scholarly journals FSM-16-SO3H nanoparticles as a novel heterogeneous catalyst: preparation, characterization, and catalytic application in the synthesis of polyhydroquinolines

2018 ◽  
Vol 41 (3-4) ◽  
pp. 91-101 ◽  
Author(s):  
Somayeh Hashemi-Uderji ◽  
Mohammad Abdollahi-Alibeik ◽  
Reza Ranjbar-Karimi

Abstract FSM-16-SO3H nanoparticles were prepared using a sol-gel method at room temperature. The prepared FSM-16-SO3H was used to catalyze the synthesis of polyhydroquinolines through a one-pot, four-component reaction of aldehydes, dimedone, ethyl cyanoacetate, and ammonium acetate under reflux condition in EtOH as a green solvent. To investigate the textural properties of the prepared catalyst, various techniques were applied such as X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscope, and Brunauer–Emmett–Teller. High catalytic activity, easy handling, and thermal stability are the superior properties that could be denoted after successive investigations of this catalyst. In addition, the catalyst can be recovered easily and reused effectively for several cycles.

2021 ◽  
Author(s):  
Mingshan Qin ◽  
Juan Gao ◽  
Dongwei Wei ◽  
Liuan Li ◽  
Cun Li ◽  
...  

Abstract Because of their unique surface area and adjustable pore size, Metal-Organic Frameworks(MOFs) have been widely used in lots of research fields, such as catalysis, energy storage, sensing, separation. In this paper, as for the Knoevenagel reaction, UiO66 and other UiO series MOFs were synthesized and modified. UiO66 nanoparticles were prepared by one-pot method. 2-aminopyridine, 3-aminopyridine and 4-aminopyridine were used to prepare UiO66-2Py, UiO66-3Py and UiO66-4Py nanoparticles. UiO66-2Py, UiO66-3Py and UiO66-4Py nanoparticles were modified by activated arginine, lysine and glycine to synthesize UiO66-2Py-Arg, UiO66-3Py-Lys and UiO66-4Py-Gly. Finally, the obtained samples were used for the Knoevenagel catalytic condensation reactions of benzaldehyde and ethyl cyanoacetate. In this process, the prepared samples and their intermediates were characterized by infrared spectroscopy (IR) and X-ray diffraction(XRD), which showed that the modification of UiO66 was successful. UiO66-3Py-Lys and UiO66-4Py-Gly showed high catalytic activity in the supernatant determined by fluorescence spectrophotometer, and UiO66-4Py-Gly showed the best catalytic effects at the volume of 0.4mL benzaldehyde.


2012 ◽  
Vol 545 ◽  
pp. 275-278 ◽  
Author(s):  
Lili Widarti Zainuddin ◽  
Norlida Kamarulzaman

A ceramics sample of LiTaO3 was prepared using a sol-gel method. The sample is annealed at 750 °C for 48 hours. X-ray diffraction analysis indicate the formation of single phase, rhombohedral structure. An ac impedance study was used to analyse the conductivity of LiTaO3 at room temperature and at various temperatures.


2017 ◽  
Vol 31 (02) ◽  
pp. 1750006 ◽  
Author(s):  
Mohammad Hossein Ghorbani ◽  
Abdol Mahmood Davarpanah

Manganese oxides are of more interest to researchers because of their ability as catalysts and lithium batteries. In this research, MnO2nanowires with diameter about 45 nm were synthesized by sol–gel method at room temperature (RT). Effect of increasing the annealing temperature from 400[Formula: see text]C to 600[Formula: see text]C on crystalline structure of nanostructure were studied and average crystallite size was estimated about 22 nm. X-ray Diffraction (XRD) method, Energy-Dispersive X-ray Diffraction (EDXD), Scanning Electron Microscopy (SEM) and Vibrating Sample Magnetometer (VSM) were used to characterize the nanowires of MnO2.


Catalysts ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1344
Author(s):  
Tim Van Everbroeck ◽  
Radu-George Ciocarlan ◽  
Wouter Van Hoey ◽  
Myrjam Mertens ◽  
Pegie Cool

Mixed oxides were synthesized by co-precipitation of a Cu source in combination with Al, Fe or Mn corresponding salts as precursors. The materials were calcined at 600 and 1000 °C in order to crystallize the phases and to mimic the reaction conditions of the catalytic application. At 600 °C a mixed spinel structure was only formed for the combination of Cu and Mn, while at 1000 °C all the materials showed mixed spinel formation. The catalysts were applied in three-way catalysis using a reactor with a gas mixture containing CO, NO and O2. All the materials calcined at 600 °C displayed the remarkable ability to oxidize CO with O2 but also to reduce NO with CO, while the pure oxides such as CuO and MnO2 were not able to. The high catalytic activity at 600 °C was attributed to small supported CuO particles present and imperfections in the spinel structure. Calcination at 1000 °C crystallized the structure further which led to a dramatic loss in catalytic activity, although CuAl2O4 and CuFe2O4 still converted some NO. The materials were characterized by X-ray diffraction (XRD), Raman spectroscopy, H2-Temperatrue Programmed Reduction (H2-TPR), N2-sorption and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX).


2012 ◽  
Vol 66 (3) ◽  
Author(s):  
Khaled Haouemi ◽  
Fathi Touati ◽  
Néji Gharbi

AbstractTiO2 nanoparticles with different shapes and sizes were synthesised by the sol-gel route in Water/Brij78/Hexane reverse microemulsions. The aqueous cores of these microemulsions were used as nanoreactors to control sol-gel reactions. We studied the effect of water/surfactant mole ratio (W 0) on the morphology, and textural properties of the final products. The materials thus obtained were characterised by different techniques. Thermogravimetric and differential thermal analysis (TG-DTA) was used to study the thermal behaviour of the products and X-ray diffraction (XRD) to identify the crystalline phases. The morphological and textural properties of the products were determined by scattering electron microscopy (SEM) and the Brunauer-Emmett-Teller (BET) method, respectively. We also studied the influence of thermal treatment on the structure and size of the TiO2 particles. The effect of W 0 on the anatase-rutile phase transition temperature was investigated.


2016 ◽  
Vol 859 ◽  
pp. 18-23 ◽  
Author(s):  
Li Ping Zhao ◽  
Wen Hong Tao ◽  
Xing Hua Fu ◽  
Wen Zhe Cao ◽  
Guo Yuan Cheng ◽  
...  

(Ba0.5Sr0.5)1-xMnxTiO3(x=0,0.01,0.03,0.05)ceramics were prepared via a new sol-gel method with titannium oxide, strontium nitrate, barium nitrate and manganous nitrate as raw materials.The effect of Mn doping on the microstructure and dielectric properties of the BST were characterized by field scanning electron microscopy,x-ray diffraction and impedance analyser.It was found that the dopted ions could not alter the basic crystal strcuture and they only improved the material properties as modified ions when x≤0.3.The (Ba0.5Sr0.5)1-xMnxTiO3 ceramics sintered at 1250°C for 2h exhibited good dielectric properties(er=1330,tand=0.03)at room temperature and f=1KHz when x=0.03 and the grains were regular and uniform ,indicating a dense microstrcture.


2016 ◽  
Vol 5 (4) ◽  
pp. 196
Author(s):  
R. Palomino-Merino ◽  
R. Lozada-Morales ◽  
J. Martínez-Juárez ◽  
G. Juárez-Díaz ◽  
J. Carmona-Rodriguez ◽  
...  

Nanocrystalline Er-doped TiO2 was prepared by sol-gel at room temperature. X-ray diffraction, photoacoustic spectroscopy (optical absorption), transmission electron microscopy (TEM), and electron dispersion microscopy (EDS) were carried out on both as-prepared and thermally-annealed (air at 700 ºC) samples, revealing the anatase crystalline phase of TiO2. The samples exhibit an average grain size from 38 to 5.1 nm, as the nominal concentration of Er varies from 0 % to 7 %. The photoacoustic spectra evidence the absorption edge at 300 nm attributed to TiO2, as well as several electronic transitions which are atomic energy absorption-line levels characteristics of Er.


2007 ◽  
Vol 546-549 ◽  
pp. 2097-2102
Author(s):  
Ting Luo ◽  
Yi Zhang ◽  
Qing Rong Feng

The relationship of the resistivity versus synthesizing temperature of sol-gel YBa2Cu3O7-x samples, with Tc 91K, was studied while synthesizing in flowing oxygen atmosphere. A set of high temperature -T curves were obtained for the whole process. After four rounds of synthesizing, the resistivity of the sample was =1.00×10-3cm at room temperature. The -T curve of the last round also showed that the orthorhombic to tetragonal phase transformation of the sample occurred around 600oC that is lower than the YBa2Cu3O7-x sample prepared in ambient atmosphere. Other measurements such as X-ray diffraction, SEM measurement, low temperature R-T and M-T measurement were also taken to get more information of these samples.


2009 ◽  
Vol 1199 ◽  
Author(s):  
Danilo G Barrionuevo ◽  
Surinder P Singh ◽  
Maharaj S. Tomar

AbstractWe synthesized BiFe1-xMnxO3 (BFMO) for various compositions by sol gel process and thin films were deposited by spin coating on platinum Pt/Ti/SiO2/Si substrates. X-ray diffraction shows all the diffraction planes corresponding to rhombohedrally distorted perovskite BiFeO3 structure. The absence of any impurity phase in the films suggests the incorporation Mn ion preferentially to Fe site in the structure for low concentration. Magnetic measurements reveal the formation of ferromagnetic phase at room temperature with increased Mn substitution. On the other hand, ferroelectric polarization decreases with increasing Mn ion concentration. Raman studies suggest the dopant induced structural distortion.


2013 ◽  
Vol 734-737 ◽  
pp. 2328-2331
Author(s):  
Yu Fei You ◽  
C.H. Xu ◽  
Jing Zhe Wang ◽  
Jun Peng Wang

Sol-gel method is used for the formation of Pb0.499Sr0.499TiO3 (PST)thin films. The initial films were prepared with spin coating sol solution on silicon wafer and drying at room temperature and then heating coated dry sol film at 400°C for 10min. This process was repeated for 1-4 times to obtain 4 initial films with different thicknesses. The 4 initial films were annealed at 700°C for 2h to obtain PST ceramics films. The morphologies of the surface and cross-section of PST films were observed with a scanning electronic microscope (SEM). The phase structures of PST films were analyzed using X-ray diffraction meter (XRD). Experimental results show that PST film prepared by coating sol on silicon with different thicknesses can be high smooth,uniform and compact film.


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