scholarly journals Hydrogenative Cyclization of Levulinic Acid to γ-Valerolactone with Methanol and Ni-Fe Bimetallic Catalysts

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.

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.


2006 ◽  
Vol 21 (1) ◽  
pp. 112-118 ◽  
Author(s):  
A. Vadivel Murugan ◽  
Mathieu Quintin ◽  
Marie-Helene Delville ◽  
Guy Campet ◽  
Annamraju Kasi Viswanath ◽  
...  

Here we demonstrate the synthesis of a new type of layered poly(3,4-ethylenedioxy- thiophene) (PEDOT)/MoS2 nanocomposite via flocculation of delaminated MoS2 with subsequent in situ oxidative polymerization of 3,4-ethylenedioxythiophene. The resulting nanocomposite was characterized by Fourier transform infrared spectroscopy, powder x-ray diffraction, x-ray photoelectron spectroscopy, thermal analysis, transmission electron microscopy, and four-probe electrical conductivity measurements with respect to temperature. X-ray diffraction results indicated that the exfoliated MoS2 and PEDOT are restacked to produce a novel nanoscale composite material containing alternate nanoribbons of PEDOT in between MoS2 with a basal distance of ∼1.38 nm. The nanocomposite, which could be used as a cathode material for small power rechargeable lithium batteries, has also been demonstrated by the electrochemical insertion of lithium into the PEDOT/MoS2 nanocomposite, where a significant enhancement in the discharge capacity is observed, compared to that of respective pristine molybdenum disulfide.


2012 ◽  
Vol 151 ◽  
pp. 392-395 ◽  
Author(s):  
Xiao Hui Gao ◽  
Yu Feng Li ◽  
Hong Chao Wang

Polyacrylate latex containing fluorine and silicon was successfully synthesized by semi-continuous seed emulsion polymerization, using organic silicon(OSi) monomer, fluorocarbon(FC), methacrylic acid(MAA), and butyl acrylate(BA) as raw materials. Transmission electron microscope(TEM) characterization indicated that the latex particles were form uniform analogous core-shell structure. Dynamic light scattering(DLS) show a narrow size distribution. The results of X-ray photoelectron spectroscopy(XPS) revealed the fluorine and silicon transfer to the film-air interface. The reaction was evaluated using fourier transform infrared(FT-IR) spectrum. The thermal stability of the latex films which analysed by thermogravimetric(TG) was improved due to the join of OSi and FC.


Polymers ◽  
2019 ◽  
Vol 11 (1) ◽  
pp. 72 ◽  
Author(s):  
Yingfeng Zuo ◽  
Xiaoyu He ◽  
Ping Li ◽  
Wenhao Li ◽  
Yiqiang Wu

Three kinds of hydrophobic groups grafted starches of maleic anhydride grafted starch (MAH-g-starch), lactic acid grafted starch (LA-g-starch), and methyl acrylate grafted starch (MA-g-starch) were prepared by in situ solid phase polymerization. The results of Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS) confirmed successful grafting. The grafting ratios of MAH-g-starch, LA-g-starch, and MA-g-starch were 6.50%, 12.45%, and 0.57%, respectively. Influenced by the grafting ratio, LA-g-starch had the best relative hydrophobicity and the largest molecular weight, and those for MA-g-starch were the worst. The surfaces of grafted starches were covered with graft polymer, with obvious surface roughness and bond degree of MAH-g-starch and LA-g-starch. The crystalline structure of grafted starches showed some damage, with LA-g-starch exhibiting the greatest decrease in crystallinity, and less of a change for MA-g-starch. Overall, the grafting reaction improved thermoplasticity, with LA-g-starch the most improved, followed by MAH-g-starch, and then MA-g-starch.


Catalysts ◽  
2018 ◽  
Vol 8 (12) ◽  
pp. 635
Author(s):  
Lingjuan Ma ◽  
Dawei Han ◽  
Hongbin Ma ◽  
Longgang Liu ◽  
Huichao Guo

Highly dispersed CuFe19Ox catalysts with different shapes were prepared and further characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), H2 temperature-programmed reduction (H2-TPR), and in-situ XRD. XRD and TEM results showed that the synthesized CuFe19Ox nanoparticles consisted of CuO and Fe2O3, while CuFe19Ox nanorods consisted of CuFe2O4 and Fe2O3. The reduction properties of CuFe19Ox samples were finely studied by H2-TPR, and the phase composition was identified by in-situ XPS, HR-TEM, and surface TPR (s-TPR). In-situ X-ray photoelectroscopy (XPS) indicated that the metallic Cu and Fe3O4 were the main species after reduction. Moreover, s-TPR studies showed that the reduction performance of copper was significantly affected by the shapes of the Fe3O4 supports. Low-temperature water gas shift (LT-WGS) was chosen to characterize the Cu species on the surface. It was found that reduced CuFe19Ox nanorods had no activity. On the contrary, reduced CuFe19Ox particles showed higher initial WGS activity, where the active Cu0 should originate from the reduction of Cu2O at lower temperatures, as confirmed by the s-TPR profiles.


Author(s):  
Yinfeng Zuo ◽  
Xiaoyu He ◽  
Ping Li ◽  
Wenhao Li ◽  
Yiqiang Wu

Three kinds of hydrophobic groups grafted starches of maleic anhydride grafted starch (MAH-g-starch), lactic acid grafted starch (LA-g-starch), and methyl acrylate grafted starch (MA-g-starch) were prepared by in-situ solid phase polymerization. The results of Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS) were confirmed successful grafting. The grafting ratios of MAH-g-starch, LA-g-starch and MA-g-starch were 6.50%, 12.45%, and 0.57%, respectively. Influenced by the grafting ratio, LA-g-starch had the best hydrophobic properties and the largest molecular weight, and those for MA-g-starch was the worst. The surfaces of grafted starches were covered with graft polymer, with obvious surface roughness and bond degree of MAH-g-starch and LA-g-starch. The crystalline structure of grafted starches showed some damage, with LA-g-starch exhibiting the greatest decrease in crystallinity, and less of a change for MA-g-starch. Overall, the grafting reaction improved thermoplasticity, with LA-g-starch the most improved, followed by MAH-g-starch, and then MA-g-starch.


Catalysts ◽  
2019 ◽  
Vol 9 (12) ◽  
pp. 1018
Author(s):  
Naveed Husnain ◽  
Enlu Wang ◽  
Shagufta Fareed ◽  
Muhammad Tuoqeer Anwar

Maghemite (γ-Fe2O3) catalysts were prepared by two different methods, and their activities and selectivities for selective catalytic reduction of NO with NH3 were investigated. The methods of X-ray powder diffraction (XRD), Brunauer–Emmett–Teller (BET), X-ray photoelectron spectroscopy (XPS), hydrogen temperature-programmed reduction (H2-TPR), ammonia temperature-programmed desorption (NH3-TPD), transmission electron microscopy (TEM), Energy-dispersive X-ray spectroscopy (EDS), and in situ diffuse reflectance infrared Fourier transform spectroscopy (in situ DRIFTS) were used to characterize the catalysts. The resulted demonstrated that the γ-Fe2O3 nanoparticles prepared by the facile method (γ-Fe2O3–FM) not only exhibited better NH3-SCR activity and selectivity than the catalyst prepared by the coprecipitation method but also showed improved SO2 tolerance. This superior NH3-SCR performance was credited to the existence of the larger surface area, better pore structure, a high concentration of lattice oxygen and surface-adsorbed oxygen, good reducibility, a lot of acid sites, lower activation energy, adsorption of the reactants, and the existence of unstable nitrates on the surface of the γ-Fe2O3–FM.


Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


2021 ◽  
pp. 174751982098472
Author(s):  
Jun Yu ◽  
Ying Han ◽  
Guoqing Chen ◽  
Xiuzhen Xiao ◽  
Haifang Mao ◽  
...  

The effect of carbon nanotubes on the catalytic properties of Rh-Mn-Li/SiO2 catalysts was investigated for CO hydrogenation. The catalysts were comprehensively characterized by means of X-ray power diffraction, N2 sorption, transmission electron microscope, H2–temperature-programmed reduction, CO–temperature-programmed desorption, temperature-programmed surface reaction, and X-ray photoelectron spectroscopy. The results showed that an appropriate amount of carbon nanotubes can be attached to the surface of the SiO2 sphere and can improve the Rh dispersion. Moderate Rh-Mn interaction can be obtained by doping with the appropriate amount of carbon nanotubes, which promotes the formation of strongly adsorbed CO and facilitates the progress of CO insertion, resulting in the increase in the selectivity of C2+ oxygenate synthesis.


2003 ◽  
Vol 18 (5) ◽  
pp. 1123-1130 ◽  
Author(s):  
V. Oliveira ◽  
R. Vilar

This paper aims to contribute to the understanding of column formation mechanisms in Al2O3–TiC ceramics micromachined using excimer lasers. Chemical and structural characterization of columns grown in Al2O3–TiC composite processed with 200 KrF laser pulses at 10 J/cm2 was carried out by scanning electron microscopy, transmission electron microscopy, x-ray photoelectron spectroscopy, and x-ray diffraction analysis. Fully developed columns consist of a core of unprocessed material surrounded by an outer layer of Al2TiO5, formed in oxidizing conditions, and an inner layer, formed in reducing conditions, composed of TiC and Al3Ti or an AlTi solid solution. Possible mechanisms of column formation are discussed.


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