Synthesis and Characterization of Quaternary Complexes [Ln(CH_2=C(CH_3)-COO)_2(NO_3)(phen)]_2

Many trinary lanthanide complexes have been studied. However, few mixed anion complexes with bidentate heterocyclic amines were synthesized. Mixed anion complexes [Ln (CH2=C(CH3)-COO)2(NO3)(phen)]2 was synthesized and its properties were determined by elemental analyses, IR and TGA. The IR spectra analysis indicate that NO3- , CH2=C(CH3)-COO- and Phen are coordinated with Ln. And the fluorescent spectra of [Eu(CH2=C(CH3)-COO)2(NO3)(phen)]2 and 1H NMR spectra of [La(CH2=C(CH3)-COO)2 (NO3)(phen)]2 was determined respectively.     

Synthesis and properties of a Pr（Ⅲ） complex with 2-acetylbenzimidazoledehyde-glycine Schiff-base ligand

Abstract The 2-acetyl-benzimidazoledehyde-glycine Schiff-base ligand and the corresponding Pr（Ⅲ） complex Pr2L3（NO3）3· 2CH3OH （L=C11H10N3O2） were synthesized in methanol and characterized by a series of methods, including chemical analysis, elemental analysis, TOF-MS, ^1H NMR, UV-, IR-, Raman spectra, thermal analysis, and the three-dimension fluorescence excitation and emission spectra. The Pr（Ⅲ） complex exhibits extraordinary water-solubility and the Pr（Ⅲ） hydroxide appears at pH≥13. The complex also possesses specific fluorescent properties. Thus, at the excitation wavelengths 200.0-280.0 and 260-350 nm the fluorescence bands were observed at 290.0 and 400.0 nm, respectively.     

Synthesis, characterization and properties of ruthenium-substituted polyoxometallic acid H_6Ru(H_2O)FeW_(11)O_(39)·18H_2O with Keggin structure

The ruthenium-substituted polyoxometallic acid H6 [Ru(H2O)FeW 11O39 ]·18H2O was synthesized by stepwise acidification and stepwise addition of solutions of the component elements, and an ion-exchange-cooling method. The product was characterized using inductively coupled plasma spectrometry (ICP), Infrared Spectroscopy (IR), Ultraviolet Spectroscopy (UV), and X-ray diffraction (XRD). The results show that this complex has the Keggin structure. The determination of the thermal stability and proton conductivi...     

DIRECT ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF NEODIMIUM( Ⅱ ) COMPLEX WITH 2-HYDROXY-2,4,6- CYCLOHEPTATRIENONE(TROPOLONE)

Tris(tropolonato)neodimium( Ⅲ )has been prepared by the electrochemical oxidation of neodimium meral anode in acetonitrile solution of 2-hydroxy - 2,4,6 - cycloheptatrienone(tropolone). The unusual divalent neodimium complex was formed at the first step of electrosyn - thesis. The final product ,Nd (C7H6O2)3, has been characterized by microanalysis and the studies of IR and H, C3 NMR spectra.     

A Novel Calixarene-containing Hyperbranched Aliphatic Polyester Incorporated with Pendant Europium Complexes

1 Results Hyperbranched polymers can be easily functionalized,while the calixarene-rare earth complexes enjoy the advantages of narrow emission bands.It is expected that materials combining their advantages can possess good luminescence properties[1-2].For this reason,in this paper,a novel calixarene-containing hyperbranched aliphatic polyester incorporated with pendant europium complexes (H2O-Cal-Eu) was synthesized and characterized by FTIR,UV and element analysis.DSC measurement shows that the glass-transition temperature (Tg) of H2O-Cal-Eu is 127 ℃,which is higher than the Tg of H2O (30 ℃).TG measurement reveals that H2O-Cal-Eu has a good thermal stability,and there is no weight loss up to 280 ℃.The decomposition temperature (Td) of H2O-Cal-Eu is in the range of 280-500 ℃.The photoluminescence (PL) properties of H2O-Cal-Eu were investigated.As predicted,H2O-Cal was proved to be an excellent energy transfer ligand for Eu3 ,with respect to photoluminescence.H2O-Cal-Eu emitted remarkably strong red luminescence.The luminescence spectra of the solid samples of complex show a narrow half spectral bandwidth of only about 10 nm,which is nearly monochromatic light.Calixarene-containing polymer incorporated with pendant Eu (Ⅲ) complexes H2O-Cal-Eu exhibits great potential as red emitting materials for future generations of electroluminescence devices.     

DIRECT ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF NEODIMIUM （Ⅲ） COMPLEX WITH 2-HYDROXY-2,4,6-CYCLOHEPTATRIENONE（TROPOLONE）

Tris(tropolonato)neodimium(Ⅲ）has been prepared by the electrochemical oxidation of neodimium metal anode in acetonitrile solution of 2-hydroxy-2,4,6-cycloheptatrienone(tropolone).The unusual divalent neodimium complex was formed at the first step of electrosyn-thesis.The final product,Nd(C7H6O2)3,has been characterized by microanalysis and the studies of IR and ^1H,C3 NMR spectra.     

A new 3-D Gd–Cu heterometallic polymer [Gd_2Cu_3(bpy)_2-(ip)_6]·6H_2O with a non-interpenetrated α-Po net

A new 3-D porous Gd-Cu heterometallic polymer [Gd2Cu3(bpy)2(ip)6]·6H2O (1) (bpy = 2,2'-bipyridine, H2ip = isophthalic acid) has been hydrothermally synthesized and structurally characterized. Compound 1 crystallizes in the triclinic space group P1and displays a 3-D non-interpenetrated α-Po network with 1-D channels filled transversely by the hexa-nuclear chain-like (H2O)6. The EPR and thermal stability of 1 were investigated.     

Thermal Stability of Poly （acrylonitrile-methyl acrylate） Copolymers

Poly （ acrylonitrile-methyl acrylate） copolymer was synthesized by water depositing polymerization and has a typical feed ratio of 85/15. And then 1 - 3 wt% lauryl alcohol maleic anhydride （LAM） was adopted as stabilizer to mix with the acrylonitrile based copolymer. The mixtures were characterized by using Fourier Transform Infrared Spectroscopy （FTIR）, Nuclear Magnetic Resonance （1 H NMR ）, Gel Permeation Chromatography （ GPC ）, Differential Scanning Calorimetry （DSC）, optic microscope and Ubbelohde viscosimetryr etc. The melting point （Tm） and glass transition temperature （Tg） of the 85/15 AN/MA copolymer mixed with LAM all decrease with the increase of stabilizer content. The lowest Tg and Tm were 116.1℃ and 209. 1℃ respectively at the heating rate of 100℃/min when the content of LAM is 2 wt%. The 85/15 AN/MA copolymer mixed with 1 - 3 w t% LAM possess good thermal stability up to 30 min at 220 ℃.     

Preparation and performance of LiNi_(0.8)Co_(0.2)O_2 cathode material based on Co-substituted α–Ni(OH)_2 precursor

Co-substituted α-Ni(OH)2 was synthesized by a novel microwave homogeneous precipitation method in the presence of urea. LiNi0.8Co0.2O2 cathode material was synthesized by calcining Co-substituted α-Ni(OH)2 precursor and LiOH·H2O at 900℃ for 10 h in flowing oxygen. XRD, FTIR, FESEM and electro- chemical tests were used to study the physical and the electrochemical performances of the materials. The results show that the prepared LiNi0.8Co0.2O2 compound has a good layered hexagonal structure. Moreover, the LiNi0.8Co0.2O2 cathode material demonstrates stable cyclability with a high initial specific discharge capacity of 183.9 mAh/g. The good electrochemical performance could be attributed to the uniform distribution of Ni2 and Co2 ions in the crystal structure and a minimal cation mixing in LiNi0.8Co0.2O2 host structure.     

Eu(Ⅲ)/Gd(Ⅲ)-HTTA-TPA-Phen配合物的共发光研究

为了研究Eu(Ⅲ)-配合物的共发光与其结构的关系,合成了Eu (Ⅲ)/Gd (Ⅲ)与2-噻酚三氟乙酰丙酮(HTTA)、对苯二甲酸(TPA)和邻菲罗啉(Phen)形成的系列配合物,并运用元素分析、红外光谱对这些配合物进行表征.共发光Gd3 离子对Eu(Ⅲ)-配合物的荧光增强效果非常明显,其共发光效果与结构的关系是:网状多核配合物Eu2(1-x)Gd2x(TPA)3Phen2 ＞ 链状多核配合物Eu1-xGdx(TPA)(TTA)Phen ＞单核配合物Eu1-xGdx(TTA)3Phen.荧光增强的机理可从配合物的单核和多核结构获得解释,异多核配合物Eu1-xGdx(TPA)(TTA)Phen与 Eu2(1-x)Gd2x(TPA)3Phen2分子内能量传递比异单核配合物Eu1-xGdx(TTA)3Phen分子间能量传递更有效.     

Formation of the Inclusion Complex of Orange II with β-Cyclodextrin and Its Photostability

Inclusion complex of Orange II with β-Cyclodextrin (β-CD) and the anti-photolysis effect under UV-light were investigated. The molar ratio of inclusion complex of β-Cyclodextrin and Orange Ⅱ is 1∶1. The formation constant K=1.236×103 L/mol was determined by the UV and Fluorescence spectra respectively, which was quite in accordance with the calculation with a modified Benesi-Hildbrand equation. The inclusion complex was characterized by the IR spectra and the molar ratio of inclusion complex is 1∶1 too. The formation constant K=1.266×103 L/mol was determined by 1 H NMR analysis and was nearly the same by UV and fluorescence spectra. The photocatalytic decolorization rate of Orange Ⅱ solutions containing β-CD and TiO2 was smaller by 51.9% than that of the Orange Ⅱ solutions only containing TiO2, while in the case of direct photolysis of Orange Ⅱ solutions, β-CD can lower the photolysis rate by 48.1% under UV-light. This result indicates β-CD can inhibit the photolysis and photocatalytic decolorization of Orange Ⅱ under UV-light. The β-CD inclusion complex was found to be persistent to UV-light photolysis.     

Synthesis and structural characterization of lanthanide coordination polymers constructed from a 13-membered macrocycle

The lanthanide coordination polymers bearing a 13-membered macrocycle, [(13-EDTA-pnOH)H2] were synthesized. The products [Ln(13-EDTA-pnOH)(H2O)2·NO3]n (Ln = Eu(1), Tb(2), Dy(3)) have been obtained by MS, IR and element analyses. The solid-state structure of 1 was established by single-crystal X-ray analysis. The coordination geometry around the central metal atom in complex 1 is a nine-coor-dinated, tricapped-trigonal prism having six donor atoms (two amine nitrogen atoms, two amide oxygen atoms and two carboxymethyl oxygen atoms) from one ligand, one oxygen atom from a neighboring ligand, and two more oxygen atoms from two water molecules. The europium atoms are linked by―Eu―O―C―O―Eu―bridges to form an infinite chain.     

Preparation and Structural Analysis of Lanthanide Complexes with α-Hydroxyl-phenyl-acetic Acid and 1, 10-Phenanthroline as Ligands

A series of ternary lanthanide complexes Ln （C6H5CHOHCOO）3（phen） （H2O） （Ln= La, Ce, Pr, Nd, Sm, Eu） were synthesized with α-hydroxyl-phenyl-acetic acid and 1, 10-phenanthroline （phen） as ligands. The sturcture and property of complexes were characterized by elemental analysis, IR, 1^H-NMR, UV and TGA, and the coordinate mede of both ligands was discussed. It was shown that the co-ordinate mode of 1, 10-phenanthroline was chelated, while α-hydraxyl-phenyl-acetate ion was monedentate or bridging. The mechanism of thermal determinde by thermogravimetry was indicated that the degree of co-ordinate ability of ligand was： α-hydroxyl-phenyl-acetate ion 〉 1, 10- phenanthroline（phen）.     

Synthesis, Characterization and Biological Activity of Transition Metals with Schiff Base Derived from Adamantaneamine and o-Vanillin

Five new solid complexes were synthesized about transition metals with Schiff base（ L, C18H23NO2 ） derived from adamantaneamine and o-vanillin, and characterized by elemental analysis, molar conductance, infrared spectra, UV-vis spectra, thermal analysis. Their chemical formula are [ML2]（ClO4）2 （ M= Mn, Co, Ni, Cu, Zn）, and the coordination numbers are four, The antibacterial activity of Schiff base ligand and its complexes was studied.     

Green Light-Emitting Region-Regular Poly（9,9-Dihexylfluorene-co-Fluorenone） Prepared from Solvent-Free Oxidative Coupling Polymerization

Soluble green light-emitting poly（9,9-dihexylfluorene- co-fluorenone） was synthesized by solvent-free oxidative coupling polymerization of 9,9-dihexylfluorene in a facile one-step reaction. The polymers were characterized by FT-IR, ^1H NMR, ^13C NMR, UV-Vis and fluorescence spectroscopy. The region-regular structure of the polymer linking at 2, 7＇-position on the fluorene moieties was obtained. The FT-IR spectra of the polymers showed fluorenone vibration. The fluorescence spectra of the solid thin film of the polymers displayed green light-emitting, which was emitted from fluorenone moieties produced in the polymerization process.     

Synthesis and Characterization of Quaternary Complexes Ln(CH_2ClCOO)_2 (NO_3) (phen)

Many binary lanthanide complexes have been studied. However, few mixed anion complexes with bidentate heterocyclic amines were synthesized. We synthesized mixed anion complexes Ln ( CH2 ClCOO )2 (NO3 ) ( phen) which was determined by elemental analyses . The IR spectra analyses indicate that NO3- , CH2 ClCOO- and phen are coordinated with Ln . The molar conductances of the complexes at 10-3 mol · L-1 were founded to be between 32.4 and 35.8 S·cm2· mol-1 , suggesting the nonelectrolytes in N-Dimethylformamide. And we determined the fluorescent spectra Eu(CH2ClCOO)2(NO3) ( phen ) and ESR spectra of Gd ( CH2 ClCOO )2 ( NO3) ( phen) .     

Preparation of nano-TiO2/diatomite-based porous ceramics and their photocatalytic kinetics for formaldehyde degradation

Diatomite-based porous ceramics were adopted as carriers to immobilize nano-TiO₂ via a hydrolysis-deposition technique. The thermal degradation of as-prepared composites was investigated using thermogravimetric-differential thermal analysis, and the phase and microstructure were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, and transmission electron microscopy. The results indicated that the carriers were encapsulated by nano-TiO₂ with a thickness of 300-450 nm. The main crystalline phase of TiO₂ calcined at 650℃ was anatase, and the average grain size was 8.3 nm. The FT-IR absorption bands at 955.38 cm-1 suggested that new chemical bonds among Ti, O, and Si had formed in the composites. The photocatalytic (PC) activity of the composites was investigated under UV irradiation. Furthermore, the photodegradation kinetics of formaldehyde was investigated using the composites as the cores of an air cleaner. A kinetics study showed that the reaction rate constants of the gas-phase PC reaction of formaldehyde were κ=0.576 mg·m-3·min-1 and K=0.048 m3.     

Inactivation of Giardia Intestinalis by Peroxone Process (H2O2/O3) and Its Disinfection Mechanisms

The efficency of peroxone( H2O2/ O3) to inactivate Giardia intestinali( G. intestinali) was investigated by the fluorescence staining method and vitro excystation. In order to investigate the mechanisms of inactivation,such as cell surface or inner cell components damage,they were comparatively examined by scanning electron microscopy( SEM),protein assay,and DNA gel analysis. When independent addition of O3 was under 1. 5mg·L- 1and contact time reached 10. 0 min,the inactivation rate achieved 99. 6%. At the same time,to achieve the same inactivation effect by H2O2/ O3,1. 0 mg·L- 1O3( [H2O2]/[O3] = 0. 8) with7. 0 min was required. Results suggest that hydroxyl radicals( ·OH) was the principal factor during the H2O2/ O3 process by testing the effect of t-butyl alcohol( TBA) and concentration change of H2O2. Although disinfectant potency of have its drawback of residual effect is transitory, but H2O2/ O3 could further strengthen the capability of inactivation, as well as reducing O3 dosage significantly. Meanwhile,SEMprotein assay,and DNA gel analysis indicate that H2O2/ O3 can destroy the cell surface,degrade the protein,and damage the genomic DNA of G. intestinali.     

Thermal Degradation Kinetics of Deoxybenzoin Polymer

The thermal degradation behavior of 4, 4-bishydroxydeoxybenzoin-polyphosphonate( BHDB-PPN) was investigated by gas chromatograph-mass spectrometer( GC-MS)and thermogravimetric analysis( TGA). It was found that BHDBPPN exhibited a different char formation way from the previous proposed mechanism based on the residue analysis by Fourier transform infrared spectra( FTIR) and the gas phase analysis by GC-MS. The thermal degradation kinetics was studied through TGA at various heating rates to identify the activation energy of BHDBPPN at two decomposition stages which were mainly attributed to the evolved phenol and benzene respectively. It was demonstrated that the activation energy at the second stage was much higher than that at the first stage,indicating that more energy was required to break the P—C bond to form benzene in comparison to the formation of phenol.     

Synthesis and structure of 3D heterometallic （3d-4f） coordination polymers： {[Ln2Cu（pydc）4（H2O）6]·2H2O}n

Two new 3D heterometallic （3d-4f） coordination polymers {[Ln2Cu（pydc）4（H2O）6]·2H2O}n [Ln = Eu （1） and Gd （2）] have been synthesized by hydrothermal reactions and characterized by elemental analysis, X-ray single-crystal analyses, and IR spectroscopy. X-ray crystal structure analyses show that 1 and 2 possess 3D networks and strong intramolecular hydrogen bonding interactions which was confirmed by thermogravimetric （TG） analysis.