scholarly journals 2D Polymeric Network of Cu/Na, A Route for the Preparation Truncated Octahedral Catalyst Applicable in the WGS Reaction

Author(s):  
Zohreh Razmara

Abstract A 2D heterometallic copper(II)–sodium(I) complex based on pyridine 2,6-dicarboxylato (dipic2-) formulated as [Cu(μ-dipic)2{Na2(µ-H2O)4}]n. 2nH2O (1) has been synthesized. Thermal stability of complex 1 was studied by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA). Single-crystal X-ray diffraction (SC-XRD) analysis showed that the parallelepiped colorless crystal of complex 1 crystallizes in a monoclinic system with the space group P2/c . A highly dispersed truncated octahedral catalyst formulated as Cu-Na/Al2O3 (CNM) was prepared by thermal decomposition of complex 1. Besides, the reference catalyst of Cu-Na/Al2O3 (CNR) was prepared by impregnation conventional method. The catalysts were examined by FT-IR, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer–Emmett–Teller (BET) surface area, and subjected to water-gas shift (WGS) reaction in the temperature range of 150-400 °C. The catalysts showed strong surface structure-activity dependence in WGS reaction. Improved catalytic performance during the water-gas shift reaction was observed for CNM compared to CNR due to its high dispersion, smaller particle size, and higher BET specific surface area.

2020 ◽  
Vol 58 (7) ◽  
pp. 495-500
Author(s):  
Young Min Jin ◽  
Joon Hyuk Lee ◽  
Sang Sun Choi

This study examined the effect of alkalis on lyocell-based activated carbon fibres (ACFs) with high Brunauer-Emmett-Teller (BET) surface areas, using X-ray diffraction (XRD). Here, alkali treatments were conducted using 10 ~ 25 % NaOH and KOH on lyocell samples for 3 h at ambient room temperature. A secondary treatment with 4 % each of KOH and H3PO4 for an additional 3 h followed. An activated form of the samples was prepared by oxidation (stabilisation), carbonisation, and activation. The final ACF form of the samples showed a porous structure with high BET surface areas (> 1,000 m<sup>2</sup> g<sup>-1</sup>). A 25 % dosage of NaOH produced the highest BET surface area compared to other samples. In terms of crystallinity, a 15 % dosage of KOH was found to be the optimum dosage to secure the highest degree of crystallinity among all samples. Meanwhile, the NaOH was successfully shifted the samples into the most distinct form of cellulose II. 15 % NaOH was found to secure the most stable thermal characteristics, as determined via thermo-gravimetric analysis. The present work demonstrates the various physio-chemistries of ACFs prepared with different proportions and types of alkalis, leading to intriguing potential applications.


Processes ◽  
2021 ◽  
Vol 9 (7) ◽  
pp. 1238
Author(s):  
Garven M. Huntley ◽  
Rudy L. Luck ◽  
Michael E. Mullins ◽  
Nick K. Newberry

Four naturally occurring zeolites were examined to verify their assignments as chabazites AZLB-Ca and AZLB-Na (Bowie, Arizona) and clinoptilolites NM-Ca (Winston, New Mexico) and NV-Na (Ash Meadows, Nevada). Based on powder X-ray diffraction, NM-Ca was discovered to be mostly quartz with some clinoptilolite residues. Treatment with concentrated HCl (12.1 M) acid resulted in AZLB-Ca and AZLB-Na, the chabazite-like species, becoming amorphous, as confirmed by powder X-ray diffraction. In contrast, NM-Ca and NV-Na, which are clinoptilolite-like species, withstood boiling in concentrated HCl acid. This treatment removes calcium, magnesium, sodium, potassium, aluminum, and iron atoms or ions from the framework while leaving the silicon framework intact as confirmed via X-ray fluorescence and diffraction. SEM images on calcined and HCl treated NV-Na were obtained. BET surface area analysis confirmed an increase in surface area for the two zeolites after treatment, NM-Ca 20.0(1) to 111(4) m2/g and NV-Na 19.0(4) to 158(7) m2/g. 29Si and 27Al MAS NMR were performed on the natural and treated NV-Na zeolite, and the data for the natural NV-Na zeolite suggested a Si:Al ratio of 4.33 similar to that determined by X-Ray fluorescence of 4.55. Removal of lead ions from solution decreased from the native NM-Ca, 0.27(14), NV-Na, 1.50(17) meq/g compared to the modified zeolites, 30 min HCl treated NM-Ca 0.06(9) and NV-Na, 0.41(23) meq/g, and also decreased upon K+ ion pretreatment in the HCl modified zeolites.


BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Arefeh Dehghani Tafti ◽  
Bi Bi Fatemeh Mirjalili ◽  
Abdolhamid Bamoniri ◽  
Naeimeh Salehi

AbstractNano-eggshell/Ti(IV) as a novel naturally based catalyst was prepared, characterized and applied for the synthesis of dihydropyrano[2,3-c]pyrazole derivatives. The characterization of nano-eggshell/Ti(IV) was performed using Fourier Transform Infrared spectroscopy, X-ray Diffraction, Field Emission Scanning Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and Thermo Gravimetric Analysis. Dihydropyrano[2,3-c]pyrazoles were synthesized in the presence of nano-eggshell/Ti(IV) via a four component reaction of aldehydes, ethyl acetoacetate, malononitrile and hydrazine hydrate at room temperature under solvent free conditions. The principal affairs of this procedure are mild condition, short reaction times, easy work-up, high yields, reusability of the catalyst and the absence of toxic organic solvents.


Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1712
Author(s):  
Appusamy Muthukrishnaraj ◽  
Salma Ahmed Al-Zahrani ◽  
Ahmed Al Otaibi ◽  
Semmedu Selvaraj Kalaivani ◽  
Ayyar Manikandan ◽  
...  

Towards the utilization of Cu2O nanomaterial for the degradation of industrial dye pollutants such as methylene blue and methyl orange, the graphene-incorporated Cu2O nanocomposites (GCC) were developed via a precipitation method. Using Hummers method, the grapheme oxide (GO) was initially synthesized. The varying weight percentages (1–4 wt %) of GO was incorporated along with the precipitation of Cu2O catalyst. Various characterization techniques such as Fourier-transform infra-red (FT-IR), X-ray diffraction (XRD), UV–visible diffused reflectance (UV-DRS), Raman spectroscopy, thermo gravimetric analysis (TGA), energy-dispersive X-ray analysis (EDX), and electro chemical impedance (EIS) were followed for characterization. The cabbage-like morphology of the developed Cu2O and its composites were ascertained from field-emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HR-TEM). In addition, the growth mechanism was also proposed. The results infer that 2 wt % GO-incorporated Cu2O composites shows the highest value of degradation efficiency (97.9% and 96.1%) for MB and MO at 160 and 220 min, respectively. Further, its catalytic performance over visible region (red shift) was also enhanced to an appreciable extent, when compared with that of other samples.


2017 ◽  
Vol 50 ◽  
pp. 18-31 ◽  
Author(s):  
Rudzani Sigwadi ◽  
Simon Dhlamini ◽  
Touhami Mokrani ◽  
Patrick Nonjola

The paper presents the synthesis and investigation of zirconium oxide (ZrO2) nanoparticles that were synthesised by precipitation method with the effects of the temperatures of reaction on the particles size, morphology, crystallite sizes and stability at high temperature. The reaction temperature effect on the particle size, morphology, crystallite sizes and stabilized a higher temperature (tetragonal and cubic) phases was studied. Thermal decomposition, band structure and functional groups were analyzed by Brunauer-Emmett-Teller (BET), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA) and Fourier transform infrared (FT-IR). The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR spectra showed the strong presence of ZrO2 nanoparticles.


2021 ◽  
Vol 11 (1) ◽  
pp. 84-106
Author(s):  
Nada Sadoon Ahmed zeki ◽  
Sattar Jalil Hussein ◽  
Khalifa K. Aoyed ◽  
Saad Kareem Ibrahim ◽  
Ibtissam K. Mehawee

This work deals with the hydrodesulfurization of three types of naphtha feedstocks; mixednaphtha (WN), heavy naphtha (HN) & light naphtha (LN) with a sulfur content of 1642.1,1334.9 & 709 ppm respectively, obtained from Missan refinery using prepared Co-Mo/γ-Al2O3catalyst. The Iraqi white kaolin was used as a starting material for the preparation of γ-Al2O3support, transferring kaolin to meta-kaolin was studied through calcination at differenttemperatures and durations, kaolin structure was investigated using X-Ray diffractiontechniques.High purity 94.83%. Crystalline γ-Al2O3 with a surface area of 129.91 m2/gm, pore volume0.9002 cm3/g was synthesized by extraction of Iraqi kaolin with H2SO4 at different acid to clayweight ratios, acid concentrations & leaching time. Ethanol was used as precipitating agent; theresultant gel was dried and calcined at 70OC, 10 hrs & 900 OC, 2 hrs respectively.The effects of different parameters on the average crystallinity and extraction % ofsynthesized γ-Al2O3 were studied like; acid: clay ratio, sulfuric acid concentration, leachingtime, leaching temperature & kaolin conversion to metakaolin. Characterization of prepared γ-Al2O3 & Co-Mo catalyst were achieved by X-ray diffraction, FTIR-spectra, texture properties& BET surface area, BJH N2 adsorption porosity, AFM, SEM, crush strength & XRF tests. Co-Mo/ γ-Al2O3 catalyst with final loading 5.702 wt% and 21.45 wt% of Co and Mo oxidesrespectively was prepared by impregnation methods.The activity of prepared Co-Mo/γ-Al2O3 catalyst after moulding to be tested forhydrodesulfurization (HDS) of naphtha feedstock W.N, H.N & L.N was performed using apilot hydrotreating unit at petroleum research & development centre, at different operatingconditions. Effects of temperature, LHSV, pressure, time & pore size distribution were studied,the best percentage of sulfur removal is increased with decreasing LHSV to 2 hr-1 as a generaltrend to be 89.71, 99.72, 99.20 % at 310oC for the whole naphtha, heavy naphtha and lightnaphtha feedstocks respectively, at 34 bar pressure and 200/200 cm3/cm3 H2/HC ratio.


2016 ◽  
Vol 30 (32n33) ◽  
pp. 1650347
Author(s):  
Amarjeet ◽  
Vinod Kumar

[Formula: see text] ([Formula: see text] = 0.1, 0.3 and 0.5) nanoparticles were prepared by chemical co-precipitation method. The developed nanoparticles were characterized for structural properties by powder X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) techniques. Peak position in the X-ray diffraction pattern confirmed the single spinel phase of the developed particles. Infrared (IR) spectroscopy in mid-IR range showed the presence of characteristic absorption bands corresponding to octahedral and tetrahedral bonds in the spinel structure of prepared samples. Thermo-gravimetric analysis (TGA) measurements showed a considerable weight loss in the developed samples above 700[Formula: see text]C. Frequency dependence of the electrical properties of the developed material pellets was studied in the frequency range of 1 kHz–5 MHz. Temperature dependence of the dielectric constant of [Formula: see text] was studied at different temperatures, i.e. at 425, 450 and 475 K, in the frequency range of 1 kHz–5 MHz. It was found that the electrical conductivity decreases with increasing Cu[Formula: see text] ion content while it increases with the increase in temperature.


Author(s):  
Nitu Bhatnagar ◽  
Avani Pareek

The present study is aimed to observe the difference in the Physico-Chemical characteristics of the marketed and formulated bhasma samples through X-Ray Diffraction analysis (XRD), Dynamic Light Scattering (DLS), Zeta potential, Thermo-Gravimetric analysis (TGA), Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray analysis (EDAX), apart from organoleptic methods. Inductively Coupled Plasma Mass Spectroscopy (ICPMS) analysis was also done to observe the presence of trace and heavy metals so that the safety of all these samples could be ensured. XRD shows variation in oxide nature of zinc as well crystallite size in all bhasma samples. DLS and SEM results show difference in particle size of marketed bhasma samples as compared to formulated Yashada bhasma. EDAX and ICPMS also confirm the alteration in elemental composition of all these bhasma samples. Thus, it can be concluded that these ayurvedic medicines should be prepared strictly using the formulation methods as mentioned in the Ayurvedic texts. This will help the prepared products to adopt the inherent quality of the ancient system of medicine, which shall be useful and devoid of any side effects for human consumption.


2001 ◽  
Vol 73 (4) ◽  
pp. 525-532 ◽  
Author(s):  
MELLATIE R. FINISIE ◽  
ATCHE JOSUÉ ◽  
VALFREDO T. FÁVERE ◽  
MAURO C. M. LARANJEIRA

Bioceramic composites were obtained from chitosan and hydroxyapatite pastes synthesized at physiological temperature according to two different syntheses approaches. Usual analytical techniques (X-ray diffraction analysis, Fourier transformed infrared spectroscopy, Thermo gravimetric analysis, Scanning electron microscopy, X-ray dispersive energy analysis and Porosimetry) were employed to characterize the resulting material. The aim of this investigation was to study the bioceramic properties of the pastes with non-decaying behavior from chitosan-hydroxyapatite composites. Chitosan, which also forms a water-insoluble gel in the presence of calcium ions, and has been reported to have pharmacologically beneficial effects on osteoconductivity, was added to the solid phase of the hydroxyapatite powder. The properties exhibited by the chitosan-hydroxyapatite composites were characteristic of bioceramics applied as bone substitutes. Hydroxyapatite contents ranging from 85 to 98% (w/w) resulted in suitable bioceramic composites for bone regeneration, since they showed a non-decaying behavior, good mechanical properties and suitable pore sizes.


2015 ◽  
Vol 1112 ◽  
pp. 489-492
Author(s):  
Ali Mufid ◽  
M. Zainuri

This research aims to form particles of hematite (α-Fe2O3) with a basis of mineral iron ore Fe3O4 from Tanah Laut. Magnetite Fe3O4 was synthesized using co-precipitation method. Further characterization using X-ray fluorescence (XRF) to obtain the percentage of the elements, obtained an iron content of 98.51%. Then characterized using thermo-gravimetric analysis and differential scanning calorimetry (TGA-DSC) to determine the calcination temperature, that at a temperature of 445 °C mass decreased by 0.369% due to increase in temperature. Further Characterization of X-ray diffraction (XRD) to determine the phases formed at the calcination temperature variation of 400 °C, 445 °C, 500 °C and 600 °C with a holding time of 5 hours to form a single phase α-Fe2O3 hematite. Testing with a particle size analyzer (PSA) to determine the particle size distribution, where test results indicate that the α-Fe2O3 phase of each having a particle size of 269.7 nm, 332.2 nm, 357.9 nm, 412.2 nm. The best quantity is shown at a temperature of 500 °C to form the hematite phase. This result is used as the calcination procedure to obtain a source of Fe ions in the manufacture of Lithium Ferro Phosphate.


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