scholarly journals The Temperature-Dependent Adsorption Behaviour of Benzene Molecules in ZSM-5 Zeolite Pores: TPD and FT-IR Spectroscopy Studies

2005 ◽  
Vol 23 (2) ◽  
pp. 95-107 ◽  
Author(s):  
Arati Sahasrabudhe ◽  
Salil Varma ◽  
Narendra M. Gupta

Temperature-programmed desorption (TPD) and in situ Fourier-transform infrared (FT-IR) spectroscopic methods were employed to investigate the effect of loading and sample temperature on the state of benzene molecules inside the channels of NaZSM-5 zeolite. TPD profiles revealed the existence of at least three distinct states of benzene adsorption, characterized by desorption peak maxima at ca. 120°C, 170°C and 220°C, respectively. Based on the growth behaviour of these bands, it is suggested that the benzene molecules occupy sinusoidal channels, straight channels and external surfaces, in that order. A reverse trend was observed during the subsequent flushing of the sample at varying temperatures. A virtually fixed amount of benzene was occluded at these three locations, depending upon the loading. The FT-IR studies revealed that the benzene molecule exists in a compressed state in the zeolitic channels, with the molecular clusters formed in the process dispersing only at temperatures above 150°C. For initial benzene loadings of up to ca. 1.5 molecules/unit cell, the spectrum obtained showed that in the O—H stretch region the bridge-bonded OH groups and hydroxyl groups associated with the internal zeolitic channels were perturbed simultaneously. The results show that even for a loading lower than necessary for saturation, a considerable amount of benzene remains condensed at the external surface of ZSM-5 zeolite.

1997 ◽  
Vol 280 (5-6) ◽  
pp. 469-474 ◽  
Author(s):  
Xing-Rong Zeng ◽  
Ke-Cheng Gong ◽  
Ke-Nan Weng ◽  
Wan-Sheng Xiao ◽  
Wen-Hong Gan ◽  
...  

2017 ◽  
Vol 17 (1) ◽  
pp. 95 ◽  
Author(s):  
Sri Sudiono ◽  
Mustika Yuniarti ◽  
Dwi Siswanta ◽  
Eko Sri Kunarti ◽  
Triyono Triyono ◽  
...  

Humic acid (HA) extracted from peat soil according to the recommended procedure of the International Humic Substances Society (IHSS) has been tested to remove AuCl4- from aqueous solution. The removal was optimum at pH 2.0 and it was mainly dictated by attachment through hydrogen bonding to unionized carboxyl (–COOH) groups and reduction by the action of the hydroxyl (–OH) groups to gold (Au) metal. The removal of AuCl4- improved after HA was purified through repeated immersion and shaking in a mixed solution containing 0.1 M HCl and 0.3 M HF. When the purification led to the sharp decrease in ash content from 39.34 to 0.85% (w/w) and significant increase in both the –COOH and –OH contents from 3240 to 3487 mmol/kg and from 4260 to 4620 mmol/kg, respectively; the removal of AuCl4- improved from 0.105 to 0.133 mmol/g. This improvement of AuCl4- removal by the purified HA was accompanied by higher ability in reduction to Au metal. The attached AuCl4- on –COOH groups of both crude and purified HAs was qualitatively observed by the characterization result of FT-IR spectroscopy, while the presence of Au metal on the surface of those HAs was verified by the characterization result of XRD.


Catalysts ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 1096
Author(s):  
Ligang Luo ◽  
Xiao Han ◽  
Qin Zeng

A series of Ni-Fe/SBA-15 catalysts was prepared and tested for the catalytic hydrogenation of levulinic acid to γ-valerolactone, adopting methanol as the only hydrogen donor, and investigating the synergism between Fe and Ni, both supported on SBA-15, towards this reaction. The characterization of the synthesized catalysts was carried out by XRD (X-ray powder diffraction), TEM (transmission electron microscopy), H2-TPD (hydrogen temperature-programmed desorption), XPS (X-ray photoelectron spectroscopy), and in situ FT-IR (Fourier transform–infrared spectroscopy) techniques. H2-TPD and XPS results have shown that electron transfer occurs from Fe to Ni, which is helpful both for the activation of the C=O bond and for the dissociative activation of H2 molecules, also in agreement with the results of the in situ FT-IR spectroscopy. The effect of temperature and reaction time on γ-valerolactone production was also investigated, identifying the best reaction conditions at 200 °C and 180 min, allowing for the complete conversion of levulinic acid and the complete selectivity to γ-valerolactone. Moreover, methanol was identified as an efficient hydrogen donor, if used in combination with the Ni-Fe/SBA-15 catalyst. The obtained results are promising, especially if compared with those obtained with the traditional and more expensive molecular hydrogen and noble-based catalysts.


2019 ◽  
Vol 3 (1) ◽  
pp. 34 ◽  
Author(s):  
Nataliia Nastasiienko ◽  
Borys Palianytsia ◽  
Mykola Kartel ◽  
Mats Larsson ◽  
Tetiana Kulik

The studies of pyrolysis of caffeic acid (CA) and its surface complexes is important for the development of technologies of heterogeneous catalytic pyrolysis of plant- and wood- based renewable biomass components. In this work, the structure and thermal transformations of the surface complexes of CA on the surface of nanoceria were investigated using Fourier transform–infrared (FT–IR) spectroscopy, thermogravimetric analysis (TGA) and temperature-programmed desorption mass spectrometry (TPD MS). It was found that CA on the surface of cerium dioxide forms several types of complexes: bidentate carboxylates, monodentate carboxylates and complexes formed as a result of interaction with phenolic hydroxyl groups. This is due to the ability of nanosized cerium dioxide to generate basic hydroxyl groups that can deprotonate phenolic groups to form phenolates on the surface. The main pyrolysis products were identified. The possible ways of forming 3,4-dihydroxyphenylethylene, acetylene carboxylic acid, pyrocatechol and phenol from surface complexes of CA were suggested. It was established that on the nanoceria surface effectively occur the decarboxylation, decarbonylation, and dehydration reactions of the CA, which are the desirable processes in biomass conversion technologies.


ChemCatChem ◽  
2012 ◽  
Vol 4 (5) ◽  
pp. 624-627 ◽  
Author(s):  
Li Wang ◽  
Qin Xin ◽  
Yue Zhao ◽  
Ge Zhang ◽  
Jie Dong ◽  
...  
Keyword(s):  

Catalysts ◽  
2019 ◽  
Vol 9 (1) ◽  
pp. 62 ◽  
Author(s):  
Gunugunuri K. Reddy ◽  
Torin C. Peck ◽  
Charles A. Roberts

Direct decomposition of NO into N2 and O2 (2NO→N2 + O2) is recognized as the “ideal” reaction for NOx removal because it needs no reductant. It was reported that the spinel Co3O4 is one of the most active single-element oxide catalysts for NO decomposition at higher reaction temperatures, however, activity remains low below 650 °C. The present study aims to investigate new promoters for Co3O4, specifically PdO vs. PtO. Interestingly, the PdO promoter effect on Co3O4 was much greater than the PtO effect, yielding a 4 times higher activity for direct NO decomposition at 650 °C. Also, Co3O4 catalysts with the PdO promoter exhibit higher selectivity to N2 compared to PtO/Co3O4 catalysts. Several characterization measurements, including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), H2-temperature programmed reduction (H2-TPR), and in situ FT-IR, were performed to understand the effect of PdO vs. PtO on the properties of Co3O4. Structural and surface analysis measurements show that impregnation of PdO on Co3O4 leads to a greater ease of reduction of the catalysts and an increased thermal stability of surface adsorbed NOx species, which contribute to promotion of direct NO decomposition activity. In contrast, rather than remaining solely as a surface species, PtO enters the Co3O4 structure, and it promotes neither redox properties nor NO adsorption properties of Co3O4, resulting in a diminished promotional effect compared to PdO.


Catalysts ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 155 ◽  
Author(s):  
Zhenheng Diao ◽  
Lushi Cheng ◽  
Xu Hou ◽  
Di Rong ◽  
Yanli Lu ◽  
...  

Hierarchical HZSM-5 membranes were prepared on the inner wall of stainless steel tubes, using amphiphilic organosilane (TPOAC) and mesitylene (TMB) as a meso-porogen and a swelling agent, respectively. The mesoporosity of the HZSM-5 membranes were tailored via formulating the TPOAC/Tetraethylorthosilicate (TPOAC/TEOS) ratio and TMB/TPOAC ratio, in synthesis gel, and the prepared membranes were systematically characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), N2 adsorption–desorption, N2 permeation, inductively coupled plasma (ICP), in situ fourier transform infrared (FT-IR), ammonia temperature-programmed desorption (NH3-TPD), etc. It was found that the increase of the TPOAC/TEOS ratio promoted a specific surface area and diffusivity of the HZSM-5 membranes, as well as decreased acidity; the increase of the TMB/TPOAC ratios led to an enlargement of the mesopore size and diffusivity of the membranes, but with constant acid properties. The catalytic performance of the prepared HZSM-5 membranes was tested using the catalytic cracking of supercritical n-dodecane (500 °C, 4 MPa) as a model reaction. The hierarchical membrane with the TPOAC/TEOS ratio of 0.1 and TMB/TPOAC ratio of 2, exhibited superior catalytic performances with the highest activity of up to 13% improvement and the lowest deactivation rate (nearly a half), compared with the microporous HZSM-5 membrane, due to the benefits of suitable acidity, together with enhanced diffusivity of n-dodecane and cracking products.


2008 ◽  
Vol 8 (9) ◽  
pp. 4743-4746 ◽  
Author(s):  
Haldorai Yuvaraj ◽  
Min Hee Woo ◽  
Eun Ju Park ◽  
Yeong-Soon Gal ◽  
Kwon Taek Lim

Poly(3-octylthiophene) (P3OT)-titanium dioxide (TiO2) nanocomposite powder where TiO2 was embedded with homogeneous dispersion was synthesized by in-situ chemical oxidative polymerization of 3-octylthiophene in the presence of TiO2 nanoparticles in supercritical carbon dioxide (scCO2), using ferric chloride as the oxidant. The synthesized materials could be obtained as dry powder upon venting of CO2 after the polymerization. The composites were subsequently characterized by FT-IR spectroscopy, transmission electron microscopy (TEM), X-ray diffraction studies (XRD), thermogravimetric analysis (TGA) and photoluminescence (PL). The incorporation of TiO2 in the composite was endorsed by FT-IR studies. TGA revealed enhanced thermal stability of P3OT/TiO2 nanocomposite compared to 3-octylthiophene. TEM analysis showed that well dispersed TiO2 nanoparticles in the polymer matrix. Photoluminescence quenching increased with increasing TiO2 concentration in the composite.


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