scholarly journals Kinetics of Highly Active TiO2 Microspheres Formation in a Presence of Ethylammonium Nitrate Ionic Liquid

Author(s):  
Anna Gołąbiewska ◽  
Micaela Checa-Suárez ◽  
Marta Paszkiewicz-Gawron ◽  
Wojciech Lisowski ◽  
Edyta Raczuk ◽  
...  

Spherical microparticles of TiO2 were synthesized by the ionic liquid-assisted solvothermal method at different reaction time (3, 6, 12 and 24h). The properties of the prepared photocatalysts were investigated by means of UV-vis diffuse-reflectance spectroscopy (DRS), BET surface area measurements, scanning electron microscopy (SEM), X-ray diffraction analysis (XRD), and X-ray photoelectron spectroscopy (XPS). The results indicated that the efficiency of phenol degradation was related with a time of the solvothermal synthesis as determined for TiO2_EAN(1:1)_24h sample. Microparticles of TiO2_EAN(1:1)_3h formed during the only 3h of synthesis time revealed really high photoactivity under visible irradiation – 75%. This value increased to 80% and 82% after 12h and 24h, respectively. The photoactivity increase was accompanied by the increase of the specific surface area thus pores size, as well as ability to absorb UV-vis irradiation. The high efficiency of phenol degradation of IL-TiO2 photocatalysts was ascribed to the interaction between the surface of TiO2 and ionic liquid components (carbon and nitrogen).

2018 ◽  
Vol 9 ◽  
pp. 580-590 ◽  
Author(s):  
Anna Gołąbiewska ◽  
Marta Paszkiewicz-Gawron ◽  
Aleksandra Sadzińska ◽  
Wojciech Lisowski ◽  
Ewelina Grabowska ◽  
...  

To investigate the effect of the ionic liquid (IL) chain length on the surface properties and photoactivity of TiO2, a series of TiO2 microspheres have been synthesized via a solvothermal method assisted by 1-methyl-3-octadecylimidazolium chloride ([ODMIM][Cl]) and 1-methyl-3-tetradecylimidazolium chloride ([TDMIM][Cl]). All as-prepared samples were characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), diffuse reflectance spectroscopy (DRS), scanning transmission microscopy (STEM) and the Brunauer–Emmett–Teller (BET) surface area method, whereas the photocatalytic activity was evaluated by the degradation of phenol in aqueous solution under visible light irradiation (λ > 420 nm). The highest photoefficiency (four times higher than pristine TiO2) was observed for the TiO2 sample obtained in the presence of [TDMIM][Cl] for a IL to TiO2 precursor molar ratio of 1:3. It was revealed that interactions between the ions of the ionic liquid and the surface of the growing titanium dioxide spheres results in a red-shift of absorption edge for the IL–TiO2 semiconductors. In this regard, the direct increase of the photoactivity of IL–TiO2 in comparison to pristine TiO2 was observed. The active species trapping experiments indicated that O2 •− is the main active species, created at the surface of the IL–TiO2 material under visible-light illumination, and is responsible for the effective phenol degradation.


Author(s):  
Irwing M. Ramírez-Sánchez ◽  
Erick R. Bandala

Iron Doped TiO2 nanoparticles (Fe-TiO2) were synthesized and photocatalitically investigated under high and low fluence values of UV-radiation. The Fe-TiO2 physical characterization was performed using X-ray Powder Diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area analysis, Transmission Electron Microscope (TEM), Scanning Electron Microscope (SEM), Diffuse Reflectance Spectroscopy (DRS), and X-Ray Photoelectron Spectroscopy (XPS) technique. The XPS evidenced that ferric ion (Fe3+) was in the lattice of TiO2 and co-dopants no intentionally added were also present due to the precursors of the synthetic method. The Fe3+ concentration played a key role in the photocatalytic generation of hydroxyl radical (•OH) and estriol (E3) degradation. Fe-TiO2 materials accomplished E3 degradation, and it was found that the catalyst with 0.3 at. % content of Fe (0.3 Fe-TiO2) enhanced the photocatalytic activity under low UV-irradiation compared with no intentionally Fe-added TiO2 (zero-iron TiO2) and Aeroxide® TiO2 P25. Furthermore, the enhanced photocatalytic activity of 0.3 Fe-TiO2 under low UV-irradiation may have applications when radiation intensity must be controlled, as in medical applications, or when strong UV absorbing species are present in water.


Catalysts ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 672 ◽  
Author(s):  
Zuzanna Bielan ◽  
Agnieszka Sulowska ◽  
Szymon Dudziak ◽  
Katarzyna Siuzdak ◽  
Jacek Ryl ◽  
...  

In the presented work, for the first time, the metal-modified defective titanium(IV) oxide nanoparticles with well-defined titanium vacancies, was successfully obtained. Introducing platinum and copper nanoparticles (NPs) as surface modifiers of defective d-TiO2 significantly increased the photocatalytic activity in both UV-Vis and Vis light ranges. Moreover, metal NPs deposition on the magnetic core allowed for the effective separation and reuse of the nanometer-sized photocatalyst from the suspension after the treatment process. The obtained Fe3O4@SiO2/d-TiO2-Pt/Cu photocatalysts were characterized by X-ray diffractometry (XRD) and specific surface area (BET) measurements, UV-Vis diffuse reflectance spectroscopy (DR-UV/Vis), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Further, the mechanism of phenol degradation and the role of four oxidative species (h+, e−, •OH, and •O2−) in the studied photocatalytic process were investigated.


Catalysts ◽  
2019 ◽  
Vol 9 (10) ◽  
pp. 847 ◽  
Author(s):  
Seyed Moeini ◽  
Chiara Battocchio ◽  
Stefano Casciardi ◽  
Igor Luisetto ◽  
Paolo Lupattelli ◽  
...  

In the present study, the catalytic activity of palladium oxide (PdOx) supported on ceria nanorods (CeO2-NR) for aerobic selective oxidation of benzyl alcohol (BnOH) to benzaldehyde (PhCHO) was evaluated. The CeO2-NR was synthesized hydrothermally and the Pd(NO3)2 was deposited by a wet impregnation method, followed by calcination to acquire PdOx/CeO2-NR. The catalysts were characterized by X-ray diffraction (XRD), temperature programmed reduction (TPR), transmission electron microscopy (TEM), Brunauer–Emmet–Teller (BET) surface area analysis, and X-ray photoelectron spectroscopy (XPS). In addition, the TPR-reduced PdOx/CeO2-NR (PdOx/CeO2-NR-Red) was studied by XRD, BET, and XPS. Characterizations showed the formation of CeO2-NR with (111) exposed plane and relatively high BET surface area. PdOx (x > 1) was detected to be the major oxide species on the PdOx/CeO2-NR. The activities of the catalysts in BnOH oxidation were evaluated using air, as an environmentally friendly oxidant, and various solvents. Effects of temperature, solvent nature and palladium oxidation state were investigated. The PdOx/CeO2-NR showed remarkable activity when protic solvents were utilized. The best result was achieved using PdOx/CeO2-NR and boiling ethanol as solvent, leading to 93% BnOH conversion and 96% selectivity toward PhCHO. A mechanistic hypothesis for BnOH oxidation with PdOx/CeO2-NR in ethanol is presented.


Catalysts ◽  
2021 ◽  
Vol 12 (1) ◽  
pp. 19
Author(s):  
Antonio Jesús Fernández-Ropero ◽  
Bartosz Zawadzki ◽  
Krzysztof Matus ◽  
Wojciech Patkowski ◽  
Mirosław Krawczyk ◽  
...  

This work presents the effect of Co loading on the performance of CNR115 carbon-supported catalysts in the continuous-flow chemoselective hydrogenation of 2-methyl-2-pentenal for the obtention of 2-methylpentanal, an intermediate in the synthesis of the sedative drug meprobamate. The Co loading catalysts (2, 6, 10, and 14 wt.%) were characterized by Brunauer–Emmett–Teller (BET) surface area analysis, transmission electron microscopy (TEM), H2 temperature-programmed reduction (H2-TPR), temperature-programmed desorption of hydrogen (H2-TPD) analysis, X-ray diffraction (XRD), and X-ray photoelectron spectroscopy for selected samples, and have been studied as hydrogenation catalysts at different pressure and temperature ranges. The results reveal that a certain amount of Co is necessary to achieve significant conversion values. However, excessive loading affects the morphological parameters, such as the surface area available for hydrogen adsorption and the particle size, preventing an increase in conversion, despite the increased presence of Co. Moreover, the larger particle size, caused by increasing the loading, alters the chemoselectivity, favouring the formation of 2-methyl-2-pentenol and, thus, decreasing the selectivity towards the desired product. The 6 wt.% Co-loaded material demonstrates the best catalytic performance, which is related to the formation of NPs with optimum size. Almost 100% selectivity towards 2-methylpentanal was obtained for the catalysts with lower Co loading (2 and 6 wt.%).


2021 ◽  
Author(s):  
Haijing Duan ◽  
Lin Zhang ◽  
Yu-long Wang ◽  
Yanhong Liu ◽  
Yangyang Wang

Abstract In this study, Fe-La binary (hydr)oxides were prepared by a co-precipitation method for phosphate removal. Various techniques, including secondary electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), powder X-ray diffraction (p-XRD) and Brunauer-Emmett-Teller (BET) surface area analysis, were employed to characterize the synthesized Fe-La binary (hydr)oxides. Batch experiments indicated that the performance of phosphate removal by Fe-La binary (hydr)oxides was excellent and increased with increasing La contents. The kinetics study showed that the adsorption was rapid and described better by the pseudo-second-order equation. The maximum adsorption capacities of Fe/La 3:1, Fe/La 1:1 and Fe/La 1:3 binary (hydr)oxides at pH 4.0 calculated by Langmuir model were 49.02, 69.44 and 136.99 mg/g, respectively. The uptake of phosphate was highly affected by solution pH and significantly reduced with the increase of pH value. The analyses of p-XRD, Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) suggested that the predominant mechanisms of phosphate removal involved surface hydroxyl exchange reactions and co-precipitation of released La3+ and phosphate ions, which resulted into the formation of amorphous phase of rhabdophane (LaPO4∙0.5H2O). The results show great potential for the application on the treatment of phosphate decontamination for their high efficiency of phosphate removal.


2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
R. M. Mohamed ◽  
M. A. Barakat

ZnO- nanoparticles were synthesized by a sol-gel technique from and tetraethyl orthosilicate (TEOS). The synthesized samples were further modified by nanosized Pt from H2PtCl6solution through photoassisted deposition (PAD) and impregnation (Img) routes. The obtained samples were characterized by a series of techniques including X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy, N2adsorption, extended X-ray absorption fine structure (EXAFS), and transmission electron microscopy (TEM). The photocatalytic activity of the Pt-ZnO/ was evaluated by photocatalytic degradation of phenol in synthetic wastewater under UV-irradiation. Results obtained revealed that the surface area and the photocatalytic activity of the prepared samples were increased in the order ZnO/ < PAD: Pt-ZnO/ < img: Pt-ZnO/. The surface area decreased from 480 to 460 and 450 m2/g, while the efficiency of the phenol degradation increased from 80 to 85 and 100%, with the ZnO/, Img: Pt-ZnO-, and PAD: Pt-ZnO- samples, respectively.


2018 ◽  
Vol 9 ◽  
pp. 447-459 ◽  
Author(s):  
Patrycja Parnicka ◽  
Paweł Mazierski ◽  
Tomasz Grzyb ◽  
Wojciech Lisowski ◽  
Ewa Kowalska ◽  
...  

Nd-modified TiO2 photocatalysts have been obtained via hydrothermal (HT) and sol–hydrothermal (SHT) methods. The as-prepared samples were characterized by X-ray diffraction (XRD), BET surface area measurements, scanning electron microscopy (SEM), diffuse reflectance spectroscopy (DRS), luminescence spectroscopy and X-ray photoelectron spectroscopy (XPS). The photocatalytic activity of the synthesized samples was evaluated by the degradation of phenol in aqueous solution under irradiation with UV–vis (λ > 350 nm) and vis (λ > 420 nm) light, as well as by the degradation of gaseous toluene under irradiation with vis (λmax = 415 nm) light. It was found that Nd-modified TiO2 is an efficient photocatalyst for the degradation of phenol and toluene under visible light. XPS analysis revealed that the photocatalyst prepared via HT method contains a three-times higher amount of hydroxy groups at the surface layer and a two-times higher amount of surface defects than that obtained by the SHT method. The photocatalytic efficiency of phenol and toluene degradation under vis irradiation in the presence of 0.25% Nd-TiO2(HT) reached 0.62 and 3.36 μmol·dm−1·min−1, respectively. Photocatalytic activity tests in the presence of Nd-TiO2 and scavenger confirm that superoxide radicals were responsible for the visible light-induced degradation of the model pollutant in aqueous solution.


Catalysts ◽  
2019 ◽  
Vol 9 (7) ◽  
pp. 624 ◽  
Author(s):  
Xiaoya Yuan ◽  
Xue Wu ◽  
Zijuan Feng ◽  
Wen Jia ◽  
Xuxu Zheng ◽  
...  

Heterojunctioned ZnO/Bi2S3 nanocomposites were prepared via a facile solvothermal method. The obtained photocatalysts were characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), High resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), UV-Vis diffuse reflectance spectroscopy (DRS), and Photoelectrochemical and Photoluminescence spectroscopy (PL), respectively. The results showed that ZnO/Bi2S3 composites exhibited the sandwiched-like structure, where ZnO nanoparticles were randomly embedded between Bi2S3 nanoflakes. The performance of photocatalytic Cr(VI) reduction under visible light indicated that ZnO/Bi2S3 composites exhibited high-efficiency photocatalytic activity in comparison with either Bi2S3 or ZnO. The 5%-ZnO/Bi2S3 photocatalyst removed 96% of Cr(VI) within 120 min at 20 mg/L initial concentration of Cr(VI). The enhanced performance of ZnO/Bi2S3 photocatalysts could be ascribed to the increased light harvesting and the effective separation and transfer of the photogenerated charge carriers across the heterojunction interface of the ZnO/Bi2S3 composite. This work could pave the way for the design of new hetero-structured materials and has great potential in environmental remediation.


Materials ◽  
2019 ◽  
Vol 12 (16) ◽  
pp. 2537 ◽  
Author(s):  
Tamás Gyulavári ◽  
Gábor Veréb ◽  
Zsolt Pap ◽  
Balázs Réti ◽  
Kornelia Baan ◽  
...  

Titanium dioxide–carbon sphere (TiO2–CS) composites were constructed via using prefabricated carbon spheres as templates. By the removal of template from the TiO2–CS, TiO2 hollow structures (HS) were synthesized. The CS templates were prepared by the hydrothermal treatment of ordinary table sugar (sucrose). TiO2–HSs were obtained by removing CSs with calcination. Our own sensitized TiO2 was used for coating the CSs. The structure of the CSs, TiO2–CS composites, and TiO2–HSs were characterized by scanning electron microscopy (SEM), infrared spectroscopy (IR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and diffuse reflectance spectroscopy (DRS). The effect of various synthesis parameters (purification method of CSs, precursor quantity, and applied furnace) on the morphology was investigated. The photocatalytic activity was investigated by phenol model pollutant degradation under visible light irradiation (λ > 400 nm). It was established that the composite samples possess lower crystallinity and photocatalytic activity compared to TiO2 hollow structures. Based on XPS measurements, the carbon content on the surface of the TiO2–HS exerts an adverse effect on the photocatalytic performance. The synthesis parameters were optimized and the TiO2–HS specimen having the best absolute and surface normalized photocatalytic efficiency was identified. The superior properties were explained in terms of its unique morphology and surface properties. The stability of this TiO2–HS was investigated via XRD and SEM measurements after three consecutive phenol degradation tests, and it was found to be highly stable as it entirely retained its crystal phase composition, morphology and photocatalytic activity.


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