scholarly journals Study the Effect of Various Sulfonation Methods on Catalytic Activity of Carbohydrate-Derived Catalysts for Ester Production

Catalysts ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 638
Author(s):  
Nur Hidayah Deris ◽  
Umer Rashid ◽  
Soroush Soltani ◽  
Thomas Shean Yaw Choong ◽  
Imededdine Arbi Nehdi

In the present study, four types of sulfonation method, including thermal treatment with concentrated sulfuric acid (H2SO4), thermal decomposition of ammonium sulphate (NHSO4), thermal treatment with chlorosulfonic in chloroform (HSO3Cl), and in situ polymerization of poly(sodium4-styrenesulfonate) (PSS), were employed to convert incomplete carbonized glucose (ICG) to sulfonated heterogeneous catalysts for the fatty acid methyl ester (FAME) production. The characteristics of synthesized catalysts were further examined using Raman spectroscopy, Fourier transformation infrared (FT-IR), ammonia temperature programmed desorption (NH3-TPD), Brunauer–Emmett–Teller (BET), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and energy dispersive X-ray (EDX). According to experiments, the sulfonic acid density was varied in a range from 4.408 to 14.643 mmol g−1 over various sulfonation methods. The catalytic activity of synthesized catalysts over different sulfonation methods was determined by performing the conversion of palm fatty acid distillate (PFAD) to ester synthesis in a batch-system reactor. The findings reveal that using PSS-ICG resulted in the highest FAME yield of 96.3% followed by HSO3Cl-ICG of 94.8%, NHSO4-ICG of 84.2%; and H2SO4-ICG of 77.2%. According to results, the ICG sulfonated by PSS method with the highest acid density (14.643 mmol g−1) gave the highest catalytic activity over PFAD conversion to biodiesel. According to experiment results, acid density played a crucial role over FAME yield percentage. Besides acid density, it is also worth mentioning that various sulfonation methods including different mechanisms, chemicals and sulfonating agents played crucial roles in the FAME yield percentage.

2015 ◽  
Vol 44 (19) ◽  
pp. 8906-8916 ◽  
Author(s):  
Sankar Das ◽  
Subhra Jana

Halloysite/metal nanocomposites have been synthesized through the immobilization of preformed and in situ synthesized metal nanoparticles over halloysite surfaces, which in turn produce efficient, cost-effective, and environmentally benign heterogeneous 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.


2007 ◽  
Vol 124-126 ◽  
pp. 287-290 ◽  
Author(s):  
Fei Liu ◽  
Yong Jun He ◽  
Jeung Soo Huh

The nano-CeO2 was synthesized by two-step solid-phase reaction. The image of TEM showed that nano-CeO2 with an average size of about 70 nm. The series of polyaniline/nano-CeO2 composites with different PANi: CeO2 ratios were prepared by in-situ polymerization in the presence of hydrochloric acid (HCl) as dopant by adding nano-CeO2 into the polymerization reaction mixture of aniline. The composites obtained were characterized by FT-IR and UV-vis spectroscopy analysis. The FT-IR spectra of nanocomposites indicate different blue-shifts, attributed to C–N stretching mode for benzenoid unit. The UV-vis spectra of nanocomposites display einstein-shifts compared with PANi at 620nm. The conductivity properties of the composites are also changed compare to the pure PANi. These results suggest that the interactions between the polymer matrix and nanoparticles take place in polyaniline/nano- CeO2 composites.


e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Inês Matos ◽  
Auguste Fernandes ◽  
Rita Catalão ◽  
Ana M. Botelho do Rego ◽  
José R. Ascenso ◽  
...  

AbstractIn this paper we present two different techniques for the preparation of single site heterogeneous catalyst. The first method consists in the impregnation of a solution of the organometallic compound in MCM41. The second method intends to establish the in situ synthesis of the complex within the solid’s pores by the reaction of the organic ligand with the metal cation previously introduced in the support. The direct deposition of the organometallic complex in the support resulted in an active catalyst which gives polyethylene with the same microstructure as the one obtained with the related homogeneous systems. The heterogeneous catalysts obtained by reaction of the ligand with the metal already present in the support showed a lower catalytic activity.


2018 ◽  
Vol 120 ◽  
pp. 140-146 ◽  
Author(s):  
Nakyung Choi ◽  
Da Som No ◽  
Heejin Kim ◽  
Byung Hee Kim ◽  
Jieun Kwak ◽  
...  

2019 ◽  
Vol 2019 ◽  
pp. 1-9
Author(s):  
Di Zhang ◽  
Huaiyin Chen ◽  
Ruoyu Hong

In this paper, the magnetite/polyaniline (PANI) nanocomposite was prepared by the novel reverse in situ polymerization method. Fe3O4 magnetic nanoparticles were synthesized in situ in PANI chloroform solution to form a suspension containing the Fe3O4/PANI nanocomposite. It overcame the disadvantage of oxidation of the Fe3O4 by the oxidant in conventional method. The Fe3O4/PANI chloroform suspension and the Fe3O4/PANI powder were characterized by FT-IR, TEM, XRD, vibrating sample magnetometer, Gouy magnetic balance, conductivity meter, and vector network analyzer. It is demonstrated that the Fe3O4/PANI suspension has a good electrical conductivity that is up to 2.135 μS/cm at the optimal ratio of reactants. The Fe3O4 nanoparticles are well dispersed in the PANI network with a particle size of about 10 nm. Fe3O4/PANI powder has high saturation magnetization and magnetic susceptibility, as well as a broad application prospect in the field of electromagnetic devices. The Fe3O4/PANI powder exhibits an excellent microwave absorption behavior, which can be an outstanding candidate for the rapid development of broadband shielding materials.


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.


1994 ◽  
Vol 48 (7) ◽  
pp. 827-832 ◽  
Author(s):  
Graeme J. Millar ◽  
David Newton ◽  
Graham A. Bowmaker ◽  
Ralph P. Cooney

An in situ infrared cell capable of studying reactions over heterogeneous catalysts in the temperature range 77 to 773 K has been designed. In particular, the adsorption of formic acid on a model Cu/SiO2 methanol synthesis catalyst was investigated. Exposure of a reduced copper surface to formic acid at 300 K resulted in the formation of both formic acid molecules, which were ligated to the copper catalyst, and chemisorbed bidentate copper formate species. Under temperature-programming conditions, the bidentate species displayed a maximum rate of desorption at 433 K, which correlates to a desorption activation energy of 120 kJ mol−1. In contrast, on the reoxidized catalyst, unidentate formate species were preferentially formed. These exhibited a maximum rate of desorption at a temperature of 408 K, and a desorption activation energy of 113 kJ mol−1. A mechanism was postulated to explain this behavior, and evidence was presented to show that useful kinetic data can be obtained for desorption from a catalyst in the form of a pressed disk.


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