s: Ultrafine A2La2Ti3O10 (A=K, Na) powders with laminar structure were successfully synthesized by citric acid sol-gel method using ANO3(A=K, Na)?La(NO3)3?Ti(OBu)4 and citric acid as starting precursors. The crystalli...s: Ultrafine A2La2Ti3O10 (A=K, Na) powders with laminar structure were successfully synthesized by citric acid sol-gel method using ANO3(A=K, Na)?La(NO3)3?Ti(OBu)4 and citric acid as starting precursors. The crystalline phase of A2La2Ti3O10 can be obtained by thermal decomposition of citrate complex precursors at a relatively low temperature of 800 ℃ (600 ℃ for A=Na), about 300 ℃(500 ℃ for A=Na) lower than that of conventional solid state reaction process. The properties of the citrate precursors and the calcined powders were characterized by Infrared spectroscopy (IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), thermal-gravimetric-differential thermal analysis (TG-DTA), inductively coupled plasma (ICP) and Brunauer-Emmett-Teller (BET) techniques. Results show that the average size of A2La2Ti3O10 powders obtained by citric acid sol-gel route was reduced to 200 nm×250 nm and the specific surface area was up to 19 m2·g-1. At the same time, the product was with more regular morphological characteristics. The synthesis process and the formation of A2La2Ti3O10 were also discussed. The obtained A2La2Ti3O10 was found to be transformed from A2La2Ti3O9.5 during the formation process.展开更多
A novel cadmium(Ⅱ) isothiocyanate complex [Cd(N-MeIM)2(SCN)2]n (N-MeIM=N-methylimidazole) has been prepared and characterized by spectroscopic analysis and crystallographic method. The title compound crystallize in t...A novel cadmium(Ⅱ) isothiocyanate complex [Cd(N-MeIM)2(SCN)2]n (N-MeIM=N-methylimidazole) has been prepared and characterized by spectroscopic analysis and crystallographic method. The title compound crystallize in the Triclinic system, space group P1, with lattice parameters a=0.589 50(12) nm, b=0.785 70(16) nm, c=0.882 00(18) nm, α=110.98(3)°, β=106.49(3)°, γ=95.08(3)°, and Z=1. The title compound exhibits an infinite chain structure in which each pair of Cd atoms is bridged by two η-1,3-SCN- groups. The unique Cd atom lies on an inversion centre and the coordination sphere is completed by two N-MeIM N atoms to form a CdS2N4 octahedron. The polymeric chains are further extended into three-dimensional network via π...π stackings interactions between the imidazole rings. The cyclic voltammetry behaviors of the compound on glass carbon electrode showed a typical irreversible process. CCDC: 265283.展开更多
The reaction of nano-SiO2 grafted with 1-octyl alcohol was carried out by the normal reflux and the microwave irradiation method respectively. The surface structure and characteristics of modified silica powder were s...The reaction of nano-SiO2 grafted with 1-octyl alcohol was carried out by the normal reflux and the microwave irradiation method respectively. The surface structure and characteristics of modified silica powder were studied and characterized by various experiments and methods such as contact angle, viscosity, FT-IR, DTA, TGA, XPS et al. The results indicated that the nano-SiO2 surface was modified notably by the two methods. Compared with the normal reflux method, the microwave irradiation method has the merits of promoting the reaction and increasing the grafting rate.展开更多
N-salicylidene-benzylamineato M(Ⅱ) complexes (ZnL2, CuL2 and CdL2) were synthesized, characterized and valued for antimicrobial activities against bacterial strands using the agar diffusion method. The crystal of ZnL...N-salicylidene-benzylamineato M(Ⅱ) complexes (ZnL2, CuL2 and CdL2) were synthesized, characterized and valued for antimicrobial activities against bacterial strands using the agar diffusion method. The crystal of ZnL2 was determined by X-ray diffraction. It crystallizes in the Monoclinic system, space group C2/c with a=2.269 1(3), b=0.918 2(1), c=1.239 5(2) nm, β=117.89(2), Z=4, R1=0.049 4, wR2=0.138 2. The complexes were found to be active against Staphylococcus aureus and Eschierichia Coli. CCDC: 249474.展开更多
A new stearic acid method(SAM) has been used to prepare ultrafine K2La2Ti3O10 nanocrystalline. Each state of synthesis process was followed by the use of FT IR analysis. The resulting materials have been characterized...A new stearic acid method(SAM) has been used to prepare ultrafine K2La2Ti3O10 nanocrystalline. Each state of synthesis process was followed by the use of FT IR analysis. The resulting materials have been characterized by means of XRD, TEM, BET surface area analysis. The acid exchanging property of the obtained product was also studied. The experimental results showed that comparing with the product of traditional solid state reaction, the particle size of the K2La2Ti3O10 synthesized by SAM is greatly reduced, BET surface area is high(more than 11.83m2· g- 1) and has different acid exchanging properties. It can be easily exfoliated in 2mol· L- 1 HNO3 solution.展开更多
A new tripodal complex (ClO4)2 (C26H31Cl2N7O8Zn) was synthesized by Schiff base condensation of 2-aminoethyl-bi(3-aminopropyl)amine with 2-pyridinecarbaldehyde in the presence of Zn2+ and characterized by X-ray diffra...A new tripodal complex (ClO4)2 (C26H31Cl2N7O8Zn) was synthesized by Schiff base condensation of 2-aminoethyl-bi(3-aminopropyl)amine with 2-pyridinecarbaldehyde in the presence of Zn2+ and characterized by X-ray diffraction and ES mass spectral analysis. It crystallized in the Monoclinic system, space group P21/c with a=1.088 5(4) nm, b=1.614 6(6) nm, c=1.783 0(5) nm, a=94.405(2) the four test bacterial organisms. CCDC: 231275.展开更多
The synthesis,structural characterization and thermal behavior of a novel one-dimensional manganese (Ⅱ) complex of formula [Mn(1,5-nds)(Him)4]n [1,5-nds=naphthalene-1,5-disulfonate,Him=imidazole] is reported.The comp...The synthesis,structural characterization and thermal behavior of a novel one-dimensional manganese (Ⅱ) complex of formula [Mn(1,5-nds)(Him)4]n [1,5-nds=naphthalene-1,5-disulfonate,Him=imidazole] is reported.The complex crystallizes in the triclinic system,space group P1,with a=0.835 42(13) nm,b=0.983 45(18) nm,c= 0.987 42(19) nm,α=60.523 0(10)°,β=97.748(2)°,γ=87.189(2)° and Z=2.The 1,5-nds ligand assumes the μ2 coordination mode and interlinks Mn(Ⅱ) ions into infinite one-dimensional chain structure along [111] direction,with the adjacent Mn…Mn distance being 1.144 99(12) nm.The chains are assembled into a three-dimensional supramolecular architecture via hydrogen bonds and C-H…π interactions.IR spectra and thermal analysis data are in agreement with the crystal structure.展开更多
首次以天然红辉沸石水热合成了 Y 型、P 型分子筛,以 IR 研究了水热合成体系中分子筛结构的演变及晶相分布规律。研究表明,在高 H_2O/Na_2O、低Ca^(2+)/Na^+体系中,主晶相为 Y 型分子筛,在低 H_2O/Na_2O、高 Ca^(2+)/Na^+体系中,主晶相...首次以天然红辉沸石水热合成了 Y 型、P 型分子筛,以 IR 研究了水热合成体系中分子筛结构的演变及晶相分布规律。研究表明,在高 H_2O/Na_2O、低Ca^(2+)/Na^+体系中,主晶相为 Y 型分子筛,在低 H_2O/Na_2O、高 Ca^(2+)/Na^+体系中,主晶相为 P 型分子筛。展开更多
The complex [Zn(acac)2(C5H4NOH)] was synthesized based on the reaction of zinc(Ⅱ)acetate,acetylaceton and 3-hydroxypyridine(C5H4NOH)in methanol medium.The structure of the complex was confirmed by IR,1H NMR,elemental...The complex [Zn(acac)2(C5H4NOH)] was synthesized based on the reaction of zinc(Ⅱ)acetate,acetylaceton and 3-hydroxypyridine(C5H4NOH)in methanol medium.The structure of the complex was confirmed by IR,1H NMR,elemental analysis,thermal analysis and X-ray single crystal diffraction.The crystal belongs to monoclinic system with space group P21/n,and a=0.743 7(3)nm,b=0.829 5(3)nm,c=2.612 5(9)nm,β=95.026(6)°,V=1.605 4(9)nm3;Dc=1.484 g·cm-3;Z=4;F(000)=744;μ=1.551 mm-1.Zinc(Ⅱ)atom lies at the center of an coordination of the distorted square pyramidal formed by four O atoms which come from two different acetylaceton ions and one N atom from the 3-hydroxypyridine molecule.CCDC:600232.展开更多
Mixed coordination compounds M(α AP)2(OAc)2 (M=Ni, Zn) were synthesized individually via solid phase reactions between α aminopyridine and nickel acetate or zinc acetate at room temperature and were characterized by...Mixed coordination compounds M(α AP)2(OAc)2 (M=Ni, Zn) were synthesized individually via solid phase reactions between α aminopyridine and nickel acetate or zinc acetate at room temperature and were characterized by elemental analysis, IR and X ray powder diffraction. Zn(α AP)2(OAc)2 was also determined by 1H NMR, TGA and X ray single crystal diffraction. The crystal belongs tomonoclinic system with space group P21/c, a=9.1900(18)?, b=13.900(3)?, c=13.310(3)?, β=92.40(3)°, V=1698.7(6)?3, Dc=1.453g·cm-3, Z=4,F(000)=768, μ=1.469mm-1, R1=0.0376, wR2=0.1202. Each zinc?atom lies at the center of a distorted tetrahedron composed of two oxygen atoms from a pair of monodentate acetate groups and two nitrogen atoms from a pair of pyridine rings.展开更多
文摘s: Ultrafine A2La2Ti3O10 (A=K, Na) powders with laminar structure were successfully synthesized by citric acid sol-gel method using ANO3(A=K, Na)?La(NO3)3?Ti(OBu)4 and citric acid as starting precursors. The crystalline phase of A2La2Ti3O10 can be obtained by thermal decomposition of citrate complex precursors at a relatively low temperature of 800 ℃ (600 ℃ for A=Na), about 300 ℃(500 ℃ for A=Na) lower than that of conventional solid state reaction process. The properties of the citrate precursors and the calcined powders were characterized by Infrared spectroscopy (IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), thermal-gravimetric-differential thermal analysis (TG-DTA), inductively coupled plasma (ICP) and Brunauer-Emmett-Teller (BET) techniques. Results show that the average size of A2La2Ti3O10 powders obtained by citric acid sol-gel route was reduced to 200 nm×250 nm and the specific surface area was up to 19 m2·g-1. At the same time, the product was with more regular morphological characteristics. The synthesis process and the formation of A2La2Ti3O10 were also discussed. The obtained A2La2Ti3O10 was found to be transformed from A2La2Ti3O9.5 during the formation process.
文摘A novel cadmium(Ⅱ) isothiocyanate complex [Cd(N-MeIM)2(SCN)2]n (N-MeIM=N-methylimidazole) has been prepared and characterized by spectroscopic analysis and crystallographic method. The title compound crystallize in the Triclinic system, space group P1, with lattice parameters a=0.589 50(12) nm, b=0.785 70(16) nm, c=0.882 00(18) nm, α=110.98(3)°, β=106.49(3)°, γ=95.08(3)°, and Z=1. The title compound exhibits an infinite chain structure in which each pair of Cd atoms is bridged by two η-1,3-SCN- groups. The unique Cd atom lies on an inversion centre and the coordination sphere is completed by two N-MeIM N atoms to form a CdS2N4 octahedron. The polymeric chains are further extended into three-dimensional network via π...π stackings interactions between the imidazole rings. The cyclic voltammetry behaviors of the compound on glass carbon electrode showed a typical irreversible process. CCDC: 265283.
文摘The reaction of nano-SiO2 grafted with 1-octyl alcohol was carried out by the normal reflux and the microwave irradiation method respectively. The surface structure and characteristics of modified silica powder were studied and characterized by various experiments and methods such as contact angle, viscosity, FT-IR, DTA, TGA, XPS et al. The results indicated that the nano-SiO2 surface was modified notably by the two methods. Compared with the normal reflux method, the microwave irradiation method has the merits of promoting the reaction and increasing the grafting rate.
文摘N-salicylidene-benzylamineato M(Ⅱ) complexes (ZnL2, CuL2 and CdL2) were synthesized, characterized and valued for antimicrobial activities against bacterial strands using the agar diffusion method. The crystal of ZnL2 was determined by X-ray diffraction. It crystallizes in the Monoclinic system, space group C2/c with a=2.269 1(3), b=0.918 2(1), c=1.239 5(2) nm, β=117.89(2), Z=4, R1=0.049 4, wR2=0.138 2. The complexes were found to be active against Staphylococcus aureus and Eschierichia Coli. CCDC: 249474.
文摘A new stearic acid method(SAM) has been used to prepare ultrafine K2La2Ti3O10 nanocrystalline. Each state of synthesis process was followed by the use of FT IR analysis. The resulting materials have been characterized by means of XRD, TEM, BET surface area analysis. The acid exchanging property of the obtained product was also studied. The experimental results showed that comparing with the product of traditional solid state reaction, the particle size of the K2La2Ti3O10 synthesized by SAM is greatly reduced, BET surface area is high(more than 11.83m2· g- 1) and has different acid exchanging properties. It can be easily exfoliated in 2mol· L- 1 HNO3 solution.
文摘A new tripodal complex (ClO4)2 (C26H31Cl2N7O8Zn) was synthesized by Schiff base condensation of 2-aminoethyl-bi(3-aminopropyl)amine with 2-pyridinecarbaldehyde in the presence of Zn2+ and characterized by X-ray diffraction and ES mass spectral analysis. It crystallized in the Monoclinic system, space group P21/c with a=1.088 5(4) nm, b=1.614 6(6) nm, c=1.783 0(5) nm, a=94.405(2) the four test bacterial organisms. CCDC: 231275.
文摘The synthesis,structural characterization and thermal behavior of a novel one-dimensional manganese (Ⅱ) complex of formula [Mn(1,5-nds)(Him)4]n [1,5-nds=naphthalene-1,5-disulfonate,Him=imidazole] is reported.The complex crystallizes in the triclinic system,space group P1,with a=0.835 42(13) nm,b=0.983 45(18) nm,c= 0.987 42(19) nm,α=60.523 0(10)°,β=97.748(2)°,γ=87.189(2)° and Z=2.The 1,5-nds ligand assumes the μ2 coordination mode and interlinks Mn(Ⅱ) ions into infinite one-dimensional chain structure along [111] direction,with the adjacent Mn…Mn distance being 1.144 99(12) nm.The chains are assembled into a three-dimensional supramolecular architecture via hydrogen bonds and C-H…π interactions.IR spectra and thermal analysis data are in agreement with the crystal structure.
文摘首次以天然红辉沸石水热合成了 Y 型、P 型分子筛,以 IR 研究了水热合成体系中分子筛结构的演变及晶相分布规律。研究表明,在高 H_2O/Na_2O、低Ca^(2+)/Na^+体系中,主晶相为 Y 型分子筛,在低 H_2O/Na_2O、高 Ca^(2+)/Na^+体系中,主晶相为 P 型分子筛。
文摘The complex [Zn(acac)2(C5H4NOH)] was synthesized based on the reaction of zinc(Ⅱ)acetate,acetylaceton and 3-hydroxypyridine(C5H4NOH)in methanol medium.The structure of the complex was confirmed by IR,1H NMR,elemental analysis,thermal analysis and X-ray single crystal diffraction.The crystal belongs to monoclinic system with space group P21/n,and a=0.743 7(3)nm,b=0.829 5(3)nm,c=2.612 5(9)nm,β=95.026(6)°,V=1.605 4(9)nm3;Dc=1.484 g·cm-3;Z=4;F(000)=744;μ=1.551 mm-1.Zinc(Ⅱ)atom lies at the center of an coordination of the distorted square pyramidal formed by four O atoms which come from two different acetylaceton ions and one N atom from the 3-hydroxypyridine molecule.CCDC:600232.
文摘Mixed coordination compounds M(α AP)2(OAc)2 (M=Ni, Zn) were synthesized individually via solid phase reactions between α aminopyridine and nickel acetate or zinc acetate at room temperature and were characterized by elemental analysis, IR and X ray powder diffraction. Zn(α AP)2(OAc)2 was also determined by 1H NMR, TGA and X ray single crystal diffraction. The crystal belongs tomonoclinic system with space group P21/c, a=9.1900(18)?, b=13.900(3)?, c=13.310(3)?, β=92.40(3)°, V=1698.7(6)?3, Dc=1.453g·cm-3, Z=4,F(000)=768, μ=1.469mm-1, R1=0.0376, wR2=0.1202. Each zinc?atom lies at the center of a distorted tetrahedron composed of two oxygen atoms from a pair of monodentate acetate groups and two nitrogen atoms from a pair of pyridine rings.
