Efficient Synthesis of Diethyl Carbonate by Mg, Zn Promoted Hydroxyapatite via Transesterification Reaction

Author(s):  
Kartikeya Shukla ◽  
Vimal Chandra Srivastava

AbstractTransesterification of propylene carbonate (PC) and ethanol is a potent non-phosgene route for the synthesis of diethyl carbonate (DEC). In the present study, hydroxyapatite was synthesized and modified using Zn and Mg (Zn/HAP and Mg/HAP). Modified hydroxyapatite was used as catalyst for the synthesis of DEC. The thermal analysis of the catalytic precursor was studied using thermogravimetric-differential thermal analysis. The structural analysis, surface morphology, and nature of active sites over the catalyst surface were studied using techniques such as Fourier transform infrared spectroscopy, X-ray diffraction, N2 adsorption-desorption, scanning electron microscopy, and CO2 temperature-programmed desorption. Effects of reaction conditions like reaction temperature, reaction time and ethanol/PC molar ratio on DEC yield were also studied. The effects of Mg and Zn on HAP were found to be promotional for the synthesis of DEC using PC and ethanol. Mg/HAP was found to be the best among the three catalysts studied owing to its high basicity. Maximum DEC yield of 52.1 % was obtained in 5 h at 433 K using Mg/HAP catalyst.

2017 ◽  
Vol 2017 ◽  
pp. 1-12 ◽  
Author(s):  
Leandro Marques Correia ◽  
Juan Antonio Cecilia ◽  
Enrique Rodríguez-Castellón ◽  
Célio Loureiro Cavalcante ◽  
Rodrigo Silveira Vieira

The CaO solid derived from natural quail eggshell was calcined and employed as catalyst to produce biodiesel via transesterification of sunflower oil. The natural quail eggshell was calcined at 900°C for 3 h, in order to modify the calcium carbonate present in its structure in CaO, the activity phase of the catalyst. Both precursor and catalyst were characterized using Hammett indicators method, X-ray fluorescence (XRF), X-ray diffraction (XRD), thermogravimetric analysis (TG/DTG), CO2temperature-programmed desorption (CO2-TPD), X-ray photoelectronic spectroscopy (XPS), Fourier infrared spectroscopy (FTIR), scanning electron microscopy (SEM), N2adsorption-desorption at −196°C, and distribution particle size. The maximum biodiesel production was of 99.00 ± 0.02 wt.% obtained in the following transesterification reaction conditions:XMR(sunflower oil/methanol molar ratio of 1 : 10.5 mol : mol),XCAT(catalyst loading of 2 wt.%),XTIME(reaction time of 2 h), stirring rate of 1000 rpm, and temperature of 60°C.


2020 ◽  
Vol 10 (6) ◽  
pp. 625
Author(s):  
Said Arhzaf ◽  
Mohammed Naciri Bennani ◽  
Sadik Abouarnadasse ◽  
Hamid Ziyat ◽  
Omar Qabaqous

<p>The fundamental character of the Mg-Al mixed oxide (Mg<sub>n</sub>(Al)O), derived from the Mg-Al hydrotalcite (Mg<sub>n</sub>Al-CO<sub>3</sub>-HT), where n corresponds to the Mg/Al molar ratio (n: 2, 2.5, 3, 3.5 and 4), was studied by using the adsorption of phenol as a probe acid molecule. The hydrotalcite precursors were prepared by the coprecipitation method. Their derived mixed oxides were obtained by thermal treatment at 450°C in a flow of air. The resulting solids were characterized by X-ray fluorescence spectroscopy (XRF), X-ray diffraction (XRD), infrared spectroscopy (FTIR), thermogravimetric and differential thermal analysis             (TG-DTA), nitrogen physisorption (BET) and phenol chemisorption. The phenol adsorption followed by UV-Visible spectrophotometry shows that the basicity increases with the Mg/Al molar ratio, such that maximum quantity of phenol adsorbed (Q<sub>ads</sub> = 0.54 mmol/g <sub>cat</sub>) was obtained with the mixed oxide derived from the Mg-Al hydrotalcite of Mg/Al molar ratio equal to 3.5.</p>


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.


2014 ◽  
Vol 798-799 ◽  
pp. 205-210
Author(s):  
Jairo Alberto Gomez-Cuaspud ◽  
Martin Schmal

We investigated the synthesis of nanosized Co3O4 oxide by the polymerization-combustion technique, with different concentrations (3, 12 and 25% w/w) in the ethanol oxidation reaction. Characterization was done by X-ray fluorescence analysis, X-ray diffraction, temperature programmed reduction, scanning and transmission electronic microscopy and CO and H2 chemisorption. Principal results from physicochemical characterization show that the concentration of the metal oxide influence the product distribution and selectivity under isothermal conditions at 420 °C showed the formation of intermediate etoxi-species and preferential dehydrogenation reaction on stream of material. Specific concentrations result in high conversions and H2 selectivity under present reaction conditions.


2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Aidong Tang ◽  
Yuehua Deng ◽  
Jiao Jin ◽  
Huaming Yang

A novel nanocomposite ZnFe2O4-TiO2/MCM-41 (ZTM) was synthesized by a sol-gel method and characterized through X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), N2adsorption-desorption, Raman spectroscopy, and ultraviolet visible (UV-vis) spectrophotometry. The results confirmed the incorporation of ZnFe2O4-TiO2nanoparticles inside the pores of the mesoporous MCM-41 host without destroying its integrity. ZnFe2O4nanoparticles can inhibit the transformation of anatase into rutile phase of TiO2. Incorporation of ZnFe2O4-TiO2within MCM-41 avoided the agglomeration of nanoparticles and reduced the band gap energy of TiO2to enhance its visible light photocatalytic activity. UV-vis absorption edges of ZTM nanocomposites redshifted with the increase of Zn/Ti molar ratio. The nanocomposite approach could be a potential choice for enhancing the photoactivity of TiO2, indicating an interesting application in the photodegradation and photoelectric fields.


2019 ◽  
Vol 44 (1) ◽  
pp. 37-44 ◽  
Author(s):  
Yunwu Yu ◽  
Lianjie Liang ◽  
Changwei Xu ◽  
Yubo Dai ◽  
Wenhao Pan ◽  
...  

A series of ceria promoted Ni2P catalysts were prepared and evaluated in dibenzothiophene hydrodesulfurization steam. These catalysts were characterized by X-ray diffraction, N2 adsorption–desorption, CO chemisorptions, and X-ray photoelectron spectroscopy. The results showed that the addition of ceria into the bulk Ni2P catalyst was conducive to the formation of the Ni2P phase and contributed to a higher surface area, leading to a better dispersion and smaller crystallite size of Ni2P particles. The CexNi2P catalysts showed higher dibenzothiophene hydrodesulfurization activity than Ni2P catalyst and the Ce0.09Ni2P catalyst showed the highest dibenzothiophene hydrodesulfurization activity. The Ce0.09Ni2P catalyst showed a dibenzothiophene hydrodesulfurization conversion of 94.5% at the reaction conditions of 320°C, 4.0 MPa, a H2/oil ratio of 500 (V/V), and a weight hourly space velocity of 8.0 h−1. The dibenzothiophene was mainly transformed through desulfurization pathway.


Catalysts ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 807
Author(s):  
Zen Maeno ◽  
Xiaopeng Wu ◽  
Shunsaku Yasumura ◽  
Takashi Toyao ◽  
Yasuharu Kanda ◽  
...  

In this study, the characterization of In-exchanged CHA zeolite (In-CHA (SiO2/Al2O3 = 22.3)) was conducted by in-situ X-ray diffraction (XRD) and ammonia temperature-programmed desorption (NH3-TPD). We also prepared other In-exchanged zeolites with different zeolite structures (In-MFI (SiO2/Al2O3 = 22.3), In-MOR (SiO2/Al2O3 = 20), and In-BEA (SiO2/Al2O3 = 25)) and different SiO2/Al2O3 ratios (In-CHA(Al-rich) (SiO2/Al2O3 = 13.7)). Their catalytic activities in nonoxidative ethane dehydrogenation were compared. Among the tested catalysts, In-CHA(Al-rich) provided the highest conversion. From kinetic experiments and in-situ Fourier transform infrared (FTIR) spectroscopy, [InH2]+ ions are formed regardless of SiO2/Al2O3 ratio, serving as the active sites.


2013 ◽  
Vol 291-294 ◽  
pp. 300-306 ◽  
Author(s):  
Hong Yuan ◽  
Qing Shu

Two cesium phosphotungstate-derived solid acid catalysts (Cs2.5H0.5PW12 and Cs0.5H2.5PW12) were prepared. The resulting catalysts were characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), N2 adsorption and desorption isotherm and temperature programmed desorption of ammonia(NH3-TPD). The Cs2.5H0.5PW12 and Cs0.5H2.5PW12 were respectively used to catalyze the tranesterification of castor oil and methanol for the synthesis of biodiesel with the assistance of microwave. Results shown microwave radiation can greatly enhance the transesterification process when compared with conventional heating method. Cs2.5H0.5PW12 showed better catalyst performance than Cs0.5H2.5PW12. A maximum yield of 90% was obtained from the using of 30:1 molar ratio of methanol to castor oil and 15 wt % mass ratio of catalyst to castor oil at 343 K under microwave radiation after 4h.


2020 ◽  
Vol 01 ◽  
Author(s):  
Huiying Wu ◽  
Feng Liang

Background: Porous Au nanomaterials show great potential in the fields of biomedicine, drug delivery and catalysis for the merits of low density, large void space and large specific surface area. The preparation of porous Au nanomaterials is usually carried out by using a hard-templating method which is cumbersome. Methods: Dandelion-like porous Au nanoparticles were synthesized through a soft-templating method in our work. The synthesized porous Au nanoparticles were characterized via transmission electron microscopy (TEM), X-ray diffraction (XRD), energy-dispersive X-ray (EDX) and cyclic voltammetry (CV). The reduction of nitrophenol was carried out to evaluate the catalytic behavior of porous Au nanoparticles. Results: Porous Au nanoparticles prepared were in uniform size (47.9±6.4 nm) and the morphology could be regulated by adjusting the molar ratio of reactants. The apparent rate constant (kapp) value of reducing nitrophenol catalyzed by porous Au nanoparticles was higher than Au nanospheres and nanobranches in similar size. It could be attributed to the large amount of active sites and high proportion of high-order crystal faces proved by CV and XRD. Conclusion: We developed a facile and reproducible method for synthesizing porous Au nanoparticles. The morphology of porous Au nanoparticles can be ajusted by changing the molar ratio of reactants. Porous Au nanoparticles we prepared behaved better in catalysis compared with Au nanospheres and Au nanobranches.


2021 ◽  
Vol 21 (12) ◽  
pp. 6082-6087
Author(s):  
Chih-Wei Tang ◽  
Hsiang-Yu Shih ◽  
Ruei-Ci Wu ◽  
Chih-Chia Wang ◽  
Chen-Bin Wang

The increase of harmful carbon monoxide (CO) caused by incomplete combustion can affect human health even lead to suffocation. Therefore reducing the CO discharged by vehicles or factories is urgent to improve the air quality. The spinel cobalt (II, III) oxide (Co3O4) is an active catalyst for CO abatement. In this study, we tried to fabricate dispersing Co3O4 via the dispersion-precipitation method with acetic acid, formic acid, and oxalic acid as the chelating dispersants. Then, the asprepared samples were calcined at 300 ºC for 4 h to obtain active catalysts, and assigned as Co(A), Co(F) and Co(O) respectively, the amount of the dispersants used are labeled as I (0.12 mole), II (0.03 mole) and III (0.01 mole). For comparison, another CoAP sample was prepared via alkaliinduced precipitation and calcined at 300 ºC. All samples were characterized by X-ray diffraction (XRD), temperature-programmed reduction (TPR), scanning electron microscope (SEM), and nitrogen adsorption/desorption system, and the catalytic activity focused on the CO oxidation. The influence of chelating dispersant on the performance of abatement of CO was pursued in this study. Apparently, the results showed that the chelating dispersant can influence the catalytic activity of CO abatement. An optimized ratio of dispersant can improve the performance, while excess dispersant lessens the surface area and catalytic performance. The series of Co(O) samples can easily donate the active oxygen since the labile Co–O bonding and indicated the preferential performance than both Co(A) and Co(F) samples. The nanorod Co(O)-II showed preferential for CO oxidation, T50 and T90 approached 96 and 127 ºC, respectively. Also, the favorable durability of Co(O)-II sample maintains 95% conversion still for 50 h at 130 ºC and does not emerge deactivation.


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