scholarly journals Study of Chemical and Morphological Transformations during Ni2Mo3N Synthesis via an Oxide Precursor Nitration Route

Catalysts ◽  
2018 ◽  
Vol 8 (10) ◽  
pp. 436
Author(s):  
Denis Leybo ◽  
Dmitry Arkhipov ◽  
Konstantin Firestein ◽  
Denis Kuznetsov

Chemical and morphological transformations during Ni2Mo3N synthesis were studied in this work. Nitride samples were synthesized from oxide precursors in H2/N2 flow and were analyzed by thermogravimetry, X-ray diffraction analysis, scanning electron microscopy, and energy dispersive X-ray spectroscopy methods. In addition, physical and chemical adsorption properties were studied using low-temperature N2 physisorption and NH3 temperature-programmed desorption. It was shown that nitride formation proceeds through a sequence of phase transformations: NiMoO4 + MoO3 → Ni + NiMo + MoO2 → Ni + NiMo + Mo2N → Ni2Mo3N. The weight changes that were calculated from the proposed reactions were in agreement with the experimental data from thermogravimetry. The morphology of the powder changed from platelets and spheres for the oxide sample, to aggregates of needle-like particles for the intermediate product, to porous particles with an extended surface area for the nitride final product. The obtained results should prove useful for subsequent Ni2Mo3N based catalysts production process optimization.

Author(s):  
Zoya Moslempour ◽  
Sepehr Sadighi ◽  
Ali Dashti ◽  
Ali Ahmadpour

Abstract To study the affinity of 3A aluminosilicate adsorbents to prevent oligomerization of olefin molecules and forming green oil, physical and chemical properties of 3A molecular sieves are measured by using characterization techniques such as temperature-programmed desorption (TPD), nitrogen (N2) and water adsorptions, X-ray diffraction (XRD), X-ray fluorescence (XRF), crushing strength, and carbon dioxide (CO2) adsorption. Moreover, coke formation affinities of the understudy adsorbents are evaluated in a bench-scale system using 1-butene and 1,3-butadiene at temperatures of 220 and 260 °C, and outcomes are validated against the actual data gathered from an industrial scale olefin dehydration plant. Results confirm that the type of binder and the amount of ion exchange affect the performance of a 3A molecular sieve nominated for dehydrating olefinic streams. The binder with the least amount of acidity is preferred, and at least 35% of Na ions of the 4A zeolite should be exchanged with K ions to make it applicable for synthesizing an appropriate 3A molecular sieve. Furthermore, to control the oligomerization and inhibit green oil formation, the CO2 adsorption and acidity of Trisiv shape molecular sieves with the sizes of 1/4 inch should be less than 0.5 wt % and 1.7 mmol NH3/g, respectively. For extrudate shape with the sizes of 1/16 inch CO2 adsorption and acidity should be less than 0.2 wt % and 2.2 mmol NH3/g, respectively.


Materials ◽  
2020 ◽  
Vol 13 (3) ◽  
pp. 580
Author(s):  
Kai Zhang ◽  
Yuze Bai ◽  
Zhijun Gong ◽  
Zengwu Zhao ◽  
Baowei Li ◽  
...  

Acid leaching and alkali roasting were used to remove impurities such as Ca and Si in Baiyun Obo rare earth concentrate. The effects of acid–base treatment on the physical and chemical properties of the samples were analyzed by scanning electron microscopy, X-ray diffraction, Brunauer–Emmett–Teller characterization, X-ray photoelectron spectroscopy, H2-temperature-programmed reduction, NH3-temperature-programmed desorption (TPD), and NO-TPD. Results showed that the content of Ce7O12 in the rare earth concentrates increased and the dispersion was uniform. The grains became smaller, the specific surface area of rare earth concentrates increased, and the active sites were more exposed. Ce coexisted in the form of Ce3+ and Ce4+, whereas Fe coexisted in the form of Fe3+ and Fe2+. The content of Fe3+ was increased. The acid–base-treated rare earth concentrates had a denitration efficiency of 87.4% at a reaction temperature of 400 °C.


2005 ◽  
Vol 482 ◽  
pp. 251-254 ◽  
Author(s):  
Regina Mikulíková ◽  
Kateřina Kolářová ◽  
Lucie Bačáková ◽  
Václav Švorčík

Physical and chemical properties of polyethylene (PE) films doped with calcium salt of oxycellulose (Ca-oxy) and its interaction with cells in culture conditions were studied. The samples with various concentrations of Ca-oxy (0-20 %) were prepared. Samples were tested by goniometer measurements, X-ray diffraction, FTIR spectroscopy and SEM. Sample weight changes during boil sterilization and adhesion and proliferation of tissue cells (3T3 mouse fibroblasts) were studied. It was found that wetting angle of the doped films decreased with increasing Ca-oxy concentration to up to 10% and then increased again. Both film surfaces had different amount of crystalline phase, thereby different surface roughness. Due to a smaller surface roughness, cell growth was much better on the inner surface of the film than on the outer one. Cells adhered better to samples with 1% of Ca-oxy and with a higher content of oxycellulose over 7%. Cell proliferation was the best on samples with 1-5% Ca-oxy. Samples were polished to modify their surface roughness. Polishing increased cell proliferation especially on samples with a lower Ca-oxy concentration (1-5%).


2010 ◽  
Vol 64 (1) ◽  
Author(s):  
Yunfei Bi ◽  
Shuangqin Zeng ◽  
Dadong Li ◽  
Hong Nie

AbstractAmmonium dioxothiotungstate was synthesized using different tungsten sources and characterized in detail by powder X-ray diffraction, energy dispersive X-ray spectrometry, transmission electron microscopy, nitrogen adsorption, and temperature-programmed sulfidation. It was found that tungsten oxide nanobelts are superior to ammonium metatungstate as tungsten source for the synthesis of ammonium dioxothiotungstate due to a time-consuming aging step being excluded from the synthesis route. Moreover, detailed characteristic data reveal that, when tungsten oxide nanobelts are used, the physical and chemical properties of the resulting ammonium dioxothiotungstate including particles size, specific surface area, and sulfidation pattern were improved. Also, the hydrodesulfurization measurements showed higher catalytic activity and balanced selectivity of the resulting ammonium dioxothiotungstate.


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.


Author(s):  
Vahid Zabihi ◽  
Mohammad Hasan Eikani ◽  
Mehdi Ardjmand ◽  
Seyed Mahdi Latifi ◽  
Alireza Salehirad

Abstract One of the most significant aspects in selective catalytic reduction (SCR) of nitrogen oxides (NOx) is developing suitable catalysts by which the process occurs in a favorable way. At the present work SCR reaction by ammonia (NH3-SCR) was conducted using Co-Mn spinel and its composite with Fe-Mn spinel, as nanocatalysts. The nanocatalysts were fabricated through liquid routes and then their physicochemical properties such as phase composition, degree of agglomeration, particle size distribution, specific surface area and also surface acidic sites have been investigated by X-ray diffraction, Field Emission Scanning Electron Microscope, Energy-dispersive X-ray spectroscopy, energy dispersive spectroscopy mapping, Brunauer–Emmett–Teller, temperature-programmed reduction (H2-TPR) and temperature-programmed desorption of ammonia (NH3-TPD) analysis techniques. The catalytic activity tests in a temperature window of 150–400 °C and gas hourly space velocities of 10,000, 18,000 and 30,000 h−1 revealed that almost in all studied conditions, CoMn2O4/FeMn2O4 nanocomposite exhibited better performance in SCR reaction than CoMn2O4 spinel.


2019 ◽  
Vol 17 (1) ◽  
pp. 1459-1465
Author(s):  
Xuedong Feng ◽  
Jing Yi ◽  
Peng Luo

AbstractWith the purpose of studying the influence of NO/O2 on the NOx storage activity, a Pt-Ba-Ce/γ-Al2O3 catalyst was synthesized by an acid-aided sol-gel method. The physical and chemical properties of the catalyst were characterized by X-ray diffraction (XRD) and Transmission Electron Microscope (TEM) methods. The results showed that the composition of the catalyst was well-crystallized and the crystalline size of CeO2 (111) was about 5.7 nm. The mechanism of NO and NO2 storage and NOx temperature programmed desorption (NO-TPD) experiments were investigated to evaluate the NOx storage capacity of the catalyst. Pt-Ba-Ce/γ-Al2O3 catalyst presented the supreme NOx storage performance at 350℃, and the maximum value reached to 668.8 μmol / gcat. Compared with O2-free condition, NO oxidation to NO2 by O2 had a beneficial effect on the storage performance of NOx. NO-TPD test results showed that the NOx species stored on the catalyst surface still kept relatively stable even below 350℃.


1987 ◽  
Vol 113 ◽  
Author(s):  
Scott Schlorholtz ◽  
Ken Bergeson ◽  
Turgut Demirel

ABSTRACTThe physical and chemical properties of fly ash produced at Ottumwa Generating Station have been monitored since April, 1985. The fly ash is produced from burning a low sulfur, sub-bituminous coal obtained from the Powder River Basin near Gillette, Wyoming. One-hundred and sixty samples of fly ash were obtained during the two year period. All of the samples were subjected to physical testing as specified by ASTM C 311. About one-hundred of the samples were also subjected to a series of tests designed to monitor the self-cementing properties of the fly ash. Many of the fly ash samples were subjected to x-ray diffraction and fluorescence analysis to define the mineralogical and chemical composition of the bulk fly ash as a function of sampling date. Hydration products in selected hardened fly ash pastes, were studied by x-ray diffraction and scanning electron microscopy. The studies indicated that power plant operating conditions influenced the compressive strength of the fly ash paste specimens. Mineralogical and morphological studies of the fly ash pastes indicated that stratlingite formation occurred in the highstrength specimens, while ettringite was the major hydration product evident in the low-strength specimens.


2003 ◽  
Vol 807 ◽  
Author(s):  
T. Advocat ◽  
F. Jorion ◽  
T. Marcillat ◽  
G. Leturcq ◽  
X. Deschanels ◽  
...  

ABSTRACTZirconolite is a potential inorganic matrix that is currently investigated in France, in the framework of the 1991 radioactive waste management law, with a view to provide durable containment of the trivalent and tetravalent minor actinides like neptunium, curium, americium and small quantities of unrecyclable plutonium separated from other nuclear waste. To confirm the actinide loading capacity of the zirconolite calcium site and to study the physical and chemical stability of this type of ceramic when subjected to alpha self-irradiation, zirconolite ceramic pellets were fabricated with 10 wt% plutonium oxide (isotope 239 or 238). The 55 pellets are dense (> 93.3% of the theoretical density on average) and free of cracks. They are characterized by a grain size of between 10 and 20 micrometers. X-ray diffraction analyses confirmed the presence of the zirconolite 2M crystalline structure.


2017 ◽  
Vol 42 (1) ◽  
pp. 23-29
Author(s):  
Hua Song ◽  
Shengnan Li ◽  
Hualin Song ◽  
Feng Li ◽  
Huapeng Cui

A number of Zn–S2O82–/ZrO2–Al2O3 (Zn( x)–SZA) catalysts with different Zn mass fractions were synthesised and characterised by using X-ray diffraction, the Brunauer–Emmett–Teller method, and H2 temperature-programmed reduction. The structure and isomerisation performance of Zn( x)–SZA catalysts were studied using n-pentane as a probe reaction. The results showed that a pure tetragonal ZrO2 phase was formed on Zn( x)–SZA, and the ZrO2 crystallite sizes of the tetragonal phase increased in the order: Zn(0.5)–SZA < Zn(1.0)–SZA < Zn(1.5)–SZA < Zn(2.0)–SZA < SZA. Zn can strengthen the interaction between persulfate ions and the support, promote the formation of stronger acidity, lead to a better dispersion of sulfate ions on the surface, and improve the redox performance of the catalysts. The Zn(1.0)–SZA catalyst exhibited the best catalytic activity for n-pentane isomerisation. At a temperature of 170 °C, a reaction pressure of 2.0 MPa, a molar H2/ n-pentane ratio of 4:1, and a weight hourly space velocity of 1.0 h−1, the isopentane yield reached 58.0%.


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