Synthesis of Biodiesel from Castor Oil Catalyzed by Cesium Phosphotungstate with the Assistance of Microwave

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.

Author(s):  
Hong Yuan ◽  
Bolun Yang ◽  
Hailiang Zhang ◽  
Xiaowei Zhou

The castor oil was adopted to synthesize biodiesel (Fatty Acid Methyl Ester, FAME) under microwave radiation. Acid catalysts (NaHSO4•H2O and AlCl3) and heterogeneous base catalyst (Na2CO3) were evaluated in the present study. The amounts of FAME in the product were analyzed by high performance liquid chromatography (HPLC). Experimental results show that the microwave radiation was an efficient method to enhance the reaction process. When the transesterification was carried out at 338 K, with 18:1 molar ratio of methanol to castor oil, 7.5wt% mass ratio of catalyst to castor oil, 200w microwave radiation power and 120 minutes reaction time, yields of 74, 73, 90% were obtained respectively using catalysts of NaHSO4•H2O, AlCl3 and Na2CO3. The energy consumed by microwave heating and conventional heating in transesterification were measured, and the results showed that the microwave heating consumed less energy than the conventional heating to achieve the same amount of FAME.


Catalysts ◽  
2019 ◽  
Vol 9 (12) ◽  
pp. 1069 ◽  
Author(s):  
Abir Azara ◽  
El-Hadi Benyoussef ◽  
Faroudja Mohellebi ◽  
Mostafa Chamoumi ◽  
François Gitzhofer ◽  
...  

In this study, iron-rich mining residue (UGSO) was used as a support to prepare a new Ni-based catalyst via a solid-state reaction protocol. Ni-UGSO with different Ni weight percentages wt.% (5, 10, and 13) were tested for C2H4 dry reforming (DR) and catalytic cracking (CC) after activation with H2. The reactions were conducted in a differential fixed-bed reactor at 550–750 °C and standard atmospheric pressure, using 0.5 g of catalyst. Pure gases were fed at a molar ratio of C2H4/CO2 = 3 for the DR reaction and C2H4/Ar = 3 for the CC reaction. The flow rate is defined by a GHSV = 4800 mLSTP/h.gcat. The catalyst performance is evaluated by calculating the C2H4 conversion as well as carbon and H2 yields. All fresh, activated, and spent catalysts, as well as deposited carbon, were characterized by Brunauer–Emmett–Teller (BET), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDX), transmission electron microscopy (TEM), temperature programmed reduction (TPR), and thermogravimetric analysis (TGA). The results so far show that the highest carbon and H2 yields are obtained with Ni-UGSO 13% at 750 °C for the CC reaction and at 650 °C for the DR reaction. The deposited carbon was found to be filamentous and of various sizes (i.e., diameters and lengths). The analyses of the results show that iron is responsible for the growth of carbon nanofilaments (CNF) and nickel is responsible for the split of C–C bonds. In terms of conversion and yield efficiencies, the performance of the catalytic formulations tested is proven at least equivalent to other Ni-based catalyst performances described by the literature.


Author(s):  
Hong Yuan ◽  
Xiaoqin Ma ◽  
Jie He ◽  
Zhaoyang Dong

AbstractThe solid acid catalysts SO42−/Fe2O3were prepared by impregnation technique, and the preparation conditions were different in calcination temperature, concentration of impregnation solution of H2SO4and impregnation time. The characterization was performed by using Fourier transform infrared spectrometer (FTIR), X-ray diffraction (XRD), Temperature programed desorption of NH3(NH3‒TPD), N2‒BET and microwave absorbing test. As shown by FTIR spectra, the S=O functional group existed in the sample, which was essential for the strong acidity of the SO42‒/MxOytype solid acids. The XRD results indicated that when the calcination temperature exceeded 400℃, iron in SO42‒/Fe2O3transformed from amorphous to crystalline phase. The results from NH3-TPD showed that the prepared sample possessed strong acid and superacid sites. As shown by N2-BET results, the BET surface area of the samples was up to 200m2/g, and their pore size distributions essentially belonged to mesoporous characteristic distribution. The SO42−/Fe2O3solid acid catalysts were used for the transesterification of castor oil under microwave radiation to produce biodiesel. The amounts of FAME in the product were analyzed by high-performance liquid chromatography. The highest yield of product was 65.3 wt.% when the reaction temperature was 65 ℃, alcohol/oil molar ratio was 30/1, catalyst loading was 20 wt.%, the reaction time was 3 h and the power of microwave was 300 w. Furthermore, the reaction results showed that SO42‒/Fe2O3had better catalytic activity under microwave radiation than under conventional heating condition.


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.


2005 ◽  
Vol 885 ◽  
Author(s):  
Oscar A. González ◽  
Miguel A. Valenzuela ◽  
Jin-An Wang

ABSTRACTSi-Ce-O mixed solids (50, 30, 10 and 5, Si/Ce molar ratio) were prepared by using Ce(NO3)3·6H2O as cerium source, tetraethyl orthosilicate (TEOS) as Si precursor and cetyltrimethylammonium bromide (CTABr) as synthesis template. The Ni catalysts were prepared by impregnation of the supports using Ni-acetilacetonate (30 wt.% Ni) as Ni source. The samples were characterized by: X-ray diffraction, temperature-programmed reduction (TPR), and TEM. The nickel reduction degree decreased with the addition of cerium, even in low concentration. When methane was decomposed over all the catalysts only hydrogen was obtained as a gaseous product. The addition of cerium brought about a significant increase in stability compared with Ni/SiO2 catalyst. These preliminary results indicated that CeO2 addition improves the dispersion of Ni particles leading to a better distribution of deposited carbon and increasing the lifetime of Ni particles.


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 15 (1) ◽  
pp. 231-241 ◽  
Author(s):  
Maria Dewi Astuti ◽  
Ditya Kristina ◽  
Rodiansono Rodiansono ◽  
Dwi Rasy Mujiyanti

One-pot selective conversion of biomass-derived furfural (FFald) into cyclopentanone (CPO) or cyclopentanol (CPL) using bimetallic nickel-based supported on TiO2 (denoted as Ni-M(3.0)/TiO2; M = Co and Fe; 3.0 is Ni/M molar ratio) have been investigated. Catalysts were synthesized via a hydrothermal method at 150 °C for 24 h, followed by H2 reduction at 450 °C for 1.5 h. X-ray Diffraction (XRD) analysis  showed that the formation of Ni-Co alloy phase at 2θ = 44.2° for Ni-Co(3.0)/TiO2 and Ni-Fe alloy at 2θ = 44.1° for Ni-Fe(3.0)/TiO2. The amount of acid sites was measured by using ammonia-temperature programmed desorption (NH3-TPD). Ni-Co(3.0)/TiO2 has three NH3 desorption peaks at 180 °C, 353 °C, and 569 °C with acid site amounts of 1.30 µmol.g-1, 1.0 µmol.g-1, and 2.0 µmol.g-1,        respectively. On the other hand, Ni-Fe(3.0)/TiO2 consisted of NH3 desorption peaks at 214 °C and 626 °C with acid site amounts of 3.3 µmol.g-1and 2.0 µmol.g-1, respectively. Both Ni-Co(3.0)/TiO2 and Ni-Fe(3.0)/TiO2 catalysts were found to be active for the selective hydrogenation of FFald to furfuryl alcohol (FFalc) at low temperature of 110 °C, H2 3.0 MPa, 3 h with FFalc selectivity of 81.1% and 82.9%, respectively. High yields of CPO (27.2%) and CPL (41.0%) were achieved upon Ni-Fe(3.0)/TiO2 when the reaction temperature was increased to 170 °C, 3.0 MPa of H2, and a reaction time of 6 h. The yield of CPO+CPL on the reused catalyst decreased slightly after the second reaction run, but the activity was maintained for at least three consecutive runs. Copyright © 2020 BCREC Group. All rights reserved


2018 ◽  
Author(s):  
Tasneem Siddiquee ◽  
Abdul Goni

Chemical treatment of CoX<sub>2</sub><b><sup>. </sup></b>6H<sub>2</sub>O (X = Cl, Br, I) with the potentially tridentate PNP pincer ligand 2,6-bis(di-<i>tert</i>-butylphosphinomethyl)pyridine in 1:1 molar ratio results in cobalt(II) halide-PNP pincer complexes. The effect of the hydrated metal source on molecular structure and geometry of the complexes was studied by single crystal X-ray diffraction analysis. The complexes are neutral and the cobalt center adopts a penta-coordinate system with potential atropisomerization. Within the unit cell there are two distinct molecules per asymmetric unit. One of the two phosphorus atoms in the PNP ligand was observed to be partially oxidized to phosphinoxide. Disorder in the structure reflects a mixture of square pyramidal and distorted tetrahedral geometry.


Catalysts ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 346
Author(s):  
Sonam Goyal ◽  
Maizatul Shima Shaharun ◽  
Ganaga Suriya Jayabal ◽  
Chong Fai Kait ◽  
Bawadi Abdullah ◽  
...  

A set of novel photocatalysts, i.e., copper-zirconia imidazolate (CuZrIm) frameworks, were synthesized using different zirconia molar ratios (i.e., 0.5, 1, and 1.5 mmol). The photoreduction process of CO2 to methanol in a continuous-flow stirred photoreactor at pressure and temperature of 1 atm and 25 °C, respectively, was studied. The physicochemical properties of the synthesized catalysts were studied using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. The highest methanol activity of 818.59 µmol/L.g was recorded when the CuZrIm1 catalyst with Cu/Zr/Im/NH4OH molar ratio of 2:1:4:2 (mmol/mmol/mmol/M) was employed. The enhanced yield is attributed to the presence of Cu2+ oxidation state and the uniformly dispersed active metals. The response surface methodology (RSM) was used to optimize the reaction parameters. The predicted results agreed well with the experimental ones with the correlation coefficient (R2) of 0.99. The optimization results showed that the highest methanol activity of 1054 µmol/L.g was recorded when the optimum parameters were employed, i.e., stirring rate (540 rpm), intensity of light (275 W/m2) and photocatalyst loading (1.3 g/L). The redox potential value for the CuZrIm1 shows that the reduction potential is −1.70 V and the oxidation potential is +1.28 V for the photoreduction of CO2 to methanol. The current work has established the potential utilization of the imidazolate framework as catalyst support for the photoreduction of CO2 to methanol.


Materials ◽  
2020 ◽  
Vol 14 (1) ◽  
pp. 48
Author(s):  
Pawel Mierczynski ◽  
Magdalena Mosińska ◽  
Lukasz Szkudlarek ◽  
Karolina Chalupka ◽  
Misa Tatsuzawa ◽  
...  

Biodiesel production from rapeseed oil and methanol via transesterification reaction facilitated by various monometallic catalyst supported on natural zeolite (NZ) was investigated. The physicochemical characteristics of the synthesized catalysts were studied by X-ray diffraction (XRD), Brunauer–Emmett–Teller method (BET), temperature-programmed-reduction in hydrogen (H2-TPR), temperature-programmed-desorption of ammonia (NH3-TPD), Scanning Electron Microscope equipped with EDX detector (SEM-EDS), and X-ray photoelectron spectroscopy (XPS) methods. The highest activity and methyl ester yields were obtained for the Pt/NZ catalyst. This catalyst showed the highest triglycerides conversion of 98.9% and fatty acids methyl esters yields of 94.6%. The activity results also confirmed the high activity of the carrier material (NZ) itself in the investigated reaction. Support material exhibited 90.5% of TG conversion and the Fatty Acid Methyl Esters yield (FAME) of 67.2%. Introduction of noble metals improves the TG conversion and FAME yield values. Increasing of the metal loading from 0.5 to 2 wt.% improves the reactivity properties of the investigated catalysts.


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