synthesized by a one-step hydrothermal method with TiO 2 nano-powder as a titanium source. The effect of the Si/Ti molar ratios on photocatalytic activity has been studied. The photocatalysts were characterized by several different analytical methods. Results showed that the amorphous structure of the SBA-15 is preserved with a highs distribution of TiO2 in the synthesized photocatalysts. Si/Ti molar ratios of TiO 2 /SBA-15 catalysts are compatible with theoretical ratios. BET surface areas and pore volumes of TiO 2 /SBA-15 decreased slightly after TiO 2 loading because of TiO 2 nanoparticle incorporation into the SBA-15 pore walls. But the pore size distribution curve shifted to a smaller range at high TiO 2 loading, whereas; the curve has the same as SBA-15 at low TiO 2 loading, indicating TiO 2 particles inserted into the mesostructure of SBA-15 into TiO 2 /SBA-15 catalyst (R values up to 16). Also, optical band gap energies slowly increase as TiO 2 amount increases for TiO 2 /SBA-15 photocatalysts. The photocatalytic efficiency of TiO2/SBA-15 has been investigated by the degradation of methylene blue under UV irradiation. The highest photocatalytic efficiency (79.6%) was obtained in the TiO 2 /SBA-15(R = 16). These results are coincided with pore distribution curve. The superior photocatalytic efficiencies of the TiO 2 /SBA-15 could be attributed to the high surface area and better dispersion of TiO 2 in SBA-15 pore walls. Also, the reusability and stability of TiO 2 /SBA-15 photocatalysts are still good for five runs. Due to their high reusability efficiency, easy separation, environment-friendly nature along with good photocatalytic performance, these photocatalysts may have sustainable potential for wastewater treatment in practical applications. Declarations Acknowledgment This study was supported by Eskişehir Technical University Scientific Research Projects Commission under grant no: 22ADP043. Declaration of Competing Interest The authors report no declarations of interest. Author Contribution Elif Akbay led the project; Sevgican Göl performed the experiment and the data analyses; Elif Akbay performed the characterization analysis and their discussion; Sevgican Göl and Elif Akbay contributed to the preparation of the manuscript. References Acosta-Silva YJ, Nava R, Hernández-Morales V, Macías-Sánchez SA, Gómez-Herrera ML, Pawelec B (2011) Methylene blue photodegradation over titania-decorated SBA-15. 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J Mol Struct 1170:9–17. https://doi.org/https://doi.org/10.1016/j.molstruc.2018.05.044 Sirisha U, Sowjanya B, Anjum R, Punugoti H, Mohamed T, Vangalapati M (2022) Synthesized TiO2 nanoparticles for the application of photocatalytic degradation of synthetic toxic dye acridine orange. Materials Today: Proceedings . https://doi.org/https://doi.org/10.1016/j.matpr.2022.04.278 Sultana M, Rownok MH, Sabrin M, Rahaman MH, Alam SMN (2022) A review on experimental chemically modified activated carbon to enhance dye and heavy metals adsorption. Clean Eng Technol 6:100382. https://doi.org/https://doi.org/10.1016/j.clet.2021.100382 Tamizhdurai P, Narayanan S, Kumaran R, Mangesh VL, Kavitha C, Vidhya Lakshmi N, Ragupathi C, Alothman ZA, Ouladsmane M, & G, M (2021) Catalytic activity of ratio-dependent SBA-15 supported cerium/Pt catalysts for highly selective oxidation reaction of benzyl alcohol to benzaldehyde. Adv Powder Technol 32(11):4286–4294. https://doi.org/https://doi.org/10.1016/j.apt.2021.09.033 Thunyaratchatanon C, Luengnaruemitchai A, Chaisuwan T, Chollacoop N, Chen S-Y, Yoshimura Y (2017) Synthesis and characterization of Zr incorporation into highly ordered mesostructured SBA-15 material and its performance for CO2 adsorption. Microporous Mesoporous Mater 253:18–28. https://doi.org/https://doi.org/10.1016/j.micromeso.2017.06.015 Tomer VK, Jangra S, Malik R, Duhan S (2015) Effect of in-situ loading of nano titania particles on structural ordering of mesoporous SBA-15 framework. Colloids Surf A 466:160–165. https://doi.org/https://doi.org/10.1016/j.colsurfa.2014.11.025 Wang X-j, Li F-t, Hao Y-j, Liu S-j, Yang M-l (2013) TiO2/SBA-15 composites prepared using H2TiO3 by hydrothermal method and its photocatalytic activity. Mater Lett 99:38–41. https://doi.org/https://doi.org/10.1016/j.matlet.2013.02.060 Wei JQ, Chen XJ, Wang PF, Han YB, Xu JC, Hong B, Jin HX, Jin DF, Peng XL, Li J, Yang YT, Ge HL, Wang XQ (2018) High surface area TiO2/SBA-15 nanocomposites: Synthesis, microstructure and adsorption-enhanced photocatalysis. Chem Phys 510:47–53. https://doi.org/https://doi.org/10.1016/j.chemphys.2018.05.012 Wróblewska A, Miądlicki P, Sreńscek-Nazzal J, Sadłowski M, Koren ZC, Michalkiewicz B (2018) Alpha-pinene isomerization over Ti-SBA-15 catalysts obtained by the direct method: The influence of titanium content, temperature, catalyst amount and reaction time. Microporous Mesoporous Mater 258:72–82. https://doi.org/https://doi.org/10.1016/j.micromeso.2017.09.007 Yuan S, Wang M, Liu J, Guo B (2020) Recent advances of SBA-15-based composites as the heterogeneous catalysts in water decontamination: A mini-review. J Environ Manage 254:109787. https://doi.org/https://doi.org/10.1016/j.jenvman.2019.109787 Zhan W, Yao J, Xiao Z, Guo Y, Wang Y, Guo Y, Lu G (2014) Catalytic performance of Ti-SBA-15 prepared by chemical vapor deposition for propylene epoxidation: The effects of SBA-15 support and silylation. Microporous Mesoporous Mater 183:150–155. https://doi.org/https://doi.org/10.1016/j.micromeso.2013.08.038 Zhou R, Jiang Y, Zhao H, Ye B, Wang L, Hou Z (2021) Synthesis of solketal from glycerol over modified SiO2 supported p-phenolsulfonic acid catalyst. Fuel 291:120207. https://doi.org/https://doi.org/10.1016/j.fuel.2021.120207 Supplementary Files Highlights.docx Supplementarydata.docx Cite Share Download PDF Status: Published Journal Publication published 13 Nov, 2023 Read the published version in ChemistrySelect → Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-1831676","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":120053900,"identity":"d9eba7e8-3934-4a04-a7bf-5af51945245d","order_by":0,"name":"Sevgi Can Göl","email":"","orcid":"","institution":"Eskisehir Teknik Universitesi","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Sevgi","middleName":"Can","lastName":"Göl","suffix":""},{"id":120053901,"identity":"a586138f-c62c-4110-9225-ffaa3b6b3c08","order_by":1,"name":"Elif Akbay","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA7UlEQVRIiWNgGAWjYHACAwaGCgYGCWYGBmYQm4EhgRgtZ9C1HCCkhbENqIUBpIWBCC387M0bH/6cZ2Mv2c7+8HFBwT2gSI4B88c9uLVI9hwrNubdlpY4m5nH2HiGQTFQ5I0Bw4FneFx1I8dMmnHb4QQ5Zh42aR6DBJAIUAsel9nfyDH/+XPOf3s5Zvbnv0Fa7AlpMZDIMWPgbTjAOJuZwYwZbIsEAS0SZ44VS/McS06c2cxjDHIYj8SZZwUHzuDRwt/evPHjjxo7e4nzxx9+5vmTIMffnrzxQQUeLRiAB0SQomEUjIJRMApGARYAANruS5csBzvyAAAAAElFTkSuQmCC","orcid":"https://orcid.org/0000-0003-0323-7938","institution":"Eskisehir Teknik Universitesi","correspondingAuthor":true,"submittingAuthor":false,"prefix":"","firstName":"Elif","middleName":"","lastName":"Akbay","suffix":""}],"badges":[],"createdAt":"2022-07-06 13:46:14","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-1831676/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-1831676/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1002/slct.202301887","type":"published","date":"2023-11-14T00:00:00+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":23823047,"identity":"f9920431-761b-49b8-9546-1a6ba42852b8","added_by":"auto","created_at":"2022-07-13 16:37:56","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":127724,"visible":true,"origin":"","legend":"\u003cp\u003eWide-angle (a) and small-angle (b) XRD patterns of SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R) photocatalysts\u003c/p\u003e","description":"","filename":"ScreenShot20220712at3.46.05PM.png","url":"https://assets-eu.researchsquare.com/files/rs-1831676/v1/8a01ed7215192eb4867c394d.png"},{"id":23823049,"identity":"53a818a5-0d3b-4853-9f13-ffc97151d943","added_by":"auto","created_at":"2022-07-13 16:37:56","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":614459,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R) photocatalysts\u0026nbsp;\u003cstrong\u003e; \u003c/strong\u003ea) SBA-15, b) TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R=64), c) TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R=32), d) TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R=16), e) TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R=11), f) TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R=8), g) TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R=\u003cem\u003e6\u003c/em\u003e)\u003c/p\u003e","description":"","filename":"ScreenShot20220712at3.47.07PM.png","url":"https://assets-eu.researchsquare.com/files/rs-1831676/v1/60a532fef8cd4ebd867a1103.png"},{"id":23823509,"identity":"c00251fa-bcd9-42a9-ad9f-ec134842132c","added_by":"auto","created_at":"2022-07-13 16:42:56","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":123306,"visible":true,"origin":"","legend":"\u003cp\u003e(a) N\u003csub\u003e2\u003c/sub\u003e adsorption-desorption isotherms and (b) pore distributions of SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R) photocatalysts.\u0026nbsp;\u003c/p\u003e","description":"","filename":"ScreenShot20220712at3.47.18PM.png","url":"https://assets-eu.researchsquare.com/files/rs-1831676/v1/b4a80e493922d704029369c3.png"},{"id":23823511,"identity":"95427d63-10e6-431a-908c-0378fab593e2","added_by":"auto","created_at":"2022-07-13 16:42:56","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":63257,"visible":true,"origin":"","legend":"\u003cp\u003eDiffuse reflectance UV–vis spectra of SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R) photocatalysts\u0026nbsp;\u003c/p\u003e","description":"","filename":"Onlinefloatimage16.png","url":"https://assets-eu.researchsquare.com/files/rs-1831676/v1/20334bdaf333fe010c9157a1.png"},{"id":23823884,"identity":"8ba999f3-2e4c-47cc-83a9-9065f49e04c3","added_by":"auto","created_at":"2022-07-13 16:47:56","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":126377,"visible":true,"origin":"","legend":"\u003cp\u003eThe photocatalytic degradation efficiency of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R) photocatalysts with a) adsorption, and b) without adsorption\u003c/p\u003e","description":"","filename":"ScreenShot20220712at3.47.46PM.png","url":"https://assets-eu.researchsquare.com/files/rs-1831676/v1/4b69ebd555a858ffcd6f6fc0.png"},{"id":23823052,"identity":"28de43a4-2c3e-4b94-a9b5-023fa6a1a003","added_by":"auto","created_at":"2022-07-13 16:37:56","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":92112,"visible":true,"origin":"","legend":"\u003cp\u003eThe reusibility efficiency of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (16) photocatalysts a) with calcination, and b) without calcination\u003c/p\u003e","description":"","filename":"Onlinefloatimage19.png","url":"https://assets-eu.researchsquare.com/files/rs-1831676/v1/2ae76eefae702d43c2947293.png"},{"id":51192140,"identity":"8b84be30-e1d3-4ef3-b3ae-74da899086d9","added_by":"auto","created_at":"2024-02-15 17:20:53","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1623973,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-1831676/v1/cf0e34dd-e4b6-4f2c-a07f-c1c8498883f8.pdf"},{"id":23823510,"identity":"89122f57-4a32-469a-8e11-3a90a5373d7e","added_by":"auto","created_at":"2022-07-13 16:42:56","extension":"docx","order_by":6,"title":"","display":"","copyAsset":false,"role":"supplement","size":15136,"visible":true,"origin":"","legend":"","description":"","filename":"Highlights.docx","url":"https://assets-eu.researchsquare.com/files/rs-1831676/v1/9e54c20716880dbda5673688.docx"},{"id":23823054,"identity":"8e5f0162-2d14-444c-928c-5c010e4ec6c2","added_by":"auto","created_at":"2022-07-13 16:37:56","extension":"docx","order_by":7,"title":"","display":"","copyAsset":false,"role":"supplement","size":580404,"visible":true,"origin":"","legend":"","description":"","filename":"Supplementarydata.docx","url":"https://assets-eu.researchsquare.com/files/rs-1831676/v1/3131bca8d6a3ee85a09d422a.docx"}],"financialInterests":"","formattedTitle":"Reusable titania-SBA-15 photocatalyst synthesized by different silica/titania ratios for enhancing methylene blue photodegradation","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eIndustries utilizing dye which are dying, textile, cosmetics, plastics, pharmaceutical, photographic, and many others, used more than 700,000 tons of various colorings produced from around 100,000 kinds of commercial synthetic dyes (Nur et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). Dye pollution discharged from these industries is a serious environmental problem, such as the textile industry is utilized an amount of dyestuff at approximately 10 000 tons per year worldwide (Katheresan et al., \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). Methods for the degradation of dyes in water by different techniques such as adsorption, absorption, ion exchange, photocatalysis, etc, have been developed (Ahmed et al., \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2017\u003c/span\u003e; Sultana et al., \u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Zhou et al., \u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Among these methods, photocatalysis is an inexpensive, green, and environmentally friendly process that provides full degradation of dyes with no production of secondary pollution (Sirisha et al., \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e2022\u003c/span\u003e)\u003c/p\u003e \u003cp\u003eTitanium dioxide (TiO\u003csub\u003e2\u003c/sub\u003e) is an important semiconductor photocatalyst used for the treatment of dye pollution (Li et al., \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). Titanium exists as different polymorphs with various physical properties such as brookite, anatase, and rutile phases (Besan\u0026ccedil;on et al., \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). Among them, the anatase phase of TiO\u003csub\u003e2\u003c/sub\u003e is the preferable semiconductor because of its long-term photostability, commercial availability, low toxicity, and excellent semiconductor which is a bandgap of 3.2 eV (Lachheb et al., \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e2011\u003c/span\u003e; Nur et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Wei et al., \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). However, photocatalytic efficiency is limited by several parameters such as low surface area, agglomeration of nanoparticles in aqueous media, and defective crystal structure (Mehta et al., \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e2016\u003c/span\u003e).Also, nano-TiO\u003csub\u003e2\u003c/sub\u003e particles have separation and recycling problems thus limiting their application on an industrial scale (Castanheira et al., \u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). One of the possible solutions to overcoming these limitations is the immobilization of TiO\u003csub\u003e2\u003c/sub\u003e in the mesoporous silica SBA-15 (Acosta-Silva et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2011\u003c/span\u003e; Ara\u0026uacute;jo et al., \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Besan\u0026ccedil;on et al., \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Calzada et al., \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Concei\u0026ccedil;\u0026atilde;o et al., \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e2017\u003c/span\u003e; Liou et al., \u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Mehta et al., \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Wei et al., \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). SBA-15 is an ideal support material owing to uniform hexagonal pores with a high specific surface area, narrow size distribution, good thermal and chemical stability, tunable surface composition, low cost, and biodegradable template (Diagboya \u0026amp; Dikio, \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Li et al., \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Yuan et al., \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e2020\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eDifferent synthesizing methods have been employed to functionalize SBA-15 with TiO\u003csub\u003e2\u003c/sub\u003e reported by several authors in the literature, the comparing results of these methods are given in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. In most reports reviewed, the obtained TiO\u003csub\u003e2\u003c/sub\u003e nanoparticles in the synthesized materials were anatase phase, and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts gave approximately seven times higher photocatalytic activity than commercial P25 Degussa or other synthesized nanoparticles form, verifying the advantage of incorporating the TiO2 in the SBA-15 matrix (Acosta-Silva et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2011\u003c/span\u003e; Sanches et al., \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Wei et al., \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2018\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eAs seen in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e, TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15photocatalysts have been prepared by the post-synthesis method and direct synthesis under hydrothermal conditions with different titanium sources and loading amounts (Acosta-Silva et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2011\u003c/span\u003e; Besan\u0026ccedil;on et al., \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Concei\u0026ccedil;\u0026atilde;o et al., \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e2017\u003c/span\u003e; Lachheb et al., \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e2011\u003c/span\u003e; Li et al., \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Liou et al., \u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Wei et al., \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). In the post-synthesis method, TiO\u003csub\u003e2\u003c/sub\u003e particles incorporated into the surface of the SBA-15 displayed high photocatalytic activity as TiO\u003csub\u003e2\u003c/sub\u003e particles were more accessible to the reactants. However, should TiO\u003csub\u003e2\u003c/sub\u003e loading increase too much, the activity decreases due to cluster formation. The optimum TiO2 loadings determined in these reports were given in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e.\u003c/p\u003e \u003cp\u003eOn the other hand, direct synthesis method requires the simultaneous addition of the precursors of SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e. This method achieves the titania heteroatom partial substitute into the silica skeleton (Thunyaratchatanon et al., \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e2017\u003c/span\u003e), the easier to perform than the post-synthesis method (Qiang et al., \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2019\u003c/span\u003e), and provides the uniform distribution of TiO\u003csub\u003e2\u003c/sub\u003e nanoparticles in the SBA-15 matrix keeping the mesostructure of the SBA-15 (Tomer et al., \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e2015\u003c/span\u003e). The amount of titanium oxide is of critical importance because it affects the mesoporous structure of the SBA-15 in this method, too. The low loadings of TiO\u003csub\u003e2\u003c/sub\u003e in SBA-15 could be achieved because titania clusters would dissolve under the acidic synthesis environment of SBA-15 (Lin et al., \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). Also, this is observed that the obtained Si/Ti molar ratio is approximately two or three times lower than the theoretical value in some study in the literature (Ara\u0026uacute;jo et al., \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Concei\u0026ccedil;\u0026atilde;o et al., \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e2017\u003c/span\u003e; Tomer et al., \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e2015\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThese two methods tend to produce TiO\u003csub\u003e2\u003c/sub\u003e particle agglomeration at high loading and use expensive titanium alkoxides as the titania source as seen in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. The rapid hydrolysis of the organic titania source causes the production of non-homogeneously dispersion of particles, therefore unpractical for industrial production (Li et al., \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Lin et al., \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). To eliminate the disadvantage of these methods, the use of inexpensive titanium sources such as TiO\u003csub\u003e2\u003c/sub\u003e nano-powder during the direct synthesis of Ti/SBA-15 can provide an opportunity to condensate TiO\u003csub\u003e2\u003c/sub\u003e nanoparticles as a unique and specific active site in the mesostructure.\u003c/p\u003e \u003cp\u003eIn this study, it has been used by a one-step hydrothermal method with TiO\u003csub\u003e2\u003c/sub\u003e nano-powder as a titanium source. The effect of the silica/titania ratio on photocatalytic activity has been studied. The synthesized photocatalysts have been characterized by kinds of different analytical methods; XRD, SEM-EDX, UV-DRS, and N2 adsorption-desorption isotherms. The photocatalytic efficiency of the synthesized TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts has been investigated by the degradation of methylene blue under UV irradiation. Also, the reusability and stability of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts have been tested for five runs. After five runs, the reused photocatalysts have been characterized by XRD, SEM-EDX, and N2 adsorption-desorption isotherms to determine the structural deviation.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eRecently reported photocatalytic systems for TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 synthesis by different methods\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"7\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e Sources\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e loading on SBA-15\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eSynthetic Methods\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003ePollutants\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eReaction Conditions\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c6\"\u003e \u003cp\u003eCatalytic Efficiency (%), Time (min)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c7\"\u003e \u003cp\u003eReferences\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTitanium Isopropoxide\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTi/Si\u0026thinsp;=\u0026thinsp;0.43\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eSol\u0026ndash;Gel Method\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eMethylene Blue\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eC\u003csub\u003eMethyleneBlue\u003c/sub\u003e = 50.0 \u0026micro;M, C\u003csub\u003eCat\u003c/sub\u003e. = 1.75 g/L, pH 4.0, UV\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e100%, 180\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e(Liou et al., \u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e2018\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTitanium (IV) Oxide (Anatase)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTi/Si\u0026thinsp;=\u0026thinsp;1.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eSol\u0026ndash;Gel Method\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eAmicarbazone\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eC\u003csub\u003eAmicarbozone\u003c/sub\u003e= 41.4 \u0026micro;M, C\u003csub\u003eCat\u003c/sub\u003e = 0.5 g/L, pH\u0026thinsp;=\u0026thinsp;5.0, UV\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e100%, 120\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e(Concei\u0026ccedil;\u0026atilde;o et al., \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e2017\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTitanium Isopropoxide\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTi/Si\u0026thinsp;=\u0026thinsp;8\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eSol\u0026ndash;Gel Method\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eMethylene Blue\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eC\u003csub\u003eMethyleneBlue\u003c/sub\u003e=30.0 mg/L C\u003csub\u003eCat\u003c/sub\u003e. = 0.5 g/L, UV\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e98%, 210\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e(Lachheb et al., \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e2011\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTitanium (IV) Isopropoxide\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e31 wt %\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003ePost-Synthesis Method\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eMethylene Blue\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eC\u003csub\u003eMethyleneBlue\u003c/sub\u003e=40.0 ppm, C\u003csub\u003eCat\u003c/sub\u003e =0.3 g/L, mercury lamp, under air flow\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e90%, 255\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e(Acosta-Silva et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2011\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eIlmenite\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e26 wt %\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003ePost-Synthesis Hydrolysis\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eDimethoate\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eC\u003csub\u003eDimethoat\u003c/sub\u003ee= 30 mg/L, C\u003csub\u003eCat\u003c/sub\u003e = 1.67 g/L, pH\u0026thinsp;=\u0026thinsp;12, UV\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e100%, 420\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e(Li et al., \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2018\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTetrabutyl Titanate\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e41.5 wt %\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eModified Implantation\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eMethylene Blue\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eC\u003csub\u003eMethyleneBlue\u003c/sub\u003e=30.0 mg/L, C\u003csub\u003eCat\u003c/sub\u003e =0.48 g/L, UV\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e85%, 150\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e(Wei et al., \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2018\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTitanium Isopropoxide\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e44 wt %\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003ePost-Synthesis Method\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eMethyl Orange\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eC\u003csub\u003emethyl orange\u003c/sub\u003e = 16 mg/L, C\u003csub\u003eCat\u003c/sub\u003e = 0.5 g/L\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e100%, 90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e(Besan\u0026ccedil;on et al., \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2016\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eMetatitanic Acid\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e17wt %\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003ePost-Synthesis Method\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eMethyl Orange\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eC\u003csub\u003emethyl orange\u003c/sub\u003e = 50 mg/L, C\u003csub\u003eCat\u003c/sub\u003e = 1.33 g/L, Mercury Lamp\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e98%, 50\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e(Wang et al., \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e2013\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTitanium Butoxide\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e5 wt%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eMicrowave-Assisted Technique\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eAlizarin Dye\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eC\u003csub\u003eAlizarin\u003c/sub\u003e = 100 mg/L, C\u003csub\u003eCat\u003c/sub\u003e = 1 g/L, UV\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e98%, 60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e(Mehta et al., \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e2016\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e"},{"header":"2. Experimental Section","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1. Chemicals\u003c/h2\u003e \u003cp\u003eTetraethyl orthosilicate (TEOS), Pluronic-123 ((triblock poly(ethylene oxide)\u0026ndash;poly(propylene oxide)\u0026ndash;poly(ethylene oxide) were obtained from Sigma Aldrich. HCl (37%) were supply form Riedel-de Haen. TiO\u003csub\u003e2\u003c/sub\u003e nano-powder was bought from Merck, and its molecular weight of 79.90 g/mol. Methylene blue was obtained from Merck, and its molecular weight of 319.85 g/mol.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2. Synthesis\u003c/h2\u003e \u003cp\u003eSBA-15 synthesis method was described previously in the our previous work (Akbay \u0026amp; \u0026Ouml;lmez, \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). A series of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts were prepared by modifying SBA-15 synthesis methods. In this method, 4 g of Pluronic-123 was mixed with 30 ml of distilled water in a magnetic stirrer at 35\u0026deg;C for 3 hours before adding 150 ml of 2 M HCl to the solution. In this step, the desired amount of TiO\u003csub\u003e2\u003c/sub\u003e nano-powder was added and stirring for 2 hours, then TEOS of 9 ml was added to the solution containing. The mixture was stirred for 20 h at 313 K and was permitted to react at 373 K during the overnight in Teflon containers. The solid product was filtered and washed with deionized water to extract excess HCl. Drying was carried out at 30\u0026deg;C for 45 h, and calcination was applied at 600\u0026deg;C under airflow for 5.5 hours.\u003c/p\u003e \u003cp\u003eThe products were designated as TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (\u003cem\u003eR\u003c/em\u003e), where R was the ratio of Si/Ti. The TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 catalyst synthesized with different amounts of TiO\u003csub\u003e2\u003c/sub\u003e is named according to the Si/Ti molar ratios as given are in Table S1.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3. Characterization\u003c/h2\u003e \u003cp\u003eLow and wide-angle X-ray diffraction (XRD) analyses were carried out by using an X-ray diffractometer (RigakuRind XRD MiniFlex 300/600) and Cu-Kα (1.54 A\u0026ordm;) radiation (40kV-15mA). The scanning was performed from 2ϴ=70\u0026deg; to 2ϴ=5\u0026deg; at a rate of 2\u0026deg; min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. Additionally, the crystallite sizes of the photocatalysts were calculated by using Scherrer\u0026rsquo;s equation of D\u0026thinsp;=\u0026thinsp;kλ/βcosθ where D is crystallite diameter, λ is the radiation wavelength (1.5406\u0026Aring;), β is the peak full with that half maximum (FWHM), θ is the diffracting angle and k\u0026thinsp;=\u0026thinsp;0.90 for spherical shape particle.\u003c/p\u003e \u003cp\u003eTo obtain information about the surface morphology of the catalysts, images were taken at various magnifications on the HITACHI TM 3030 Plus branded SEM device. Rigaku ZSX Primus II brand device was used for XRF analysis. The BET (Brunauer\u0026ndash;Emmett\u0026ndash;Taller) specific surface area was obtained from an N2 adsorption-desorption isotherms measured at 77 K in an automatic adsorption apparatus (Tristar II 3020 Operator Manual v3.02, Micrometric). Before measurement, photocatalysts were degassed at 250\u0026ordm;C for about 4 h. The pore size distributions of catalysts were calculated by Barrett\u0026ndash;Joyner\u0026ndash;Halenda (BJH) method. UV Diffuse Reflectance Spectra (DRS) were done from the range of 200 to 700 nm using a UV\u0026ndash;vis spectrophotometer (Shimadzu UV-3600).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e2.4. Photocatalytic runs\u003c/h2\u003e \u003cp\u003eActivities of synthesized photocatalysts was investigated by degradation of methylene blue. Photocatalytic experiments were carried out in a quartz reactor system with temperature controller. The reactor system included a thin layer of aluminum foil with a purity of 99%. The light source was four 8 W UV lamps (364nm) low-pressure mercury lamps.\u003c/p\u003e \u003cp\u003eIn a typical run, methylene blue of 150 ml with 20 ppm concentration at natural pH was prepared and then a known amount of catalyst (given in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003eS) whose TiO\u003csub\u003e2\u003c/sub\u003e content was equal to 6 mg, was added to the solution because only the semiconductor particles have the photocatalytic activity. For obtaining the adsorption-desorption equilibrium the reaction mixture was magnetically stirred in the dark for 1 h before the irradiation. By taken 2 ml of the reaction mixture, the catalyst was removed by centrifugation at 13000 rpm for 20 min. at given time intervals. The concentration of the samples was determined by using the spectrophotometric method (SHIMADZU UV-2600 UV Spectrophotometer device). The decrease in the intensity of the absorption band of the methylene blue spectra, typically at 664 nm, was used to follow the degradation of the methylene blue solution. The degradation efficiency of methylene blue was calculated by the following equation:\u003c/p\u003e\u003cp\u003e\u003cimg 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\"\u003e\u003c/p\u003e \u003cp\u003ewhere C\u003csub\u003e0\u003c/sub\u003e and C are the concentration of the initial and the concentration of methylene blue at a specific interval of time, respectively.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003e2.5. Reusability\u003c/h2\u003e \u003cp\u003eAfter complete photocatalytic experiments, the catalyst was recollected through centrifugation and reused five times to check the stability and reusability of the photocatalyst under the same experimental conditions. Before the next cycle, the catalyst was washed with ethanol and dried on filter paper to separate the methylene blue trapped in the photocatalyst. The catalyst was refreshed in two ways; the first is the direct use of the dried sample after filtration, and the second is the use of the photocatalyst after calcination. The calcination was carried out in an airflow oven at 400\u0026deg;C for 2 hours.\u003c/p\u003e \u003c/div\u003e"},{"header":"3. Results And Discussions","content":"\u003cp\u003eTo investigate the structural, textural and morphological change stimulated by the silica/titania ratio on the TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalyst, a combination of XRD, SEM-EDX, N2 adsorption-desorption isotherms, XRF, and UV-DRS were employed. The activity and stability of the synthesized TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts were investigated by the degradation of methylene blue under UV irradiation. Also, reused catalysts were characterized for the determination of the structural deviation.\u003c/p\u003e \u003cdiv id=\"Sec9\" class=\"Section2\"\u003e \u003ch2\u003e3.1. Characterization Results\u003c/h2\u003e \u003cp\u003eThe synthesized photocatalysts were characterized by using low-angle and wide-angle XRD patterns shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ea and b. As seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ea, the XRD patterns display a reflection peak the characteristic of mesoporous silica SBA-15 and is in agreement with the literature (Sanches et al., \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). The main peak at 2Ɵ̴̴̴̴\u0026cong;0.8\u0026deg; (100) is related to the cylindrical hexagonal geometric structure of SBA-15, and two broad diffraction peaks of low intensity 1.5\u0026deg; (110), 1.7\u0026deg; (200), and crystallographic planes, respectively. These peaks are the reflection of the p6mm space group, the ordered 2D hexagonal mesostructure (Tomer et al., \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e2015\u003c/span\u003e). These peaks, showing the characteristics of SBA-15 in the synthesized TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 catalysts, proved that the TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) synthesis was successful and the SBA-15 pore structure and channels did not deteriorate.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe insertion of titania created the peak shift to higher 2Ɵ̴̴̴̴ angles on the reflection plane (100) and no decrease in all diffraction peaks. Therefore, no contradiction of lattice parameter (a\u003csub\u003e0\u003c/sub\u003e) of photocatalyst, obtained from the d100 spacing included in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e, was observed. All lattice parameters have small variations from the SBA-15, which may be caused by the incorporation of TiO\u003csub\u003e2\u003c/sub\u003e into the SBA-15 mesoporous walls (Nogueira et al., \u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e2013\u003c/span\u003e). The crystallite size of TiO\u003csub\u003e2\u003c/sub\u003e in TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 was calculated according to the Scherrer formula; the results are shown in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e. The catalyst crystallite size approximately has the similar value at all contents because of pore diameter restrictions. Also, the very weak peaks attributed to the (110) and (200) diffraction planes reveal that the pore properties of SBA-15 were slightly affected by the decreasing R ratios (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ea), indicating that the titania particles incorporated into the silica framework prevent the collapse of the SBA-15 mesostructure. This assumption was also confirmed by SEM.\u003c/p\u003e \u003cp\u003eWide-angle XRD patterns of synthesized catalysts have confirmed the presence of any crystalline species in the mesoporous TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R) catalyst (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eb). As seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eb, TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) catalysts have patterns with a broad peak centered at 2θ\u0026thinsp;\u0026cong;\u0026thinsp;23\u0026deg; corresponding to the amorphous silica walls of the SBA-15(Acosta-Silva et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2011\u003c/span\u003e). The new diffraction peaks that appeared at \u0026cong;\u0026thinsp;25\u0026deg;(101), 38\u0026deg; (004), 48\u0026deg; (200), 54\u0026deg; (105), 55\u0026deg; (211), and 63\u0026deg; (204) exhibit the crystal structure of anatase TiO\u003csub\u003e2\u003c/sub\u003e and no diffraction peaks were detected that confirmed the rutile TiO\u003csub\u003e2\u003c/sub\u003e phase whereas the pure-TiO\u003csub\u003e2\u003c/sub\u003e shows both anatase (JCPDS card no. 01-084-1285) and rutile phase (JCPDS card no. 01-088-1172), which indicates that the rutile phase was completely transformed into anatase phase during the synthesis of the photocatalyst. Also, the increase in peak intensity with decreasing R indicates the increment in TiO\u003csub\u003e2\u003c/sub\u003e loading in the mesoporous silica framework (Ara\u0026uacute;jo et al., \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Calzada et al., \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2019\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eTo examine the morphological structure of synthesized SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) photocatalysts, SEM images were taken at various magnifications at 15 kV, and the results are given in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e. As seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ea, the SBA-15 has agglomerated tubular-like morphology (Tamizhdurai et al., \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). SEM images of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) catalysts given in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eb-e. SBA-15 retained the filamentous structure to prevent the collapse of the silica mesostructure after titania nanoparticles were inserted into the silica framework. It was observed that titanium particles were distributed evenly on the SBA-15 pore walls in TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eSEM-EDX and XRF analyses were performed to detect the chemical composition of the photocatalysts (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). As seen in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e, the Si/Ti molar ratios are close to the expected nominal ratios, calculated values by SEM-EDX and XRF. The numerical difference between the SEM-EDX and XRF results is because SEM-EDX analysis is performed on the sample surface and the other on the bulk. The Si/Ti molar ratios obtained by XRF are very good compared to the study conducted by Araujo et al. (2016)(Ara\u0026uacute;jo et al., \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2016\u003c/span\u003e) found about two times lower than the expected value despite using the TiO\u003csub\u003e2\u003c/sub\u003e nano-powders as a titanium source.\u003c/p\u003e \u003cp\u003eThe textural properties of the SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) samples were studied by the N2 adsorption-desorption isotherms method. N2 adsorption-desorption isotherms and the pore size distributions curves of synthesized SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) were given by using the BJH model from the desorption branch, are displayed in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e, and the related textual data of the synthesized photocatalyst are given in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe synthesized SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) exhibited type IV characteristic curves with type H1 hysteresis loop, according to the IUPAC classification (Acosta-Silva et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2011\u003c/span\u003e). The SBA-15 presented the hysteresis loop at high relative pressures (0.6\u0026thinsp;\u0026lt;\u0026thinsp;p/p\u003csub\u003e0\u003c/sub\u003e\u0026thinsp;\u0026lt;\u0026thinsp;0.8) in a range of representing the self-filling of mesopores due to capillary condensation and indicating the presence of uniform mesopores. The synthesized TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) photocatalysts (lower R values than 16) showed a hysteresis loop with a little bit low relative pressure ranges (0.5\u0026thinsp;\u0026lt;\u0026thinsp;p/p\u003csub\u003e0\u003c/sub\u003e\u0026thinsp;\u0026lt;\u0026thinsp;0.8) due to the reduction in mesopores size with some of the small TiO\u003csub\u003e2\u003c/sub\u003e particles dispersed in the pores of SBA-15 (Wei et al., \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). In TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) photocatalysts, especially R\u0026thinsp;=\u0026thinsp;16 and 64, the hysteresis loop is some open over the P/Po region of 0.8, displays that the SBA-15 pores are slightly clogged by TiO\u003csub\u003e2\u003c/sub\u003e nanoparticles (Devi et al., \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e2018\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eIn Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eb, SBA-15 exhibited a uniform, narrow pore size distribution in the range of 65\u0026ndash;85 Aͦ, which is the characteristic of mesoporous materials (Qiang et al., \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). There appears to be a pore size peak shifted to a smaller range at high TiO\u003csub\u003e2\u003c/sub\u003e loading (lower R values than 16), whereas; the pore size peak has the same as SBA-15 at low TiO2 loading, indicating TiO\u003csub\u003e2\u003c/sub\u003e particles inserted into the mesostructure of SBA-15 in TiO2/SBA-15(R) photocatalyst (R values up to 16).\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eStructural, chemical, and textural properties of SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"11\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c8\" colnum=\"8\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c9\" colnum=\"9\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c10\" colnum=\"10\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c11\" colnum=\"11\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003eCatalyst\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colspan=\"3\" nameend=\"c4\" namest=\"c2\"\u003e \u003cp\u003eStoichiometric ratio Si/Ti\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003eCrystallite sizes of TiO\u003csub\u003e2\u003c/sub\u003e (nm)\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c6\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003eSurface Area BET\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003cp\u003e(m\u003csup\u003e2\u003c/sup\u003e/g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c7\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003ePore Volume\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003cp\u003e(cm\u003csup\u003e3\u003c/sup\u003e/g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c8\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003ePore Diameter (nm)\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c9\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003eLattice parameter a\u003csub\u003e0\u003c/sub\u003e(nm)\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c10\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003ePore Wall Thickness\u003c/p\u003e \u003cp\u003enm\u003csup\u003ed\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c11\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003eBand Gap energy (eV)\u003csup\u003ef\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTheoretical ratio\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eDetermined by XRF\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eDetermined by SEM-EDX\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSBA-15\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e732\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0,89\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e5,95\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e13,33\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c10\"\u003e \u003cp\u003e7,38\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c11\"\u003e \u003cp\u003e2.37\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R\u0026thinsp;=\u0026thinsp;64)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e64\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e68\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e54\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e11,27\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e621\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0,83\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e5,84\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e13,01\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c10\"\u003e \u003cp\u003e7,26\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c11\"\u003e \u003cp\u003e3.30\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R\u0026thinsp;=\u0026thinsp;32)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e32\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e34\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e41\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e11,61\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e616\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0,81\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e5,64\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e13,41\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c10\"\u003e \u003cp\u003e7,77\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c11\"\u003e \u003cp\u003e3.31\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R\u0026thinsp;=\u0026thinsp;16)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e16\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e15\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e13\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e11,23\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e609\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0,76\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e5,45\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e12,97\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c10\"\u003e \u003cp\u003e7,52\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c11\"\u003e \u003cp\u003e3.31\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R\u0026thinsp;=\u0026thinsp;11)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e11\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e13\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e7\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e11,23\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e593\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0,76\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e5,41\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e12,97\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c10\"\u003e \u003cp\u003e7,56\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c11\"\u003e \u003cp\u003e3.31\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R\u0026thinsp;=\u0026thinsp;8)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e8\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e10\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e6\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e10,98\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e541\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0,64\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e5,16\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e12,68\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c10\"\u003e \u003cp\u003e7,52\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c11\"\u003e \u003cp\u003e3.32\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R\u0026thinsp;=\u0026thinsp;6)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e6\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e7\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e8\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e11,09\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e583\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0,67\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e5,21\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e12,81\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c10\"\u003e \u003cp\u003e7,60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c11\"\u003e \u003cp\u003e3.32\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003ctfoot\u003e \u003ctr\u003e\u003ctd colspan=\"11\"\u003e\u003csup\u003ea\u003c/sup\u003e from XRD, \u003csup\u003ea\u003c/sup\u003e Multipoint BET method., \u003csup\u003eb\u003c/sup\u003e from BJH method., \u003csup\u003ed\u003c/sup\u003eWall thickness (a\u003csub\u003e0\u003c/sub\u003e\u0026thinsp;\u0026minus;\u0026thinsp;pore diameter)., \u003csup\u003ef\u003c/sup\u003e fron UV-DRS\u003c/td\u003e\u003c/tr\u003e\u003c/tfoot\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eAs seen in Table 2, the surface area of SBA-15was found to be 732 m\u003csup\u003e2\u003c/sup\u003e/g, and falls within the range of high-quality SBA-15 as 500\u0026ndash;1300 m\u003csup\u003e2\u003c/sup\u003e/g\u0026nbsp;(Zhan et al., 2014). Although the surface area and pore volume decreased slightly after TiO\u003csub\u003e2\u003c/sub\u003e loading, the BET area values of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) are still high as the range 621\u0026ndash;583 m\u003csup\u003e2\u003c/sup\u003e/g. Additionally, the decrease in R values is ideal for promoting an increase in the wall thickness. These effects may be due to the presence of TiO\u003csub\u003e2\u003c/sub\u003e nanocrystals in the SBA-15 mesopores and is complied with the XRD and SEM results\u0026nbsp;(Han et al., 2011; Malik et al., 2016). \u003c/p\u003e\n\u003cp\u003eDRS analyses of synthesized TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) photocatalysts were performed and given in Figure 4. It was observed that all samples have an absorption band at wavelengths from 250 to 380 nm, and the large absorption drop around 380 nm, which is complied with the absorb on the bandgap of anatase TiO\u003csub\u003e2\u003c/sub\u003e (Chang et al., 2016; Wr\u0026oacute;blewska et al., 2018). The adsorption edges of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) photocatalysts are slightly blue-shifted with increasing R ratios, indicating that the\u0026nbsp;SBA-15 effectively suppresses the agglomerate of TiO\u003csub\u003e2\u003c/sub\u003e nanoparticles. Also, the strong adsorption peak at about 350\u0026ndash;400 nm demonstrate the TiO\u003csub\u003e2\u0026nbsp;\u003c/sub\u003eparticle whose size is the larger than 5 nm (Acosta-Silva et al., 2011). These observations are in good agreement with XRD results.\u003c/p\u003e \u003cp\u003eThe bandgap energy (E\u003csub\u003eg\u003c/sub\u003e) was found by using the modified plot of the Kubelka\u0026ndash;Munk function given in Figure S1 and Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e (Garc\u0026iacute;a et al., \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). The calculated values of the optical band gap energies were considerably blue-shifted compared with that of TiO\u003csub\u003e2\u003c/sub\u003e anatase phase (3.2 eV) (Garc\u0026iacute;a et al., \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). The increment in the bandgap energies of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15s is indicative of quantization effects (Ara\u0026uacute;jo et al., \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2016\u003c/span\u003e), which improves the photocatalytic properties.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec10\" class=\"Section2\"\u003e \u003ch2\u003e3.2. Photocatalytic activity\u003c/h2\u003e \u003cp\u003ePhotocatalytic activities of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R) were evaluated by degradation of methylene blue under UV-light irradiation. To compare their catalytic efficiencies, the amount of active TiO\u003csub\u003e2\u003c/sub\u003e inserted in SBA-15, or TiO\u003csub\u003e2\u003c/sub\u003enano powder is the same, which is 6 mg of TiO\u003csub\u003e2\u003c/sub\u003e.Results of photocatalyst efficiencies of TiO2/SBA-15(R) photocatalysts are given with and without adsorption in Figs.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ea and b.\u003c/p\u003e \u003cp\u003eAs seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e, blank tests were carried out in the absence of a photocatalyst no methylene blue degradation was observed (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003eb). The second test was made in the presence of SBA-15, the concentration of methylene blue, no changed after the light was turned on, indicating the SBA-15 reached the adsorption equilibrium of methylene blue (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ea). It is obvious that SBA-15 has no photocatalytic activity due to having no radical groups in an amorphous silica structure (Ara\u0026uacute;jo et al., \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). Therefore, all catalyst in methylene blue solution were stirred for 1 h for adsorption equilibrium.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e nano powder have low photoactivity (27.52%) due to the poor dispersion of active phases. Its photocatalytic efficiency is increased as a result of high dispersion of TiO\u003csub\u003e2\u003c/sub\u003e into the SBA-15 in all synthesized photocatalyst. This result shows that the titanium incorporated into SBA-15 framework is enhanced the photoactivity of TiO\u003csub\u003e2\u003c/sub\u003e. As seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003eb, methylene blue degradation efficiencies are 57%, 67.5%, 61.7%, 79.6%, 70.9%, and 75.6% with increasing R ratios, respectively. Among them, TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R\u0026thinsp;=\u0026thinsp;16) presented the best photocatalytic performance. Therefore, the improved photocatalytic activity should be attributed to the insert of the TiO\u003csub\u003e2\u003c/sub\u003e particles in the SBA-15 pore walls with an increase in Ti amount (R; 64, 32, and 16). At the lower R values than 16, decreasing efficiency in the photocatalytic activity may depend on clogging of TiO\u003csub\u003e2\u003c/sub\u003e particles in mesopore channels of SBA-15. Also, this phenomenon is seen in the pore distribution curve in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eb. These results show that good TiO\u003csub\u003e2\u003c/sub\u003e dispersion into the SBA-15 reveals more active sites near the adsorbed dye molecules, resulting in an increase in degradation rates.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003e3.3. Reusability\u003c/h2\u003e \u003cp\u003eCatalyst reusability is one of the major factors in the photocatalytic degradation industries. The reusability studies were conducted on the TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (R\u0026thinsp;=\u0026thinsp;16) catalyst for five runs given in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e. Each of run was examined by using the fresh dye solution in the presence of the same amount of the used catalyst, refreshed with and without calcination described in the Experimental Section. As seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e, the activity of the reused catalyst with and without calcination in the fifth run was the same as that of the fresh catalyst. Therefore, photocatalyst could use for long periods without loss of activity.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eAfter the fifth run, the used catalyst was characterized by XRD, SEM-EDX, and N2 adsorption-desorption isotherms/desorption analyses, and results are given in Figures S2, S3, and S4 and Table S3. It is seen in Figure S2, reused catalyst retained the crystal structure of anatase TiO\u003csub\u003e2\u003c/sub\u003e and the hexagonal structure of SBA-15. The photocatalyst still had type IV characteristic curves with a type H1 hysteresis loop. Pore distribution curves show that some pore-clogging occurs without calcination due to the adsorption of methylene blue on the catalyst while the pore size changed slightly, from 5.45 to 4.75 nm during the calcination process. As seen in Table S3, the calcined catalyst BET surface area, pore-volume, and diameter values were higher than the fresh catalyst and reused catalyst without calcination because of the removal of the dye remaining in the pores during the calcination process performed in each of run. Photocatalyst activity and stability was maintained after reuse for several cycles.\u003c/p\u003e \u003c/div\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003eIn this study, a series of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts were synthesized by a one-step hydrothermal method with TiO\u003csub\u003e2\u003c/sub\u003e nano-powder as a titanium source. The effect of the Si/Ti molar ratios on photocatalytic activity has been studied. The photocatalysts were characterized by several different analytical methods. Results showed that the amorphous structure of the SBA-15 is preserved with a highs distribution of TiO2 in the synthesized photocatalysts. Si/Ti molar ratios of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 catalysts are compatible with theoretical ratios. BET surface areas and pore volumes of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 decreased slightly after TiO\u003csub\u003e2\u003c/sub\u003e loading because of TiO\u003csub\u003e2\u003c/sub\u003e nanoparticle incorporation into the SBA-15 pore walls. But the pore size distribution curve shifted to a smaller range at high TiO\u003csub\u003e2\u003c/sub\u003e loading, whereas; the curve has the same as SBA-15 at low TiO\u003csub\u003e2\u003c/sub\u003e loading, indicating TiO\u003csub\u003e2\u003c/sub\u003e particles inserted into the mesostructure of SBA-15 into TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 catalyst (R values up to 16). Also, optical band gap energies slowly increase as TiO\u003csub\u003e2\u003c/sub\u003e amount increases for TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts.\u003c/p\u003e \u003cp\u003eThe photocatalytic efficiency of TiO2/SBA-15 has been investigated by the degradation of methylene blue under UV irradiation. The highest photocatalytic efficiency (79.6%) was obtained in the TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15(R\u0026thinsp;=\u0026thinsp;16). These results are coincided with pore distribution curve. The superior photocatalytic efficiencies of the TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 could be attributed to the high surface area and better dispersion of TiO\u003csub\u003e2\u003c/sub\u003e in SBA-15 pore walls. Also, the reusability and stability of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts are still good for five runs. Due to their high reusability efficiency, easy separation, environment-friendly nature along with good photocatalytic performance, these photocatalysts may have sustainable potential for wastewater treatment in practical applications.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAcknowledgment\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThis study was supported by Eskişehir Technical University Scientific Research Projects Commission under grant no: 22ADP043.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eDeclaration of Competing Interest\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors report no declarations of interest.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor Contribution\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eElif Akbay led the project; Sevgican G\u0026ouml;l performed the experiment and the data analyses; Elif Akbay performed the characterization analysis and their discussion; Sevgican G\u0026ouml;l and Elif Akbay contributed to the preparation of the manuscript.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eAcosta-Silva YJ, Nava R, Hern\u0026aacute;ndez-Morales V, Mac\u0026iacute;as-S\u0026aacute;nchez SA, G\u0026oacute;mez-Herrera ML, Pawelec B (2011) Methylene blue photodegradation over titania-decorated SBA-15. 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Fuel 291:120207. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/https://doi.org/10.1016/j.fuel.2021.120207\u003c/span\u003e\u003cspan address=\"10.1016/j.fuel.2021.120207\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":true,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Mesoporous material, TiO2/ SBA-15, Photocatalytic degradation, Reusability","lastPublishedDoi":"10.21203/rs.3.rs-1831676/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-1831676/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eIn this study, a series of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 photocatalysts were synthesized with different Si/Ti ratios by a one-step hydrothermal method with TiO\u003csub\u003e2\u003c/sub\u003e nano-powder as a titanium source. These materials were characterized by XRD, SEM-EDX, N2 adsorption-desorption isotherms-desorption isotherms, XRF, and UV-DRS analysis. During the synthesis of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15s, the SBA-15 pore structure and channels did not deteriorate, and the Si/Ti molar ratios are close to the expected nominal ratios. SBA-15 and TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15s exhibited a uniform- narrow pore size distribution, but TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15s pore size shifted to a smaller range, and the BET area values of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15s materials are in the range of the 621\u0026ndash;583 m2/g. TiO\u003csub\u003e2\u003c/sub\u003e nanocrystals into the SBA-15 mesopores walls wall up to the ratio of Si/Ti\u0026thinsp;=\u0026thinsp;16. With high TiO2 loading of that value, clogging occurs in the SBA-15 pores. The optical band gap energies were significantly blue-shifted which is the quantization effects improving the photocatalytic activities\u003c/p\u003e \u003cp\u003ePhotocatalytic activities of TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15s were evaluated by degradation of methylene blue under UV-light irradiation at constant TiO\u003csub\u003e2\u003c/sub\u003e content. The highest efficiency was obtained in the TiO\u003csub\u003e2\u003c/sub\u003e/SBA-15 (16) photocatalyst at 79.6%, and all efficiencies in synthesized photocatalyst are higher than bulk TiO\u003csub\u003e2\u003c/sub\u003e photocatalyst activity (27.52%) due to the poor dispersion of active phases. Reused photocatalyst has no activity losses for five runs and may be used for long periods without loss of activity. For the stability of the photocatalyst, a combination of XRD, SEM, and N2 adsorption-desorption isotherms was employed after the fifth run. These results demonstrate that the photocatalyst activity and stability are good, and photocatalytic activity was sustainable after reuse for several cycles.\u003c/p\u003e","manuscriptTitle":"Reusable titania-SBA-15 photocatalyst synthesized by different silica/titania ratios for enhancing methylene blue photodegradation","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2022-07-13 16:37:54","doi":"10.21203/rs.3.rs-1831676/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"13a1d87f-7304-4d8a-abea-78658dda7fd1","owner":[],"postedDate":"July 13th, 2022","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2024-02-15T17:20:47+00:00","versionOfRecord":{"articleIdentity":"rs-1831676","link":"https://doi.org/10.1002/slct.202301887","journal":{"identity":"chemistryselect","isVorOnly":true,"title":"ChemistrySelect"},"publishedOn":"2023-11-14 00:00:00","publishedOnDateReadable":"November 14th, 2023"},"versionCreatedAt":"2022-07-13 16:37:54","video":"","vorDoi":"10.1002/slct.202301887","vorDoiUrl":"https://doi.org/10.1002/slct.202301887","workflowStages":[]},"version":"v1","identity":"rs-1831676","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-1831676","identity":"rs-1831676","version":["v1"]},"buildId":"7rjqhiLT3MXkJMwkYKINL","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}