Reaktive E=C(p-p)π-Systeme, XLIII [1] Darstellung und Charakterisierung P-Phosphino- oder P-Arsino-substituierter Fluorphosphaalkene des Typs R2E-P=C(F)NEt2 (R = Me, CF3, Me2N; E = P, As) / Reactive E=C(p-p)-π Systems XLIII [1] Synthesis and Characterization of P-Phosphino or P-Arsino Substituted Fluorophosphaalkenes of the Type R2E-P=C(F)NEt2 (R= Me, CF3, Me2N; E = P As)

1996 ◽  
Vol 51 (6) ◽  
pp. 778-784 ◽  
Author(s):  
Joseph Grobe ◽  
Duc Le Van ◽  
Jost Winnemöller ◽  
Bernt Krebs ◽  
Mechtild Läge
Keyword(s):  
Lone Pair ◽  
Molar Ratio ◽  
Analogous Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nitrogen Lone Pair ◽  
Type Interaction ◽  
The Stability ◽  
High Yields

Abstract The easily accessible phosphaalkene HP=C(F)NEt2 (lb) reacts with halophosphanes or -arsanes R2EX (X = Cl, I) in the presence of NEt3 to give P-phosphino- or -P-arsino substituted fluorophosphaalkenes of the type RiE-P=C(F)NEti (2 - 6) in high yields (60 - 85 %) [R2E: (CF3)2P (2), Me2N(CF3)P (3), Me2P (4), (CF3)2As (5), Me2As (6)]. The analogous reaction of ib with CF3PI2 (molar ratio 1:2) unexpectedly leads to the triphosphetene Et2N - C=P-PCF3-PCF3 (7). The stability of compounds 2 - 6 as a function of R2E decreases from As to P and from CF3 to Me, respectively. Compounds 2 - 6 generally show the Z-configuration and have been characterized by thorough spectroscopic investigations (MS,IR; 1H, 19F, 11C, 31PNMR). A single crystal X-ray diffraction study of 2 proves the π-type interaction of the nitrogen lone pair with the P=C bond thus enhancing the stability of the system and the PP bond order

scholarly journals Rapid four-component synthesis of dihydropyrano[2,3-c]pyrazoles using nano-eggshell/Ti(IV) as a highly compatible natural based catalyst

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Arefeh Dehghani Tafti ◽  
Bi Bi Fatemeh Mirjalili ◽  
Abdolhamid Bamoniri ◽  
Naeimeh Salehi
Keyword(s):  
Thermo Gravimetric Analysis ◽  
Reaction Times ◽  
Diffraction Field ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solvent Free Conditions ◽  
High Yields ◽  
Work Up

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.

Stability of sodalite relative to nepheline in NaCl–H2O brines at 750 °C: Implications for hydrothermal formation of sodalite

2020 ◽  
Vol 58 (1) ◽  
pp. 3-18 ◽  
Author(s):  
Jonathan B. Schneider ◽  
David M. Jenkins
Keyword(s):  
Infrared Spectroscopy ◽  
Constant Temperature ◽  
Molar Ratio ◽  
Standard State ◽  
X Ray Diffraction ◽  
Cage Structure ◽  
X Ray ◽  
Brine Concentration

ABSTRACT Formation of the feldspathoid sodalite (Na6Al6Si6O24·2NaCl) by reaction of nepheline (NaAlSiO4) with NaCl-bearing brines was investigated at 3 and 6 kbar and at a constant temperature of 750 °C to determine the brine concentration at which sodalite forms with variation in pressure. The reaction boundary was located by reaction-reversal experiments in the system NaAlSiO4–NaCl–H2O at a brine concentration of 0.16 ± 0.08 XNaCl [= molar ratio NaCl/(NaCl + H2O)] at 3 kbar and at a brine concentration of 0.35 ± 0.03 XNaCl at 6 kbar. Characterization of the sodalite using both X-ray diffraction and infrared spectroscopy after treatment in these brines indicated no obvious evidence of water or hydroxyl incorporation into the cage structure of sodalite. The data from this study were combined with earlier results by Wellman (1970) and Sharp et al. (1989) at lower (1–1.5 kbar) and higher (7–8 kbar) pressures, respectively, on sodalite formation from nepheline and NaCl which models as a concave-down curve in XNaCl – P space. In general, sodalite buffers the concentration of neutral aqueous NaCl° in the brine to relatively low values at P < 4 kbar, but NaCl° increases rapidly at higher pressures. Thermochemical modeling of these data was done to determine the activity of the aqueous NaCl° relative to a 1 molal (m) standard state, demonstrating very low activities (<0.2 m, or 1.2 wt.%) of NaCl° at 3 kbar and lower, but rising to relatively high activities (>20 m, or 54 wt.%) of NaCl° at 6 kbar or higher. The results from this study place constraints on the concentration of NaCl° in brines coexisting with nepheline and sodalite and, because of the relative insensitivity of this reaction to temperature, can provide a convenient geobarometer for those localities where the fluid compositions that formed nepheline and sodalite can be determined independently.

Bioceramic Production from Giant Purple Barnacle (Megabalanus tintinnabulum)

2014 ◽  
Vol 631 ◽  
pp. 137-142 ◽  
Author(s):  
F.N. Oktar ◽  
H. Gokce ◽  
O. Gunduz ◽  
Y.M. Sahin ◽  
D. Agaogullari ◽  
...  
Keyword(s):  
Chemical Properties ◽  
Complete Characterization ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Hot Plate ◽  
X Ray ◽  
Fine Powders ◽  
Simple Economic ◽  
And Chemical Properties

In this study the structural and chemical properties of barnacle shell based bioceramic materials (i.e. hydroxyapatite, whitlockite, monetite and other phases) were produced by using mechano-chemical (hot-plate) conversion method. Cleaned barnacle shells were ball milled down to <75µm in diameter. Differential thermal and gravimetric analyses (DTA/TGA) were performed to determine the exact CaCO3 content. Sample batches of 2g were prepared from the fine powders produced. For each batch, the required volume of an aqueous H3PO4 solution was calculated in order to set the stoichiometric molar ratio of Ca/P equal to 1.5 for ß-tricalcium phosphate (ß-TCP) or to 1.667 for hydroxyapatite (HA). The temperature was set to 80°C for 15 minutes to complete the process. After the titration of the equivalent amount of H3PO4 into the prepared solution, agitation was carried out on a hot-plate (i.e. mechano-chemical processing) for 8 hours. The sediments formed were dried and the resulting TCP and HA powders were calcined at 400°C and 800°C respectively. For complete characterization of the bioceramics produced, scanning electron microscopy (SEM), fourier transform infrared spectroscopy (FTIR) and x-ray diffraction (XRD) analyses were carried out. The current study proposes a simple, economic and time efficient method for nano-bioceramic production.

scholarly journals Synthesis and Characterization of New Diiron and Diruthenium μ-Aminocarbyne Complexes Containing Terminal S-, P- and C-Ligands

2007 ◽  
Vol 62 (3) ◽  
pp. 427-438 ◽  
Author(s):  
Vincenzo G. Albano ◽  
Luigi Busetto ◽  
Fabio Marchetti ◽  
Magda Monari ◽  
Stefano Zacchini ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Coordination Mode ◽  
Bond Cleavage ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dithiocarbamate Ligand ◽  
High Yields

The diiron aminocarbyne complexes [Fe2{μ-CN(Me)(R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (R = Xy1, 1a; R = Me, 1b; R = CH2Ph, 1c; Xy1 = 2,6-Me2C6H3) undergo replacement of the coordinated nitrile by halides, diethyldithiocarbamate, and dicyanomethanide to give [Fe2{μ-CN(Me) (R)}(μ-CO)(CO)(X)(Cp)2] complexes (R = Me, X = Br, 4a; R = Me, X = I, 4b; R = CH2Ph, X = Cl, 4c; R = CH2Ph, X = Br, 4d; R = CH2Ph, X = I, 4e; R = Xy1, X = SC(S)NEt2, 5a; R = Me, X = SC(S)NEt2, 5b; R = Xy1, X = CH(CN)2, 7), in good yields. The molecular structure of 5a shows an unusual η1 coordination mode of the dithiocarbamate ligand. Similarly, treatment of [M2{μ-CN(Me) (R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (M = Fe, R = Xy1, 1a; M = Fe, R = Me, 1b; M = Ru, R = Xy1, 2a; M = Ru, R = Me, 2b) with a series of phosphanes generates the cationic complexes [M2{μ- CN(Me)(R)}(μ-CO)(CO)(P)(Cp)2][SO3CF3] (M = Fe, R = Xy1, P = PPh2H, 6a; M = Fe, R = Xy1, P = PPh3, 6b; M = Fe, R = Xy1, P = PMe3, 6c; M = Fe, R = Me, P = PMe2Ph, 6d; M = Fe, R = Me, P = PPh3, 6e; M = Fe, R = Me, P = PMePh2, 6f; M = Ru, R = Xy1, P = PPh2H, 6g; M = Ru, R = Me, P = PPh2H, 6h), in high yields. The molecular structure of 6a has been elucidated by an X-ray diffraction study. The reactions of [Fe2{μ-CN(Me)(Xyl)}(μ-CO)(CO)(NCR′)(Cp)2][SO3CF3] [R′ = Me, 1a; R′ = tBu, 3] with PhLi and PPh2Li yield [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(Ph)(Cp)2] (8) and [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(PPh2)(Cp)2] (9), respectively. The molecular structure of 8 has been ascertained by X-ray diffraction. Conversely, the reaction of 1a with MeLi generates the aminoalkylidene compound [Fe2{C(Me)N(Me)(Xy1)}(μ-CO)2(CO)(Cp)2] (10).Finally, the acetone complex [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(OCMe2)(Cp)2][SO3CF3] (12) reacts with lithium acetylides to give complexes [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(C≡CR)(Cp)2] (R = p-C6H4Me, 11a; R = Ph, 11b; R = SiMe3, 11c), in high yields. Filtration through alumina of a solution of 11a in CH2Cl2 results in hydration of the acetylide group and C-Si bond cleavage, affording [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO){C(O)Me}(Cp)2] (12).

Synthesis and characterization of the pentazolate anion cyclo-N5ˉ in (N5)6(H3O)3(NH4)4Cl

Science ◽  
2017 ◽  
Vol 355 (6323) ◽  
pp. 374-376 ◽  
Author(s):  
Chong Zhang ◽  
Chengguo Sun ◽  
Bingcheng Hu ◽  
Chuanming Yu ◽  
Ming Lu
Keyword(s):  
Thermal Analysis ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Decomposition Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Onset Decomposition Temperature ◽  
The Stability

Pentazole (HN5), an unstable molecular ring comprising five nitrogen atoms, has been of great interest to researchers for the better part of a century. We report the synthesis and characterization of the pentazolate anion stabilized in a (N5)6(H3O)3(NH4)4Cl salt. The anion was generated by direct cleavage of the C–N bond in a multisubstituted arylpentazole using m-chloroperbenzoic acid and ferrous bisglycinate. The structure was confirmed by single-crystal x-ray diffraction analysis, which highlighted stabilization of the cyclo-N5ˉ ring by chloride, ammonium, and hydronium. Thermal analysis indicated the stability of the salt below 117°C on the basis of thermogravimetry-measured onset decomposition temperature.

The Study and Characterization of a Novel Structure of 1,3,5-Benzenetricarboxylic Acid

2013 ◽  
Vol 830 ◽  
pp. 202-206
Author(s):  
Hai Yan Tan ◽  
Cheng Liu ◽  
Jin Ping Wu
Keyword(s):  
Relevant Information ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
X Ray ◽  
Novel Structure ◽  
Ft Ir ◽  
Benzenetricarboxylic Acid ◽  
The Stability ◽  
Lamella Structure

A novel ten-interpenetrating structure of 1,3,5-benzenetricarboxylic acid was grown under solvothemal condition after heated it 16 hours. It was characterized by FT-IR, HNMR, X-ray diffraction, HRTEM. HRTEM obtain the relevant information of structural morphologies. The result of HRTEM showsed this material owned special lamella structure. X-ray diffraction showed the crystal of the new structure is of monoclinic system, space groupP1 with a=26.5039(17), b=16.4121(17),c=26.550(2)Å,α=90.00, β=91.533(2), γ=90.00, V=11544.4(17)Å3, Z=8, Dc=1.451g/cm3,μ=0.126mm-1,F(000)=5184, R=0.0891 and w (R)=0.1819 for 11318 observed reflection with I>2(I),hydrogen bond contributed to the stability of the structure. The fluorescence spectra indicated that the title compound had two stronger emission peak at 346nm and 400nm. Keywords:1, 3, 5-benzenetricarboxylic acid; novel structure; ten-interpenetrating

scholarly journals Synthesis and Characterization of Hydroxyapatite from Duck Eggshell by Wet Precipitation Process

2021 ◽  
Vol 3 (1) ◽  
pp. 8-11
Author(s):  
Yelmida Azis ◽  
Cory Dian Alfarisi ◽  
Komalasari Komalasari ◽  
Khairat Khairat ◽  
Yusnimar Sahan
Keyword(s):  
Xrd Analysis ◽  
Precipitation Method ◽  
Molar Ratio ◽  
Precipitation Process ◽  
Stable Form ◽  
X Ray Diffraction ◽  
Precipitated Calcium Carbonate ◽  
X Ray ◽  
Inorganic Mineral

Hydroxyapatite (HAp, Ca10(PO4)6(OH)2) is the most stable form of calcium phosphate and widely used in various medical applications, mainly in orthopedics and dentistry due to its close similarities with the inorganic mineral component of bone and teeth. This study aims to synthesize hydroxyapatite from duck eggshell using the precipitation method. The duck eggshell was calcined, hydrated (slaking) and underwent carbonation to form Precipitated Calcium Carbonate (PCC).  Afterwards, (NH4)2HPO4 was added to produce HAp by varying the molar ratio of Ca/P by 1.67, 1.77 and 1.87 and stirring speed by 200, 250, 300rpm under basic condition (pH 10 – 11). The best results were obtained at a molar ratio of 1.77 with 200rpm stirring speed. Furthermore, the X-ray Diffraction (XRD) analysis showed that its crystals were hexagonal with sizes of 23.062nm, in the absence of other crystalline phases. Therefore, the hydroxyapatite was obtained in the agglomerates form with a specific surface area of ??55.929m2/g.

scholarly journals Synthesis and Characterization of Zeolite X from Boiler Ash and Aluminum Foil Waste

2021 ◽  
Vol 4 (1) ◽  
pp. 15
Author(s):  
Intan Ayu Safitri ◽  
Iis Siti Jahro
Keyword(s):  
Aluminum Foil ◽  
Degree Of Crystallinity ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Zeolite X ◽  
X Ray ◽  
X Zeolite ◽  
Ft Ir ◽  
Boiler Ash

This study aims to determine the effect of the Si/Al molar ratio and the number of Na2EDTA additions on the purity and crystallinity levels of the synthesized zeolite X. zeolite X was synthesized by hydrothermal method at 70°C and 120°C for 3 and 6 hours, respectively. In the synthesis of zeolite X used boiler ash and aluminum foil waste. The results of characterization using Fourier Transform Infra Red (FT-IR) and X-Ray Diffraction (XRD) showed that the level of purity and crystallinity of the synthesized zeolite X was influenced by the variation of Si/Al molar rasio and amount of Na2EDTA addition. The zeolite with the best quality was obtained from the synthesis with a Si/Al molar ratio of 1.6 and the amount of Na2EDTA added as much as 3.0 g. The synthesized zeolite X has a purity level of 75% and a degree of crystallinity with a total intensity of 845.

Synthesis and Characterization of Polyaniline Nanotubes Doped with Amino Acetic Acid

2012 ◽  
Vol 184-185 ◽  
pp. 1285-1288 ◽  
Author(s):  
Xue Lian Bai ◽  
Jian Ting Mei ◽  
Yun Bai ◽  
Zhong Guo Mu
Keyword(s):  
Acetic Acid ◽  
Self Assembly ◽  
Ammonium Persulfate ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure And Property ◽  
Assembly Method ◽  
Doped Polyaniline

Doped polyaniline (PANI) nanostructure has been prepared at room temperature using amino acetic acid (AA) as dopant and ammonium persulfate (APS) as oxidant by a self-assembly method. The structure and property of polyaniline nanostructure were characterized by SEM, TEM，IR and X-ray diffraction (XRD) and applying the 4 probes method. The results showed the production was PANI. The effect of molar ratio of AA to An affected the morphology of the product and room template conductivity of the products were studied.

Synthesis and Characterization of Phosphoric Silica Catalyst from Bamboo Leaves for Production of Triacetin

2022 ◽  
Vol 54 ◽  
pp. 129-137
Author(s):  
Renita Manurung ◽  
Muhammad Dedi Anggreawan ◽  
Alwi Gery Agustan Siregar
Keyword(s):  
High Performance ◽  
Catalytic Amount ◽  
Raw Material ◽  
Molar Ratio ◽  
Solid Catalyst ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bamboo Leaves ◽  
Bamboo Leaf Ash

In this research, the bamboo leaf shows promise as an alternative raw material for silica production. This study investigated the performance of heterogeneous catalyst prepared from silica derived bamboo leaf ash after that impregnated with phosphoric acid at ratio various. The catalyst was characterized by X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscope Energy Dispersive X-Ray Spectroscopy (SEM-EDS), Brunauer Emmet Teller (BET) and Barrett, Joyner and Halenda (BJH) method and triacetin product analyzed by GC-MS. The optimum condition phosphoric silica catalyst was obtained at phosphoric silica molar ratio of 1:2 and employed in the acetylation of glycerol, respectively. As result, 24 % selectivity for triacetin was obtained in the presence of catalytic amount 5%, molar ratio 1:9 at 100 °C for 4 hours. Bamboo leaf derived phosphoric silica calcined showed high potential to be used as an easy to prepare and high-performance solid catalyst for industrial scale.

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