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1.
Chunlin Ma Qianli Li Rufen Zhang 《Journal of Inorganic and Organometallic Polymers and Materials》2009,19(2):208-214
Three types of di- and trimethyltin(IV) polymers [Me2Sn(C9H4N2O4)]n · 4H2O 1, [(Me3Sn)2(C9H4N2O4)]n · H2O 2 and [(Me3Sn)2(C9H4N2O4)]n · CH3OH 3 have been synthesized by the reaction of trimethyltin chloride with benzimidazole-5,6-dicarboxylic acid under three different
experimental conditions. All the complexes were characterized by elemental analysis, IR, NMR (1H, 13C, 119Sn) spectroscopy and X-ray crystallography diffraction analysis. The structure analyses reveal that complex 1 has a 1D helical chain in which benzimidazole-5,6-dicarboxylic acid act as a tetradentate (O,O-chelation) ligand coordinating to dimethyltin (IV) ions, two water molecules take part in the coordination giving seven-coordinated
tin centers in the component. Complex 2 and 3 are 2D and 3D corrugated polymers in which the deprotoned acid as tetradentate ligand affords by three oxygen atoms and a
nitrogen atom. 相似文献
2.
Louwanda Lakiss Anglique Simon-Masseron Volker Gramlich Grald Chaplais Joël Patarin 《Microporous and mesoporous materials》2008,114(1-3):82-92
One way to obtain new materials is to exploit the in situ generation of the structure-directing agent. By this synthetic route, solvents or precursors of the templates are introduced into the starting mixtures, and during the synthesis, they partly decompose into molecules that act as templates. This paper deals with the synthesis of a fluorogallophosphate with a new template precursor, the N-formylmorpholine. This compound, used as main solvent, is unstable in acidic media. At high temperature it decomposes and generates in situ the morpholine molecules. We report the structure of a two-dimensional fluorogallophosphate named Mu-38 structurally related to ULM-9. This compound Ga3P3O12F3[C4H10NO]3 (Z = 4) consists of anionic inorganic layers containing single four rings units linked and charge-balanced by protonated morpholine. It was also characterized by powder XRD, SEM, elemental and thermal analyses, and solid state NMR spectroscopy (13C, 19F and 31P MAS and 31P CP MAS experiments). 相似文献
3.
Fenghui Liu Wanzhi Chen Xiaozeng You 《Journal of Inorganic and Organometallic Polymers》2003,13(1):1-8
Reactions of K2Cr2O7 and K2CrO4 with Me3SnCl yielded [(Me3Sn)2CrO4] (1) and [(Me3Sn)2CrO4(Me3SnOH)] (2), respectively, which were characterized by elemental analysis, 1H-NMR spectroscopy, and an X-ray diffraction study. Compound 1 shows a novel square grid-like structure consisting of CrO4
2– and Me3Sn+ ions, whereas 2 exhibits a three-dimensional structure composed of CrO4
2–, Me3Sn+, and [(Me3Sn)2SnOH]+ ions. 相似文献
4.
Rufen Zhang Yun Ren Qingfeng Wang Chunlin Ma 《Journal of Inorganic and Organometallic Polymers and Materials》2010,20(2):399-404
Two types of di- and trimethyltin(IV) polymers [(Me2Sn)4O2(C10H8O4)4]
n
1 and [(Me3Sn)2(C10H8O4)]
n
·DMF 2 have been synthesized by the reaction of trimethyltin chloride with (±)-phenylsuccinic acid under two different experimental
conditions. Both of the complexes are characterized by elemental analysis, IR, NMR (1H, 13C, 119Sn) spectroscopy and X-ray crystallographic diffraction analysis. The structural analyses show that complex 1 is a two-dimensional corrugated sheet polymer consisting of dimeric tetraorganodistannoxane units and bridging ligands. Complex
2 is a 3D corrugated polymer in which the deprotoned acid occurs as a tetradentate ligand and is bonded by the four oxygen
atoms. It is worth noting that the X-ray diffraction study reveals that complex 2 crystallizes in the orthorhombic space group P212121, which is chiral space group. 相似文献
5.
Abstract
A vanadium–magnesium oxide catalyst (VMgO) with a V2O5 concentration of 15% by weight was employed for the oxidative dehydrogenation of n-octane to produce the corresponding linear octenes and C8 aromatics. The catalyst was synthesized by the wet impregnation method, and was characterized by in situ XRD, TGA-DSC, and 51V MAS NMR. The used catalysts were characterized by powder XRD, BET, pore volume analysis, SEM, EDX, ICP-OES, and 15V MAS NMR. The catalytic testing was carried out at different n-octane/O2 molar ratios (viz. 0.1, 0.4, 0.8, 1.2, and 1.6) at a GHSV of 8,000 h−1 in a continuous flow fixed bed reactor. The results showed that the catalytic performance with regard to both activity and selectivity was very sensitive to the strength of the oxidative environment (n-octane to oxygen ratio). No phasic changes were observed in the used catalysts. However, some textural changes were induced by the catalytic testing. 相似文献6.
Ru-Fen Zhang Bao-Ying Zhang Yun Ren Chun-Lin Ma 《Journal of Inorganic and Organometallic Polymers and Materials》2012,22(1):149-157
A series of organotin(IV) carboxylates complexes; namely, [(Me2Sn)4O2(RCOO)4] (R = C12H15
1, C9H11
2, C8H8ClO 3, C7H9
4) and [Me3(RCOO)]n (R = C12H15
5, C9H11
6, C8H8ClO 7, C7H9
8) have been synthesized. All complexes were characterized by elemental analysis, FT-IR, and NMR (1H, 13C and 119Sn) spectroscopy. Among them, the structures of complexes 1–3 and 5–8 were also determined by X-ray crystallography. The structural analysis showed that complexes 1–3 are the same tetranuclear monomer, and complexes 5–8 are the same 1D zigzag chain coordination polymer. Furthermore, each complex 1, 2 and 3, can form a supramolecular chain through weak intermolecular interactions. 相似文献
7.
Marta Abrantes Anabela A. Valente Martyn Pillinger Carlos C. Romão Isabel S. Gonçalves 《Catalysis Letters》2007,114(1-2):103-109
Vibrational spectroscopy and EXAFS studies of an organotin molybdate with the formula [((Me)2(menthyl)Sn)2MoO4(H2O)3.5] reveal that the compound is polymeric and contains [MoO4]2− tetrahedra coordinated to [R3Sn]+ cationic spacers. The compound can be used as a recyclable solid catalyst for the selective epoxidation of cyclooctene by
tert-butylhydroperoxide. In the epoxidation of prochiral olefins such as trans-β-methylstyrene, the corresponding epoxide isomers are obtained with fairly good to excellent selectivity, albeit with low
enantiomeric or diastereomeric excesses. 相似文献
8.
Chunlin Ma Qingfeng Wang Rufen Zhang 《Journal of Inorganic and Organometallic Polymers and Materials》2009,19(2):152-156
A novel 3D tri-n-butyltin complex [(n-Bu3Sn)2(C2H2N4SCO2)]n (1) has been solvothermally synthesized and structurally characterized by elemental analysis, FT-IR, NMR (1H, 13C, and 119Sn) spectra and X-ray crystallography. X-ray data of complex 1 reveals that it is a 3D tri-n-butyltin coordination polymer with a metal-organic framework (MOF) structure , significant N → Sn interactions plays an important
role in the construction of this structure. 相似文献
9.
Safaa Eldin H. Etaiw Tarek A. Fayed Mohamed B. El-zaria Safaa N. Abdou 《Journal of Inorganic and Organometallic Polymers and Materials》2011,21(1):36-42
Self assembly of K3[Cu(CN)4] with Me3SnCl and quinoxaline (qox) affords the new organotin ternary adduct ∞3[Cu2(CN)3·Me3Sn·qox], 1, as orange platelet crystals. The supramolecular architecture of 1 consists of [Cu2(CN)3]− building blocks connected by the (Me3Sn)+ cations forming infinite corrugated 1D-chains. The chains are bridged by the qox molecules forming 2D-layers containing fused
distorted polygons. The layers are interwoven forming 3D-network structure, which are stabilized by close packing effects
such as H-bonds as well as Cu···Cu and π–π interactions. IR and mass spectra as well as TGA are investigated. 相似文献
10.
AnaC. Coelho SaleteS. Balula SofiaM. Bruno JooC. Alonso Nicolas Bion Paula Ferreira Martyn Pillinger AnabelaA. Valente Joo Rocha IsabelS. Gonalves 《Advanced Synthesis \u0026amp; Catalysis》2010,352(10):1759-1769
Arenetricarbonyl complexes, or the general formula C6H4Mo(CO)3 , were incorporated into crystal‐like mesoporous phenylene‐silica by liquid‐phase deposition of molybdenum hexacarbonyl [Mo(CO)6]. By adjusting the reaction conditions, different molybdenum loadings of 1.5 and 5.9 wt% were obtained, which correspond to 3% and 14% of the phenylene contents. The texture properties of the materials as well as the nature of the surface‐fixed complexes were characterized by powder X‐ray diffraction, transmission electron microscopy (TEM), N2 adsorption, FT‐IR, UV‐vis and MAS (13C, 29Si) NMR spectroscopy. The derivatized organosilicas were examined as catalyst precursors for the liquid‐phase epoxidation of cis‐cyclooctene, 1‐octene, trans‐2‐octene and (R)‐(+)‐limonene at 55 °C, using tert‐butyl hydroperoxide as the oxidant. For each olefin the corresponding epoxide was the only product detected. In the case of cyclooctene, the intrinsic reaction rates per surface molybdenum atom were similar for both Mo loadings (TOF∼1150 mol molMo−1 h−1), suggesting that the resultant materials act as single site epoxidation catalysts. Leaching tests and metal analyses of reaction solutions showed that the catalytic activity stemmed from the immobilized species and not from the leaching of active species into solution. The oxidation of limonene gave limonene oxide as the only product in 95% yield at 3 h, which reveals an outstanding regioselectivity to the epoxidation of the endocyclic double bond. 相似文献
11.
Rufen Zhang Yinfeng Han Chunlin Ma 《Journal of Inorganic and Organometallic Polymers and Materials》2006,16(1):25-29
A novel one-dimensional (1D) supramolecular dimethyltin compound of (Me2SnO)2(Me2SnOCH3)(O2CCH2SC4H3N2-2,6)[Me2Sn(O2CCH2SC4H3N2-2,6)2]·CH3OH was prepared by the reaction of (CH3)2SnCl2 with (2-pyrimidylthio)acetic acid with CH3ONa as a base. The title compound contained four different tin atom environments. Among them, Sn(1) and Sn(2) were both five-coordinate
with distorted trigonal bipyramidal geometries, Sn(3) was six-coordinate with a distorted octahedral geometry and Sn(4) was
seven-coordinate with pentagonal bipyramidal geometry. Meanwhile, the compound was stabilized in a 1D infinite chain by intermolecular
Sn–O bonds.
An erratum to this article can be found at 相似文献
12.
Proton conduction in novel anhydrous membranes based on host polymer, poly(4-vinylbenzylboronic acid), (P4VBBA) and phosphoric acid, (H3PO4) as proton solvent was studied. The materials were prepared by the insertion of the proton solvent into P4VBBA at different stoichiometric ratios to get P4VBBA·xH3PO4 composite electrolytes. Homopolymer and the composite materials were characterized by FT-IR, 11B MAS NMR and 31P MAS NMR. 11B MAS NMR results suggested that acid doping favors or leads to a four-coordinated boron arrangement. 31P MAS NMR results illustrated the immobilization of phosphoric acid to the polymer through condensation with boron functional groups (B-O-P and/or B-O-P-O-B). Thermogravimetric analysis (TGA) showed that the condensation of composite materials starts approximately at 140 °C. An exponential weight loss above this temperature was attributed to intermolecular condensation of acidic units forming cross-linked polymer. The insertion of phosphoric acid into the matrix softened the materials shifting Tg to lower temperatures. The temperature dependence of the proton conductivity was modeled with Arrhenius relation. P4VBBA·2H3PO4 has a maximum proton conductivity of 0.0013 S/cm at RT and 0.005 S/cm at 80 °C. 相似文献
13.
《国际聚合物材料杂志》2012,61(3-4):695-700
Abstract The effect of addition of poly (propylene oxide) (PPO) and polystyrene with low molecular weight (LPS) to polystyrene (PS) was investigated blending these polymers in a Haake internal mixer. The PPO and LPS range was established up to 10% by weight. The blends were analysed by differential scanning calorimetry (DSC) and carbon-13 nuclear magnetic resonance spectroscopy at solid state (NMR), using conventional NMR techniques as cross-polarisation/magic angle spinning (CP/MAS) and proton spin-lattice relaxation time in the rotating frame (T 1 H p ). The addition of 1 and 5% of PPO and 5% of LPS to PS made the blends of PS/PPO and PS/LPS more rigid. 相似文献
14.
Zohreh Rashidi Ranjbar Ali Morsali 《Journal of Inorganic and Organometallic Polymers and Materials》2011,21(3):421-430
A new zinc(II) coordination polymer, {[Zn(bpcdp)2(DMF)4](ClO4)2·(H2O)2}n (1) bpcdp = 2,6-bis(4-pyridinecarboxamide)pyridine has been synthesized and characterized by IR, 1HNMR and 13CNMR spectroscopy. The single crystal X-ray data of compound 1 shows the zinc(II) atom has been considered as octahedral with ZnN2O4 coordination sphere. Two nitrogen atoms of bpcdp ligand and four oxygen atoms of DMF molecules have occupied coordination
sphere around zinc(II) atoms. The prepared zinc(II) coordination polymer grows in three-dimensional network by hydrogen bonding
and π–π stacking interaction. The nanostructure of compound 1 were obtained by sonochemical process and studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD),
IR and NMR spectroscopy. Thermal stabilities of single crystalline and nano-size samples of compound 1 were studied by thermal gravimetric (TG) and differential thermal analyses (DTA). The ZnO nanoparticles were obtained by
direct calcination of compound 1 at 400 °C and by thermolysis in oleic acid at 200 °C. The obtained zinc(II) oxide nanoparticles were characterized by X-ray
diffraction (XRD) and scanning electron microscopy (SEM). 相似文献
15.
Rufen Zhang Shaoliang Zhang Chunlin Ma Qingfeng Wang 《Journal of Inorganic and Organometallic Polymers and Materials》2012,22(2):500-506
Four new organotin (IV) complexes of two types [(R2Sn)2(C7H10O4)(μ3-O)]
n
(R = Me: 1; nBu: 2; and {(R3Sn)2[C5H10(COO)2]}
n
(R = Me: 3; nBu: 4) have been synthesized by the reaction of 3-methyladipic acid with the corresponding R3SnCl (R = Me, nBu) under two different experimental conditions. All the complexes were characterized by elemental analysis, FT-IR, and NMR
(1H, 13C, 119Sn) spectroscopy. Except for 2, all of the complexes were also characterized by X-ray crystallography. The structural analyzes show that complex 1 is a 1D infinite chain polymer and forms a 2D organotin framework through intermolecular C–H···O interactions and weak Sn···O
interactions. Complexes 3 and 4 are 2D network polymers in which 3-methyladipic acid acts as a tetra dentate ligand coordinated to the trialkyltin (IV) ion. 相似文献
16.
A series of Al2O3-SnO2 catalysts with the mole ratio of Al2O3 to SnO2 equal to 1:1, 1 0.5, 1 0.1, 1 0.05 and 1 0.01 were characterized by31P NMR of adsorbed trimethyl phosphine (TMP) and119Sn MAS NMR spectroscopy. It was found from31P NMR that no Brønsted acid sites exist in these samples. Pure SnO2 shows two different types of Lewis acid sites; in the mixed oxide samples a Lewis peak characteristic of pure Al2O3 is always seen, together with either one or two other Lewis peaks, depending on the Sn concentration.119Sn CP/MAS NMR spectra of the highest Sn-content sample show one narrow line at –603 ppm superimposed on a very broad line, indicating a strong interaction between Al and Sn oxides. 相似文献
17.
Thermogravimetry (TG), differential thermal analysis (DTA), and differential scanning calorimetry (DSC) have been used to examine the thermal behavior of Sn+KClO3, Sn+KNO3, and Sn+KClO4 pyrotechnic systems and the results were compared with thermal characteristics of individual constituents. TG curves for tin powder, heated alone in air, showed a relatively slow oxidation above 570 °C. From thermal results the decomposition temperatures of KClO3, KClO4, and KNO3, in nitrogen atmosphere, were measured at 472, 592 and 700 °C, respectively. For the Sn+KNO3 pyrotechnic system, the tin oxidation was completed within the range of 480 to 500 °C. Replacing KNO3 with KClO4 led to an increase of thermal stability of the pyrotechnic mixture. Among above‐mentioned pyrotechnic mixtures, Sn+KClO3 has the lowest ignition temperature at about 390 °C. The apparent activation energy (E), ΔG#, ΔH# and ΔS# of the combustion processes were obtained from the DSC experiments. Based on these kinetic data and ignition temperatures, the relative reactivity of these mixtures was found to obey in the following order: Sn+KClO3>Sn+KNO3>Sn+KClO4. 相似文献
18.
Zhongjun Gao Handong Yin Li Sun 《Journal of Inorganic and Organometallic Polymers and Materials》2006,16(1):83-89
Two types of diorganotins [R2Sn(OCOC5H3N-3-Br-5)2]
n
and {[R2Sn(OH2)(OCOC5H3N-3-Br-5)2]2}
n
(R= Me, n-Bu, Ph, n-Oc), are prepared from 5-Br-omonicotinic acid and diorganotin oxides. All the compounds, 1–8, are characterized by elemental analysis as well as IR and 1H-NMR spectroscopy. The crystal structures of [R2Sn(OCOC5H3N-3-Br-5)2]
n
(2) and {[R2Sn(OH2)(OCOC5H3N-3-Br-5)2]2}
n
(8) were determined by single crystal X-ray diffraction. In compound 2, each carboxylate moiety of 5-Br-omonicotinic acid is involved in coordination to one Sn atom via two O-atoms, and the N-atom
of one pyridine-ring coordinates to the neighboring Sn atom which leads to a polymeric chain. And the N-atom of the other
pyridine-ring is dissociative. In compound 8, the compound proves to be dinuclear macrocyclic compounds with 5-Br-omonicotinic acid bridging the adjacent tin atoms with
a 12-member ring. The hydrogen bonds (
) are observed in the compound 8. These intermolecular hydrogen bonds form another ring, and lead to a polymeric chain in the lattice at the same time.
An erratum to this article can be found at 相似文献
19.
The epoxidation of 1-octene with t-butyl hydroperoxide in the presence of Mo(CO)6 has been studied. The influence of the crucial parameters on the yield of 1,2-epoxyoctane in relation to hydroperoxide, on the hydroperoxide conversion, on the selectivity of the transformation of 1-octene to epoxy compound and on the yield of 1,2-epoxyoctane in relation to 1-octene has been described by the use of regression functions in the form of a second order polynomial. The optimal values of parameters: reaction time, temperature, olefin to hydroperoxide mol ratio, Mo(CO)6 to hydroperoxide mol ratio, ensuring the maximum values of these functions have been determined. 相似文献
20.
《分离科学与技术》2012,47(14):2987-2999
Abstract Magnetic π‐complexation sorbents were studied for petroleum product desulfurization by fluorescent technique. The ability of metal cation to form π‐complexation decreases in the order following: Cu+>Ni2+>Co2+>Al3+. The order is consistent with that of desulfurization performance of their corresponding magnetic sorbents (γ‐Al2O3‐Cu(I)>γ‐Al2O3‐Ni(II)>γ‐Al2O3‐Co(II)>γ‐Al2O3). Both π‐complexation strength and desulfurization performance of the sorbents increase with temperature. The adsorptive performances of magnetic γ‐Al2O3‐Cu(I) sorbent to different compounds have the following orders: DBT>fluorene, and pyrene>naphthalene>benzene, respectively. In this study, dibenzothiophene (DBT) was used as a model sulphur‐containing compound for desulfurization. The maximal adsorption amount of magnetic γ‐Al2O3‐Cu(I), was 0.362 mmol DBT g?1. 相似文献