NaZSM-5-catalyzed dimethyl carbonate synthesis via the transesterification of ethylene carbonate with methanol

2011 ◽  
Vol 89 (5) ◽  
pp. 544-548 ◽  
Author(s):  
Zhen-Zhen Yang ◽  
Xiao-Yong Dou ◽  
Fang Wu ◽  
Liang-Nian He

NaZSM-5 zeolite was found to be an efficient heterogeneous catalyst for the synthesis of dimethyl carbonate (DMC), which can serve as a building block, an additive to fuel oil, and an electrolyte in batteries, via the transesterification of ethylene carbonate (EC) with methanol. Notably, 77% DMC yield and 97% selectivity were achieved under mild reaction conditions. Furthermore, the effects of various reaction parameters such as catalyst loading, reaction time, and methanol/EC molar ratio on the catalytic performance were investigated in detail. This protocol was found to be applicable to a variety of alcohols, producing the corresponding dialkyl carbonates with moderate yields and selectivities. Moreover, the catalyst can be recovered by simple filtration with retention of catalytic activity; a stable crystal configuration and a slight alteration of its superficial structure were observed by X-ray diffraction and BET measurements.

2014 ◽  
Vol 1008-1009 ◽  
pp. 319-322
Author(s):  
Gong De Wu ◽  
Xiao Li Wang ◽  
Zhi Li Zhai ◽  
Ao Yun Cao

The Mg-Al mixed oxides were deposited on the MCM-41 via the coprecipitation followed by thermal decomposition and characterized by many techniques. In the transesterification of glycerol (GL) with dimethyl carbonate (DMC), the resulting supported catalysts exhibited much higher catalytic performance than the pure Mg-Al mixed oxides, which was ascribed to the increased basicity. Under the optimal reaction conditions, the obtained data showed that at DMC/glycerol molar ratio of 3:1, catalyst loading of 0.3 g and reaction temperature of 373 K, the glycerol conversion and glycerol carbonate yield from the process was 98.7 % and 92.5%, respectively.


Catalysts ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 710
Author(s):  
Linmeng Huo ◽  
Tian Wang ◽  
Keng Xuan ◽  
Lei Li ◽  
Yanfeng Pu ◽  
...  

The adsorption and activation of both CO2 and methanol are mainly affected by the distance of the Lewis acid site, Zr4+, and Lewis base, Zr4+/O2−, of the Zr-based catalysts. In this paper, Zr-incorporated SBA-15 (Zr-SBA-15) and Zr-grafted SBA-15 (Zr/SBA-15) catalysts were prepared with different Zr environments, and were analyzed with N2 adsorption–desorption isotherms, X-ray diffraction, UV-vis spectra, and XPS. It was proposed that Zr-SBA-15 catalyst with Si-O-Zr-OH and Zr-O-Si-OH structure exhibited non-adjacent sites between Zr4+ and Zr4+/O2−, while Zr/SBA-15 catalyst with Zr-O-Zr-OH structure showed neighboring sites between Zr4+ and Zr4+/O2−. Furthermore, the Zr/SBA-15 catalyst exhibited good catalytic activity, while no DMC was detected over the Zr-SBA-15 catalyst at the same reaction conditions. For combined in situ infrared and catalytic performance, it was indicated that the methanol and CO2 could be activated to form DMC, only when the Zr4+ and Zr4+/O2− sites existed and were adjacent to each other in the Zr-O-Zr-OH of Zr/SBA-15 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.


Polymers ◽  
2021 ◽  
Vol 13 (22) ◽  
pp. 3924
Author(s):  
José Castanheiro

Esterification of caprylic acid with methanol was performed over chitosan with sulfonic acid groups, as a catalyst, at 60 °C. The sulfonic acid groups were introduced into chitosan (CH) by using chlorosulfonic acid. Catalysts were characterized by scanning electron microscopy (SEM), elemental analysis, thermogravimetric analysis (TGA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and acid–base titration. Catalytic activity increased with the amount of sulfonic acid groups present on chitosan. The 4–CH–SO3H catalyst (chitosan with sulfonic acid groups—sample 4 prepared) showed the highest activity of all materials. The esterification of caprylic acid with methanol was optimized using a 4–CH–SO3H catalyst. Under optimized reaction conditions, it was found that, at 60 °C, with 0.2 g of catalyst loading and with a molar ratio methanol to caprylic acid equal 1:95, a caprylic acid conversion of about 83%, after 4 h could be obtained. Catalytic stability of the 4–CH–SO3H material was evaluated through consecutive batch runs. After the second batch, the catalytic activity stabilized.


Author(s):  
SUNNY SONI ◽  
MADHU AGARWAL

Biodiesel is a renewable liquid fuel made from natural, renewable biological sources such as edible and non edible oils. Over the last years, biodiesel has gained more market due to its benefits and because it appears as the natural substitute for diesel. Reasons for growing interest in biodiesel include its potential for reducing noxious emissions, potential contributions to rural economic development, as an additional demand center for agricultural commodities, and as a way to reduce reliance on foreign oil. Biodiesel was prepared from soybean oil by transesterification with methanol in the presence of cement clinker. Cement clinker was examined as a catalyst for a conversion of soybean oil to fatty acid methyl esters (FAMEs). It can be a promising heterogeneous catalyst for the production of biodiesel fuels from soybean oil because of high activity in the conversion and no leaching in the transesterification reaction. The reaction conditions were optimized. A study for optimizing the reaction parameters such as the reaction temperature, and reaction time, was carried out. The catalyst cement clinker composition was characterized by XRF. The results demonstrate that the cement clinker shows high catalytic performance & it was found that the yield of biodiesel can reach as high as 84.52% after 1 h reaction at 65°C, with a 6:1 molar ratio of methanol to oil, 21 wt% KOH/cement clinker as catalyst.


Synthesis ◽  
2019 ◽  
Vol 51 (08) ◽  
pp. 1770-1778 ◽  
Author(s):  
Manuele Musolino ◽  
Fabio Aricò

A novel halogen-free synthesis of benzo-fused six-membered 1,4-heterocycles through the chemistry of dialkyl carbonates is reported. Commercially available catechol, 2-aminophenol, and 2-amino­thiophenol were reacted first with ethylene carbonate in an autoclave to give O-hydroxyethyl, N-hydroxyethyl, and S-hydroxyethyl derivatives respectively, through a BAl2 mechanism. Then 2-(2-hydroxyethoxy)phenol and 2-(2-hydroxyethylamino)phenol were cyclized in excellent yields by reaction with dimethyl carbonate (DMC) and DABCO as a bi­cyclic organic base to give the corresponding benzodioxine and benzoxazine derivative, respectively. Moreover, 2-(2-aminophenylthio)ethanol afforded the benzothiazine derivative in good yield by reaction with DMC with an excess of a strong base such as NaH. The investigation on the cyclization reaction has highlighted that several equilibria are involved leading to the formation of carbonate and carbamate intermediates through BAc2 mechanisms. Depending on the reaction conditions employed, these intermediates may undergo either kinetic-controlled ring closure by a BAl2 mechanism or by-product formation.


2019 ◽  
Vol 11 (12) ◽  
pp. 1764-1772 ◽  
Author(s):  
Ji-Bin An ◽  
Dai-Peng Hu ◽  
Yan-Lin Li ◽  
Na-Li Chen

The Magnetic photocatalytic cobalt ferrite/graphitic-carbon nitride (CoFe2O4/g-C3N4) composites with enhanced photocatalytic activity were successfully fabricated through a simple calcination method. Scanning electron microscopy, powder X-ray diffraction, and infrared spectroscopy were applied to characterize the samples. The photocatalytic behavior of CoFe2O4/g-C3N4 was assessed by degradation of atrazine in photo Fenton-like system under visible light irradiation. The results showed that CoFe2O4/g-C3N4 with 2.0 gL–1 catalyst loading in the presence of 1 mM peroxymonosulfate (PMS) exhibited the best catalytic performance, and more than 97% of atrazine was destructed in 12 min. This enhancement could be attributed to the synergistic effect between CoFe2O4 and g-C3N4 promoting longer lifetime of separated electron–hole pairs derived from the formation of the heterojunction between CoFe2O4 and g-C3N4. This could enhance the composite-mediated activation of PMS for the visible-light driven degradation of atrazine. Moreover, the quenching tests showed that sulfate radicals were responsible for the atrazine degradation. CoFe2O4/g-C3N4 composites have strong magnetic ability, thus their recovery from water could be readily achieved by applying external magnetic field. This study demonstrates reasonable performance of the PMS/CoFe2O4/g-C3N4 system in water matrix as potentially important candidate for environmental remediation.


Author(s):  
Marwan Marwan ◽  
Eti Indarti ◽  
Darmadi Darmadi ◽  
Wahyu Rinaldi ◽  
Dzikri Hamzah ◽  
...  

Triacetin, an alternative biodiesel additive, was prepared by esterification of glycerol with acetic acid in the presence of chemically activated natural zeolite. The esterification was carried out in a small reaction flask under microwave irradiation. The catalyst was characterized for its morphology by SEM and its chemical composition by X-ray Diffraction (XRD). The Scanning Electron Microscopy (SEM) micrograph indicates improved surface area of the zeolite, while the XRD analysis shows an increase in Si/Al ratio from natural zeolite to 6.042 and its crystallinity value of 12.23%. The Fourier Transform Infra Red (FTIR) analysis obtained showed that microwave-heated samples have an esters group spectrum of triacetin at 1702 cm-1. The conversion value of glycerol was more than 95% at molar ratio of the reactants 1:9 and catalyst loading of 3%. The selectivities for monoacetin, diacetin and triacetin were 80.1%, 15.4%, and 4.5% at 60 minutes, and 43.0%, 48.6%, and 8.3% at 90 minutes. It shows that the conversion took place in consecutive steps and the use of microwave allows the reaction proceeding at milder condition. Copyright © 2019 BCREC Group. All rights reserved 


Catalysts ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 478 ◽  
Author(s):  
Alex de Nazaré de Oliveira ◽  
Erika Tallyta Leite Lima ◽  
Eloisa Helena de Aguiar Andrade ◽  
José Roberto Zamian ◽  
Geraldo Narciso da Rocha Filho ◽  
...  

The present work was aimed to investigate the catalytic activity of a mesoporous catalyst synthesized from 3-mercaptopropyltrimethoxysilane (MPTS) functionalized Amazonian flint kaolin in the acetylation of eugenol with acetic anhydride. Materials were characterized by thermogravimetry (TGA), N2 adsorption (BET), X-ray dispersive energy spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and acid-base titration. The results presented proved the efficiency of flint kaolin as an alternative source in the preparation of mesoporous materials, since the material exhibited textural properties (specific surface area of 1071 m2 g−1, pore volume of 1.05 cm3 g−1 and pore diameter of 3.85 nm) and structural properties (d100 = 4.35 nm, a0 = 5.06 nm and Wt = 1.21 nm) within the required and characteristic material standards. The catalyst with the total amount of acidic sites of 4.89 mmol H+ g−1 was efficient in converting 99.9% of eugenol (eugenol to acetic anhydride molar ratio of 1:5, 2% catalyst, temperature and reaction time 80 °C and 40 min reaction). In addition, the reused catalyst could be successfully recycled with 92% conversion activity under identical reaction conditions.


Author(s):  
Ganapati D. Yadav ◽  
Jyoti B. Sontakke

Optically active 1-phenylethanol is used as a chiral building block and synthetic intermediate in pharmaceutical and fine-chemical industries. Lipase - catalyzed kinetic resolution of (R,S)-1-phenylethanol with vinyl acetate as an acyl donor and Candida antarctica immobilized lipase as a biocatalyst in a batch reactor was optimized using Response Surface Methodology (RSM). Four-factor-five-level central composite rotatable design (CCRD) was employed to evaluate the effect of synthesis parameters such as speed of agitation, enzyme loading, temperature and acyl donor/alcohol molar ratio, on conversion, enantiomeric excess (ee), enantioselectivity and initial rate. Optimum reaction conditions obtained were; mole ratio of acyl donor: ester of 2:1, temperature of 42.5 °C, catalyst loading of 1.6x10-3 g.cm-3 and speed of agitation of 336 rpm. Analysis of variance was performed to determine significantly affecting variables and interactions between the process parameters.


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