Synthesis and characterizations of TiN–SBA-15 mesoporous materials for CO2 dry reforming enhancement

2020 ◽  
Vol 92 (4) ◽  
pp. 545-556
Author(s):  
Maslin Chotirach ◽  
Supawan Tantayanon ◽  
Duangamol Nuntasri Tungasmita ◽  
Junliang Sun ◽  
Sukkaneste Tungasmita

AbstractA novel approach of titanium nitride (TiN) incorporated into SBA-15 framework was developed using one-step hydrothermal synthesis method. TiN contents up to ~18 wt% were directly dispersed in a synthetic gel under a typical strong acidic condition. The physico-chemical characteristics and the surface properties were investigated by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), N2 adsorption-desorption, field emission scanning electron microscope (FESEM) equipped with energy dispersive X-ray spectroscopy (EDS), wavelength dispersive X-ray fluorescence (WDXRF) and CO2-temperature programmed desorption (CO2-TPD). The results indicated that the highly ordered mesostructured was effectively maintained with high specific surface area of 532–685 m2g−1. The basicity of the modified SBA-15 increased with rising TiN loading. These modified materials were applied as a support of Ni catalyst in dry reforming of methane (DRM). Their catalytic behavior possessed superior conversions for both CO2 and CH4 with the highest H2/CO ratio (0.83) as well as 50 % lower carbon formation, compared to bare SBA-15 support.

Catalysts ◽  
2021 ◽  
Vol 11 (10) ◽  
pp. 1233
Author(s):  
Abdulaziz Bagabas ◽  
Ahmed Sadeq Al-Fatesh ◽  
Samsudeen Olajide Kasim ◽  
Rasheed Arasheed ◽  
Ahmed Aidid Ibrahim ◽  
...  

The dry reforming of methane (DRM) process has attracted research interest because of its ability to mitigate the detrimental impacts of greenhouse gases such as methane (CH4) and carbon dioxide (CO2) and produce alcohols and clean fuel. In view of this importance of DRM, we disclosed the efficiency of a new nickel-based catalyst, which was promoted with magnesia (MgO) and supported over gamma-alumina (g-Al2O3) doped with silica (SiO2), toward DRM. The synthesized catalysts were characterized by H2 temperature-programmed reduction (H2-TPR), X-ray diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Thermogravimetric analysis (TGA), and Transmission electron microscopy (TEM) techniques. The effect of MgO weight percent loading (0.0, 1.0, 2.0, and 3.0 wt. %) was examined because the catalytic performance was found to be a function of this parameter. An optimum loading of 2.0 wt. % of MgO was obtained, where the conversion of CH4 and CO2 at 800 °C were 86% and 91%, respectively, while the syngas (H2/CO) ratios relied on temperature and were in the range of 0.85 to 0.95. The TGA measurement of the best catalyst, which was operated over a 15-hour reaction time, displayed negligible weight loss (<9.0 wt. %) due to carbon deposition, indicating the good resistance of our catalyst system to the deposition of carbon owing to the dopant and the modifier. TEM images showed the presence of multiwalled carbon nanotubes, confirming the TGA.


Catalysts ◽  
2019 ◽  
Vol 9 (1) ◽  
pp. 56 ◽  
Author(s):  
Katarzyna Świrk ◽  
Magnus Rønning ◽  
Monika Motak ◽  
Patricia Beaunier ◽  
Patrick Da Costa ◽  
...  

Ce- and Y-promoted double-layered hydroxides were synthesized and tested in dry reforming of methane (CH4/CO2 = 1/1). The characterization of the catalysts was performed using X-ray fluorescence (XRF), X-ray diffraction (XRD), N2 sorption, temperature-programmed reduction in H2 (TPR-H2), temperature-programmed desorption of CO2 (TPD-CO2), H2 chemisorption, thermogravimetric analysis coupled by mass spectrometry (TGA/MS), Raman, and high-resolution transmission electron microscopy (HRTEM). The promotion with cerium influences textural properties, improves the Ni dispersion, decreases the number of total basic sites, and increases the reduction temperature of nickel species. After promotion with yttrium, the increase in basicity is not directly correlated with the increasing Y loading on the contrary of Ni dispersion. Dry reforming of methane (DRM) was performed as a function of temperature and in isothermal conditions at 700 °C for 5 h. For catalytic tests, a slight increase of the activity is observed for both Y and Ce doped catalysts. This improvement can of course be explained by Ni dispersion, which was found higher for both Y and Ce promoted catalysts. During DRM, the H2/CO ratio was found below unity, which can be explained by side reactions occurrence. These side reactions are linked with the increase of CO2 conversion and led to carbon deposition. By HRTEM, only multi-walled and helical-shaped carbon nanotubes were identified on Y and Ce promoted catalysts. Finally, from Raman spectroscopy, it was found that on Y and Ce promoted catalysts, the formed C is less graphitic as compared to only Ce-based catalyst.


Materials ◽  
2019 ◽  
Vol 12 (11) ◽  
pp. 1771 ◽  
Author(s):  
Stefan Neatu ◽  
Mihaela M. Trandafir ◽  
Adelina Stănoiu ◽  
Ovidiu G. Florea ◽  
Cristian E. Simion ◽  
...  

This study presents the synthesis and characterization of lanthanum-modified alumina supported cerium–manganese mixed oxides, which were prepared by three different methods (coprecipitation, impregnation and citrate-based sol-gel method) followed by calcination at 500 °C. The physicochemical properties of the synthesized materials were investigated by various characterization techniques, namely: nitrogen adsorption-desorption isotherms, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and H2–temperature programmed reduction (TPR). This experimental study demonstrated that the role of the catalytic surface is much more important than the bulk one. Indeed, the incipient impregnation of CeO2–MnOx catalyst, supported on an optimized amount of 4 wt.% La2O3–Al2O3, provided the best results of the catalytic combustion of methane on our catalytic micro-convertors. This is mainly due to: (i) the highest pore size dimensions according to the Brunauer-Emmett-Teller (BET) investigations, (ii) the highest amount of Mn4+ or/and Ce4+ on the surface as revealed by XPS, (iii) the presence of a mixed phase (Ce2MnO6) as shown by X-ray diffraction; and (iv) a higher reducibility of Mn4+ or/and Ce4+ species as displayed by H2–TPR and therefore more reactive oxygen species.


2017 ◽  
Vol 23 (1) ◽  
pp. 49-56 ◽  
Author(s):  
Yajing Zhang ◽  
Yu Zhang ◽  
Fu Ding ◽  
Kangjun Wang ◽  
Wang Xiaolei ◽  
...  

A series of La2O3-modified CuO-ZnO-ZrO2/HZSM-5 catalysts were prepared by an oxalate co-precipitation method. The catalysts were fully characterized by X-ray diffraction (XRD), N2 adsorption-desorption, hydrogen temperature pro-grammed reduction (H2-TPR), ammonia temperature programmed desorption (NH3-TPD), and X-ray photoelectron spectroscopy (XPS) techniques. The effect of the La2O3 content on the structure and performance of the catalysts was thoroughly investigated. The catalysts were evaluated for the direct synthesis of dimethyl ether (DME) from CO2 hydrogenation. The results displayed that La2O3 addition enhanced catalytic performance, and the maximal CO2 conversion (34.3%) and DME selectivity (57.3%) were obtained over the catalyst with 1% La2O3, which due to the smaller size of Cu species and a larger ratio of Cu+/Cu.


2021 ◽  
Vol 16 (1) ◽  
pp. 97-110
Author(s):  
Faris A. Jassim Al-Doghachi ◽  
Diyar M. A. Murad ◽  
Huda S. Al-Niaeem ◽  
Salam H. H. Al-Jaberi ◽  
Surahim Mohamad ◽  
...  

Co/Mg1−XCe3+XO (x = 0, 0.03, 0.07, 0.15; 1 wt% cobalt each) catalysts for the dry reforming of methane (DRM) reaction were prepared using the co-precipitation method with K2CO3 as precipitant. Characterization of the catalysts was achieved by X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), X-ray photoelectron spectroscopy (XPS), temperature programmed reduction (H2-TPR), Brunauer–Emmett–Teller (BET), transmission electron microscopy (TEM), and thermal gravimetric analysis (TGA). The role of several reactant and catalyst concentrations, and reaction temperatures (700–900 °C) on the catalytic performance of the DRM reaction was measured in a tubular fixed-bed reactor under atmospheric pressure at various CH4/CO2 concentration ratios (1:1 to 2:1). Using X-ray diffraction, a surface area of 19.2 m2.g−1 was exhibited by the Co/Mg0.85Ce3+0.15O catalyst and MgO phase (average crystallite size of 61.4 nm) was detected on the surface of the catalyst. H2 temperature programmed reaction revealed a reduction of CoO particles to metallic Co0 phase. The catalytic stability of the Co/Mg0.85Ce3+0.15O catalyst was achieved for 200 h on-stream at 900 °C for the 1:1 CH4:CO2 ratio with an H2/CO ratio of 1.0 and a CH4, CO2 conversions of 75% and 86%, respectively. In the present study, the conversion of CH4 was improved (75%–84%) when conducting the experiment at a lower flow of oxygen (1.25%). Finally, the deposition of carbon on the spent catalysts was analyzed using TEM and Temperature programmed oxidation-mass spectroscopy (TPO-MS) following 200 h under an oxygen stream. Better anti-coking activity of the reduced catalyst was observed by both, TEM, and TPO-MS analysis. Copyright © 2021 by Authors, Published by BCREC Group. This is an open access article under the CC BY-SA   License (https://creativecommons.org/licenses/by-sa/4.0). 


Catalysts ◽  
2020 ◽  
Vol 10 (8) ◽  
pp. 878 ◽  
Author(s):  
Benjamín Torres-Olea ◽  
Sandra Mérida-Morales ◽  
Cristina García-Sancho ◽  
Juan Antonio Cecilia ◽  
Pedro Maireles-Torres

In the present work, a series of catalysts based on aluminum and zirconium oxides was studied for the transformation of glucose into 5-hydroxymethylfurfural. These catalysts were characterized by using experimental techniques, such as X-ray diffraction, N2 adsorption–desorption at −196 °C, X-ray photoelectron spectroscopy, temperature-programmed desorption of NH3 and CO2, and scanning transmission electron microscopy. The catalytic behavior in glucose dehydration was evaluated in a water-methyl isobutyl ketone biphasic system, in the presence of CaCl2, in order to minimize losses due to unwanted secondary reactions. High glucose conversion and 5-hydroxymethylfurfural (HMF) yield values were obtained in the presence of an Al(Zr)Ox catalyst with an Al:Zr molar ratio of 7:3, reaching 97% and 47%, respectively, at 150 °C after 120 min. Under tested conditions, this catalyst retained most of its catalytic activity for four reuses.


Materials ◽  
2019 ◽  
Vol 12 (20) ◽  
pp. 3349 ◽  
Author(s):  
Pablo A. Ochoa Rodríguez ◽  
Tamara B. Benzaquén ◽  
Gina A. Pecchi ◽  
Sandra G. Casuscelli ◽  
Verónica R. Elías ◽  
...  

Titanium dioxide materials were synthesized using two different methods. The samples were characterized by X-ray diffraction (XRD), UV–Visible diffusion reflectance spectroscopy (UV-Vis DR), Raman spectroscopy, N2 adsorption/desorption, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron spectroscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Although both kind of materials were found to have mesoporous structure and anatase crystalline phase, one of them was obtained from a synthesis method that does not involve the use of surfactants, and therefore, does not require calcination at high temperatures. This implies that the synthesized solid was self-doped with carbon species, coming only from the same source used for titanium. Then, the relationship between the presence of these species, the final calcination temperature, and the photocatalytic activity of the solids was studied in terms of the degradation and mineralization of an Acid Orange 7 aqueous solution, under visible radiation. A photosensitizing effect caused by the non-metal presence, that allows the solid to extend its absorption range, was found. Hence, a novel route to prepare C-modified photoactive mesoporous TiO2, simpler and cheaper, where neither a template nor an external carbon source is used, could be performed.


2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Feng-shan Zhou ◽  
Dai-mei Chen ◽  
Bao-lin Cui ◽  
Wei-heng Wang

Sodium montmorillonite (MMT) was chosen as the carrier; a serial of CdS/TiO2-MMT nanocomposites with enhanced visible-light absorption ability was prepared by hydrothermal synthesis method combination with semiconductor compound modification method. The samples are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and ultraviolet visible (UV-Vis) spectroscopy; the results showed that TiO2and CdS nanoparticles were loaded on the surface of montmorillonite uniformly. N2adsorption-desorption experiment showed that the specific surface area of TiO2/montmorillonite nanocomposite made by this method can reach 200 m2/g and pore-size distribution was from 4 to 6 nm; UV-Vis showed that the recombination of CdS and TiO2enhanced visible-light absorption ability of samples of TiO2/montmorillonite and visible-light absorption ability increase with the increased of the adsorption of CdS.


Materials ◽  
2020 ◽  
Vol 13 (9) ◽  
pp. 2196
Author(s):  
Cristian E. Simion ◽  
Ovidiu G. Florea ◽  
Mihaela Florea ◽  
Florentina Neaţu ◽  
Ştefan Neaţu ◽  
...  

Mesoporous CeO2:Mn3O4 materials (3:7 and 7:3 molar ratio) were prepared by co-precipitation and deposited as porous thick films over alumina (Al2O3) planar substrate provided with Pt meander. The aim was oriented towards detecting low levels methane (CH4) at moderate operating temperatures. Herein we demonstrated that the sensitivity of catalytic micro-converters (CMCs) towards a given peak of CH4 concentration corresponds to specific gas-surface interaction phenomena. More precisely, a transition from thermal conductivity to combustion rate is likely to occur when CMCs are operated under real atmospheric conditions (normal pressure, presence of relative humidity, and constant operating temperature). The response to CH4 was analyzed over different gas flows and different gas concentrations under the same operating regime. The materials were fully characterized by adsorption-desorption isotherms, H2-Temperature Programmed Reduction (H2-TPR), X-ray Diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), and Raman spectroscopies. Thus, the applicative aspect of using CeO2:Mn3O4 as moderate temperature CMC for CH4 detection is brought to the fore.


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