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2015 Volume 31 Issue 2
2015, (2): 215-221
doi: 10.11862/CJIC.2015.059
Abstract:
Gold nanorods(GNR) with longitudinal surface plasma resonance (LSPR) absorption at 785 nm were synthesized by seed-mediated growth method and their surface was modified with polyethylene glycol (PEG) macromolecular (PEG-GNR). The photothermal conversion effect and cytotoxicity of PEG-GNRwere investigated. Different bacteria, including gram-positive bacterium Staphylococcus aureus and Bacillus cereus, gram-negative bacterium Escherichia coli and Pseudomonas aeruginosa were used to analyze the influences of concentration of PEG-GNRand laser output power on the inhibition effects. The results show that the PEG-GNRhas good antibacterial properties for both Gram positive and negative bacterium under the radiation of near-IRlaser. The concentration of PEG-GNRand laser output power determined antibacterial effects of the PEG-GNR. The preliminary investigation on the antibacterial mechanism was explored by studying of bacteria apoptosis status with fluorescence microscope and transmission electronic microscope, suggesting that the effective absorption of the PEG-GNRby the cells is one of the key factors in the process of photothermal antibiosis.
Gold nanorods(GNR) with longitudinal surface plasma resonance (LSPR) absorption at 785 nm were synthesized by seed-mediated growth method and their surface was modified with polyethylene glycol (PEG) macromolecular (PEG-GNR). The photothermal conversion effect and cytotoxicity of PEG-GNRwere investigated. Different bacteria, including gram-positive bacterium Staphylococcus aureus and Bacillus cereus, gram-negative bacterium Escherichia coli and Pseudomonas aeruginosa were used to analyze the influences of concentration of PEG-GNRand laser output power on the inhibition effects. The results show that the PEG-GNRhas good antibacterial properties for both Gram positive and negative bacterium under the radiation of near-IRlaser. The concentration of PEG-GNRand laser output power determined antibacterial effects of the PEG-GNR. The preliminary investigation on the antibacterial mechanism was explored by studying of bacteria apoptosis status with fluorescence microscope and transmission electronic microscope, suggesting that the effective absorption of the PEG-GNRby the cells is one of the key factors in the process of photothermal antibiosis.
Synthesis of White LED Eu3+/Eu3+, Tb3+ Co-doped NaLu(MO4)(M=W, Mo) Phosphor via Microemulsion Method
2015, (2): 222-228
doi: 10.11862/CJIC.2015.053
Abstract:
8%Eu3+/y%Eu3+,5%Tb3+(y=1, 3, 5, 7, 9)codoped NaLu(WO4)2-x(MoO4)x (x=0, 0.5, 1.0, 1.5, 2.0) phosphor were prepared via microemulsion method at room temperature. X-ray diffraction (XRD), scanning electron microscopy (SEM) and fluorescence spectroscopy were used to characterize the samples. The XRDof as-prepared samples were in agreement with the PDF#27-0729, showing that sample was the scheelite structure, belongs to the tetragonal crystal system. SEMimages showed that the as-prepared particles were shuttle. Particle size was about 110 nm. The critical activator molar concentration (Eu3+) in NaLu(WO4)(MoO4):Eu3+ was 8%. As the Mo content increased, the intensity of emission of Eu3+ activated at wavelength of 394 nm and 466 nm increased and reached a maximum when the relative ratio of nMo/nW was 1:1. The intense red-emission of the tungstomolybdate phosphors at near-UVand blue excitation suggested that the material was a potential candidate for white light emitting diode (WLEDs). This phosphor excited by 268, 394 and 466 nm, exhibited orange-red, yellow and pale yellow respectively, meeting the needs of the different light color. In the systems of NaLu(WO4)(MoO4):y%Eu3+,5%Tb3+(y=1, 3, 5, 7, 9) phosphors, with the increase of the doped concentration of Eu3+(y), the emission color of the co-doped NaLu(WO4)(MoO4) phosphors can be tuned precisely from green (x=0.278, y=0.514)to white (x=0.356, y=0.373), (x=0.385, y=0.313). At the same time, a very efficient energy-transfer from Tb3+ to Eu3+ can be observed.
8%Eu3+/y%Eu3+,5%Tb3+(y=1, 3, 5, 7, 9)codoped NaLu(WO4)2-x(MoO4)x (x=0, 0.5, 1.0, 1.5, 2.0) phosphor were prepared via microemulsion method at room temperature. X-ray diffraction (XRD), scanning electron microscopy (SEM) and fluorescence spectroscopy were used to characterize the samples. The XRDof as-prepared samples were in agreement with the PDF#27-0729, showing that sample was the scheelite structure, belongs to the tetragonal crystal system. SEMimages showed that the as-prepared particles were shuttle. Particle size was about 110 nm. The critical activator molar concentration (Eu3+) in NaLu(WO4)(MoO4):Eu3+ was 8%. As the Mo content increased, the intensity of emission of Eu3+ activated at wavelength of 394 nm and 466 nm increased and reached a maximum when the relative ratio of nMo/nW was 1:1. The intense red-emission of the tungstomolybdate phosphors at near-UVand blue excitation suggested that the material was a potential candidate for white light emitting diode (WLEDs). This phosphor excited by 268, 394 and 466 nm, exhibited orange-red, yellow and pale yellow respectively, meeting the needs of the different light color. In the systems of NaLu(WO4)(MoO4):y%Eu3+,5%Tb3+(y=1, 3, 5, 7, 9) phosphors, with the increase of the doped concentration of Eu3+(y), the emission color of the co-doped NaLu(WO4)(MoO4) phosphors can be tuned precisely from green (x=0.278, y=0.514)to white (x=0.356, y=0.373), (x=0.385, y=0.313). At the same time, a very efficient energy-transfer from Tb3+ to Eu3+ can be observed.
2015, (2): 229-236
doi: 10.11862/CJIC.2015.031
Abstract:
Ba1.97Zn1-xMgxSi2O7:0.03Eu and Ba1.97-yZn0.9Mg0.1Si2O7:0.03Eu,yCe3+ phosphors were synthesized in air condition by a high temperature solid-state reaction. Crystallization and optical properties were investigated by using powder X-ray diffraction and fluorescence spectrophotometer, respectively. Under the excitation of ultraviolet (330~360 nm), the emission spectra of these solid-solution phosphors exhibit multi-emission bands peaked at about 360 nm(blue-purple color), 500 nm (green color) and 590~725 nm (red color), the two formers are corresponding to the 4f65d1-4f7 transition of Eu2+, the latter is originated from the 5D0-7FJ (J=1,2,3,4) transitions of Eu3+. The investigated results indicate that part of Eu3+ can be self-reduced to Eu2+ in the matrix and will reach the maximum when x=0.1 mol. When co-doping Ce3+ ions, the luminescent colors of the phosphors Ba1.97-yZn0.9 Mg0.1Si2O7:0.03Eu,yCe3+ can be tunable from green to white to orange area. It had been found that the nominal composition Ba1.96Zn0.9Mg0.1Si2O7:0.03Eu,0.01Ce3+ phosphor provides a white emission (0.323, 0.311) that is very close to the standard white (x=0.33, y=0.33), which shows that it is a potential white phosphor for LED-based UV-chip. The energy transfer processes among rare earths and the luminescent mechanism were discussed.
Ba1.97Zn1-xMgxSi2O7:0.03Eu and Ba1.97-yZn0.9Mg0.1Si2O7:0.03Eu,yCe3+ phosphors were synthesized in air condition by a high temperature solid-state reaction. Crystallization and optical properties were investigated by using powder X-ray diffraction and fluorescence spectrophotometer, respectively. Under the excitation of ultraviolet (330~360 nm), the emission spectra of these solid-solution phosphors exhibit multi-emission bands peaked at about 360 nm(blue-purple color), 500 nm (green color) and 590~725 nm (red color), the two formers are corresponding to the 4f65d1-4f7 transition of Eu2+, the latter is originated from the 5D0-7FJ (J=1,2,3,4) transitions of Eu3+. The investigated results indicate that part of Eu3+ can be self-reduced to Eu2+ in the matrix and will reach the maximum when x=0.1 mol. When co-doping Ce3+ ions, the luminescent colors of the phosphors Ba1.97-yZn0.9 Mg0.1Si2O7:0.03Eu,yCe3+ can be tunable from green to white to orange area. It had been found that the nominal composition Ba1.96Zn0.9Mg0.1Si2O7:0.03Eu,0.01Ce3+ phosphor provides a white emission (0.323, 0.311) that is very close to the standard white (x=0.33, y=0.33), which shows that it is a potential white phosphor for LED-based UV-chip. The energy transfer processes among rare earths and the luminescent mechanism were discussed.
2015, (2): 237-242
doi: 10.11862/CJIC.2015.018
Abstract:
The tri(3,5-dimethylbenzyl)tin chloride (1) and the tetra(m-cyanobenzyl)tin (2) have been synthesized. The crystal structures of the complexes were determined by X-ray diffraction. The crystal of 1 belongs to monoclinic space group P21/m with a=0.58403(4) nm, b=1.96637(14) nm, c=0.85646(5) nm, β=95.138(3)°, V=0.97962(11) nm3, Z=2, Dc=1.735 g·cm-3, μ(Mo Kα)=14.53 cm-1, F(000)=524, R1=0.0437, wR2=0.1232. The crystal 2 belongs to monoclinic space group C2/c with a=1.69221(12) nm, b=1.16741(8) nm, c=1.53941(11) nm, β=116.615(10)°, V=2.7189(3) nm3, Z=4, Dc=1.424 g·cm-3, μ(Mo Kα)=9.67 cm-1, F(000)=1176, R1=0.0175, wR2=0.0461. The tin atoms have a distorted tetrahedral geometry. The stabilities, some frontier molecular orbital energies and composition characteristics of some frontier molecular orbital of the complex have been investigated by quantum chemistry calculation. CCDC: 1030252, 1; 1030251, 2.
The tri(3,5-dimethylbenzyl)tin chloride (1) and the tetra(m-cyanobenzyl)tin (2) have been synthesized. The crystal structures of the complexes were determined by X-ray diffraction. The crystal of 1 belongs to monoclinic space group P21/m with a=0.58403(4) nm, b=1.96637(14) nm, c=0.85646(5) nm, β=95.138(3)°, V=0.97962(11) nm3, Z=2, Dc=1.735 g·cm-3, μ(Mo Kα)=14.53 cm-1, F(000)=524, R1=0.0437, wR2=0.1232. The crystal 2 belongs to monoclinic space group C2/c with a=1.69221(12) nm, b=1.16741(8) nm, c=1.53941(11) nm, β=116.615(10)°, V=2.7189(3) nm3, Z=4, Dc=1.424 g·cm-3, μ(Mo Kα)=9.67 cm-1, F(000)=1176, R1=0.0175, wR2=0.0461. The tin atoms have a distorted tetrahedral geometry. The stabilities, some frontier molecular orbital energies and composition characteristics of some frontier molecular orbital of the complex have been investigated by quantum chemistry calculation. CCDC: 1030252, 1; 1030251, 2.
2015, (2): 243-252
doi: 10.11862/CJIC.2015.008
Abstract:
Nickel-Zinc Ferrite (NixZn1-xFe2O4), Ni0.7Zn0.3Fe2O4/expanded graphite binary composites (NZF/EG) and its ternary composites coated by Polyaniline (NZF/EG/PANI) were prepared by co-precipitation methods and in situ polymerization, respectively. The composition, structure, morphology and electromagnetic properties of the as-prepared samples were characterized by the modern testing technologies. The results showed that the NZFparticles had been embed into the interlamination of EG, and NZF/EGparticles had been well coated by PANI. The magnetic properties of ternary composites weaken with the decrease of magnetic component, while its electrical conductivities related to the natural characteristic and relative content of EGand PANI. In addition, it presented the excellent electrical and magnetic loss property, and its loss properties were better than those of binary composites. The minimum reflection loss values (corresponding vailable bandwidth) of the ternary composites with ωPANIof 70wt% at thicknesses of 1.5, 2.0 and 2.5 mm reached-19.99 dB (5.82 GHz), -20.33 dB (4.08 GHz) and -25.28 dB (3.67 GHz), respectively, presenting the excellent absorbing effect on electromagnetic wave.
Nickel-Zinc Ferrite (NixZn1-xFe2O4), Ni0.7Zn0.3Fe2O4/expanded graphite binary composites (NZF/EG) and its ternary composites coated by Polyaniline (NZF/EG/PANI) were prepared by co-precipitation methods and in situ polymerization, respectively. The composition, structure, morphology and electromagnetic properties of the as-prepared samples were characterized by the modern testing technologies. The results showed that the NZFparticles had been embed into the interlamination of EG, and NZF/EGparticles had been well coated by PANI. The magnetic properties of ternary composites weaken with the decrease of magnetic component, while its electrical conductivities related to the natural characteristic and relative content of EGand PANI. In addition, it presented the excellent electrical and magnetic loss property, and its loss properties were better than those of binary composites. The minimum reflection loss values (corresponding vailable bandwidth) of the ternary composites with ωPANIof 70wt% at thicknesses of 1.5, 2.0 and 2.5 mm reached-19.99 dB (5.82 GHz), -20.33 dB (4.08 GHz) and -25.28 dB (3.67 GHz), respectively, presenting the excellent absorbing effect on electromagnetic wave.
2015, (2): 253-259
doi: 10.11862/CJIC.2015.061
Abstract:
Pure Ca2Zn4Ti16O38:Pr3+ phosphors were synthesized by a hydrothermal assisted method with the molar ratio of nCa:nZn:nTi being 2:4.1:15 and then calcined at 1050 ℃ for 5 h. Crystal phase, microstructure and optical properties were investigated by X-ray diffractometer, scanning electron microscope, UV-Vis spectroscope and luminescence spectrofluorometer. As-synthetic phosphors retain sphere even though firing at 1050 ℃ for 5 h. The optimum Pr3+ concentration was 0.015. Upon excitation with 471 nm, the red emission spectra can be fitting into three peaks using Gaussian method. The three emission peaks located at 605, 620 and 645 nm can be ascribed to 1D2→3H4, 3P0→3H6 and 3P0→3F2 transition of Pr3+, respectively. It is noted that excited at 471 nm, the phosphor displays a super-long afterglow with the emission peak at 614 nm, indicating it being a persistent red long phosphor for visible-light conversion.
Pure Ca2Zn4Ti16O38:Pr3+ phosphors were synthesized by a hydrothermal assisted method with the molar ratio of nCa:nZn:nTi being 2:4.1:15 and then calcined at 1050 ℃ for 5 h. Crystal phase, microstructure and optical properties were investigated by X-ray diffractometer, scanning electron microscope, UV-Vis spectroscope and luminescence spectrofluorometer. As-synthetic phosphors retain sphere even though firing at 1050 ℃ for 5 h. The optimum Pr3+ concentration was 0.015. Upon excitation with 471 nm, the red emission spectra can be fitting into three peaks using Gaussian method. The three emission peaks located at 605, 620 and 645 nm can be ascribed to 1D2→3H4, 3P0→3H6 and 3P0→3F2 transition of Pr3+, respectively. It is noted that excited at 471 nm, the phosphor displays a super-long afterglow with the emission peak at 614 nm, indicating it being a persistent red long phosphor for visible-light conversion.
2015, (2): 260-266
doi: 10.11862/CJIC.2015.016
Abstract:
Ag/ZnO/ZnSe heterostructure nanocatalysts were successfully synthesized via twice immersion method by use of as-prepared Ag nanowire. The structure and morphology of Ag/ZnO/ZnSe heterostructure are investigated by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDS) field emission transmission electron microscopy (FETEM). It is proved that Ag/ZnO/ZnSe heterostructure was consisted with vermicular Ag/ZnOheterostructure coated by ZnSe nanoparticles. Compared with pure Ag nanowire, pure ZnOnanosphere and Ag/ZnOheterostructure, the results showed that the photocatalytic activity of the Ag/ZnO/ZnSe heterostructure was higher than other samples. The enhanced photocatalytic activity could be attributed to the formation of heterostructure, which might improve the separation of photogenerated electron-hole pairs, and decrease recombination probability.
Ag/ZnO/ZnSe heterostructure nanocatalysts were successfully synthesized via twice immersion method by use of as-prepared Ag nanowire. The structure and morphology of Ag/ZnO/ZnSe heterostructure are investigated by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDS) field emission transmission electron microscopy (FETEM). It is proved that Ag/ZnO/ZnSe heterostructure was consisted with vermicular Ag/ZnOheterostructure coated by ZnSe nanoparticles. Compared with pure Ag nanowire, pure ZnOnanosphere and Ag/ZnOheterostructure, the results showed that the photocatalytic activity of the Ag/ZnO/ZnSe heterostructure was higher than other samples. The enhanced photocatalytic activity could be attributed to the formation of heterostructure, which might improve the separation of photogenerated electron-hole pairs, and decrease recombination probability.
2015, (2): 267-274
doi: 10.11862/CJIC.2015.050
Abstract:
Ni-Al2O3, Ni-ZrO2, Ni-La2O3 and Ni-CeO2 catalysts were prepared by solution combustion method using Al(NO3)3, ZrO(NO3)2, La(NO3)3 and Ce(NO3)3 (mixed with Ni(NO3)2 and urea in aqueous solution) as the support precursor, respectively. The COmethanation performances of catalysts were studied in slurry-bed reactor, and the catalysts were characterized by low temperature N2 adsorption-desorption, XRD, SEM, TEM, H2-TPRand H2 chemsorption. The results show that the combustion preparation process of Ni-Al2O3 catalyst using Al(NO3)2 as the precursor is stable for long-duration(up to 23 s) and the catalyst has larger surface area (468 m2·g-1) and metal surface area (10 m2·g-1), smaller Ni particle (3~5 nm), excellent dispersion of Ni, and the catalyst has good catalytic performance, whose COconversion and CH4 selectivity are 94% and 95%, respectively, and no catalyst deactivation is observed in 100h. The preparation process for catalysts using ZrO(NO3)2 and La(NO3)3 as precursors does not show obvious flame and burning time is also shorter (12 s and 5 s), the surface areas, metal surface areas and catalytic performances are lower than that of Ni-Al2O3 while that for the catalyst using Ce(NO3)2 as the precursor has high intensity combustion. The catalyst obtained from Ce(NO3)2 precursor shows lower surface area (22 m2·g-1) and metal surface area (5 m2·g-1), larger Ni particle and worse dispersion of Ni and the worst methanation catalytic performance with COconversion and CH4 selectivity of 41% and 89%, respectively.
Ni-Al2O3, Ni-ZrO2, Ni-La2O3 and Ni-CeO2 catalysts were prepared by solution combustion method using Al(NO3)3, ZrO(NO3)2, La(NO3)3 and Ce(NO3)3 (mixed with Ni(NO3)2 and urea in aqueous solution) as the support precursor, respectively. The COmethanation performances of catalysts were studied in slurry-bed reactor, and the catalysts were characterized by low temperature N2 adsorption-desorption, XRD, SEM, TEM, H2-TPRand H2 chemsorption. The results show that the combustion preparation process of Ni-Al2O3 catalyst using Al(NO3)2 as the precursor is stable for long-duration(up to 23 s) and the catalyst has larger surface area (468 m2·g-1) and metal surface area (10 m2·g-1), smaller Ni particle (3~5 nm), excellent dispersion of Ni, and the catalyst has good catalytic performance, whose COconversion and CH4 selectivity are 94% and 95%, respectively, and no catalyst deactivation is observed in 100h. The preparation process for catalysts using ZrO(NO3)2 and La(NO3)3 as precursors does not show obvious flame and burning time is also shorter (12 s and 5 s), the surface areas, metal surface areas and catalytic performances are lower than that of Ni-Al2O3 while that for the catalyst using Ce(NO3)2 as the precursor has high intensity combustion. The catalyst obtained from Ce(NO3)2 precursor shows lower surface area (22 m2·g-1) and metal surface area (5 m2·g-1), larger Ni particle and worse dispersion of Ni and the worst methanation catalytic performance with COconversion and CH4 selectivity of 41% and 89%, respectively.
2015, (2): 275-281
doi: 10.11862/CJIC.2015.060
Abstract:
The graphene oxide samples with different oxidation degree were prepared by modified Hummers method followed ultrasonic stripping and subsequent processing. The evolution of oxygen-containing functional groups, structure, surface characteristics and electrical conductivity of the samples were carried out by XPS, XRD, AFM, UV-Vis and four-point probe method. The results show that monolayer graphene oxide with the thickness of 1.4 nm can be dispersed in the condition of water phase by ultrasonic. The monolayer graphene oxide reconfigured stacked along the c axis under the action of hydrogen bond force, led the layered condensate with better ordering to form. With the dosage of KMnO4 increasing, the oxygen-containing functional groups in the carbon basal plane keep increasing. Especially the adding of hydroxyl group (C-OH) led the maximal basal spacing along the a-b axis (d100 and d110) to continue increasing, and the values of d100 and d110 reach the maximum with the 3.0 g of KMnO4. The values of d100 and d110 slightly reducing with the 4.0 g of KMnO4 are due to the hydrolysis of partial C-OH. The increasing content of the oxygen-containing functional groups, especially the increasing content of C-O-C, led to the increasing of the energy gap and the conductivity dropping.
The graphene oxide samples with different oxidation degree were prepared by modified Hummers method followed ultrasonic stripping and subsequent processing. The evolution of oxygen-containing functional groups, structure, surface characteristics and electrical conductivity of the samples were carried out by XPS, XRD, AFM, UV-Vis and four-point probe method. The results show that monolayer graphene oxide with the thickness of 1.4 nm can be dispersed in the condition of water phase by ultrasonic. The monolayer graphene oxide reconfigured stacked along the c axis under the action of hydrogen bond force, led the layered condensate with better ordering to form. With the dosage of KMnO4 increasing, the oxygen-containing functional groups in the carbon basal plane keep increasing. Especially the adding of hydroxyl group (C-OH) led the maximal basal spacing along the a-b axis (d100 and d110) to continue increasing, and the values of d100 and d110 reach the maximum with the 3.0 g of KMnO4. The values of d100 and d110 slightly reducing with the 4.0 g of KMnO4 are due to the hydrolysis of partial C-OH. The increasing content of the oxygen-containing functional groups, especially the increasing content of C-O-C, led to the increasing of the energy gap and the conductivity dropping.
2015, (2): 282-290
doi: 10.11862/CJIC.2015.039
Abstract:
Highly ordered mesoporous carbon co-modified with Ni-Ncan be prepared via homogeneous phase route as well as dual-phase route, named as Ni-N-OMC-1 and Ni-N-OMC-2 respectively. Triblock copolymer Pluronic F127 were employed as the template agent, urea as the Nprecursor, NiCl2 as the Ni source and resorcinol-formaldehyde resin as the carbon precursor. X-ray diffraction (XRD), Raman, and transmission electron microscope (TEM) showed that nickel particles dispersed in the carbon matrix in forms of metal nickel, in situ catalyzing the graphitization of amorphous carbon. X-ray photoelectron spectroscopy (XPS) revealed that urea existed in four different Nspecies after heat treatment: sp3 nitrogen atoms bonded to carbon atoms, pyridine-like N, sp3 nitrogen atoms bonded to carbon atoms and quaternary-Natoms. The co-modification of nitrogen and nickel changed the physicochemical properties of carbon matrix, thus making for the loading and dispersing of Pt. Pt nanoparticles deposited on Ni-N-OMC-1 nanocompsite showed excellent electrocatalytic activity. The electrochemical active surface area of hydrogen oxidation was 138.53 m2·g-1 and the limiting current density in ORRwas 5.32 mA·cm-2, which indicated higher electrocatalytic ability than that of the commercial 20% Pt/Ccatalysts (4.49 mA·cm-2, 96.98 m2·g-1).
Highly ordered mesoporous carbon co-modified with Ni-Ncan be prepared via homogeneous phase route as well as dual-phase route, named as Ni-N-OMC-1 and Ni-N-OMC-2 respectively. Triblock copolymer Pluronic F127 were employed as the template agent, urea as the Nprecursor, NiCl2 as the Ni source and resorcinol-formaldehyde resin as the carbon precursor. X-ray diffraction (XRD), Raman, and transmission electron microscope (TEM) showed that nickel particles dispersed in the carbon matrix in forms of metal nickel, in situ catalyzing the graphitization of amorphous carbon. X-ray photoelectron spectroscopy (XPS) revealed that urea existed in four different Nspecies after heat treatment: sp3 nitrogen atoms bonded to carbon atoms, pyridine-like N, sp3 nitrogen atoms bonded to carbon atoms and quaternary-Natoms. The co-modification of nitrogen and nickel changed the physicochemical properties of carbon matrix, thus making for the loading and dispersing of Pt. Pt nanoparticles deposited on Ni-N-OMC-1 nanocompsite showed excellent electrocatalytic activity. The electrochemical active surface area of hydrogen oxidation was 138.53 m2·g-1 and the limiting current density in ORRwas 5.32 mA·cm-2, which indicated higher electrocatalytic ability than that of the commercial 20% Pt/Ccatalysts (4.49 mA·cm-2, 96.98 m2·g-1).
2015, (2): 291-296
doi: 10.11862/CJIC.2015.045
Abstract:
Complexes [Co(L)2(H2O)2(NO3)2] (1) and [Ag(L)2(NO3)] (2) were synthesized (L=4-(3H)-quinazolinone), and were both characterized by single crystal X-ray diffraction analysis and thermogravimetric analysis. Single crystal X-ray diffraction analysis showed that they all belong to triclinic space group, but 1 is six-coordinated and 2 is three-coordinated. Meanwhile, the solid-state fluorescence and anticancer activity of 2 also were studied. CCDC: 1011403, 1; 1011401, 2.
Complexes [Co(L)2(H2O)2(NO3)2] (1) and [Ag(L)2(NO3)] (2) were synthesized (L=4-(3H)-quinazolinone), and were both characterized by single crystal X-ray diffraction analysis and thermogravimetric analysis. Single crystal X-ray diffraction analysis showed that they all belong to triclinic space group, but 1 is six-coordinated and 2 is three-coordinated. Meanwhile, the solid-state fluorescence and anticancer activity of 2 also were studied. CCDC: 1011403, 1; 1011401, 2.
2015, (2): 297-302
doi: 10.11862/CJIC.2015.056
Abstract:
Selective hydrogenolysis of tetrahydrofurfuryl alcohol to 1,5-pentanediol was investigated over Mo modified Rh/AC (Rh-MoOx/AC) catalysts. The Rh-MoOx/ACcatalysts were characterized by TEM, XPSand microcalorimetry of NH3 adsorption. The reaction conditions of the hydrogenolysis were optimized. The results show that the medium strength acid site, provided by MoOx with lower oxidation state by doping molybdenum, is the main factor for improving the catalytic activity. The optimized reaction conditions are catalyst-Rh-MoOx/ACwith molar ratio nMo/nRh of 0.15, reduction temperature of 550 ℃, reaction temperature of 120 ℃, reaction pressure of 8 MPa, reaction time of 10 h and using water as the solvent,. Under these conditions, 64% conversion of tetrahydrofurfuryl alcohol with selectivity of almost 100% toward 1,5-pentanediol is obtained.
Selective hydrogenolysis of tetrahydrofurfuryl alcohol to 1,5-pentanediol was investigated over Mo modified Rh/AC (Rh-MoOx/AC) catalysts. The Rh-MoOx/ACcatalysts were characterized by TEM, XPSand microcalorimetry of NH3 adsorption. The reaction conditions of the hydrogenolysis were optimized. The results show that the medium strength acid site, provided by MoOx with lower oxidation state by doping molybdenum, is the main factor for improving the catalytic activity. The optimized reaction conditions are catalyst-Rh-MoOx/ACwith molar ratio nMo/nRh of 0.15, reduction temperature of 550 ℃, reaction temperature of 120 ℃, reaction pressure of 8 MPa, reaction time of 10 h and using water as the solvent,. Under these conditions, 64% conversion of tetrahydrofurfuryl alcohol with selectivity of almost 100% toward 1,5-pentanediol is obtained.
2015, (2): 303-308
doi: 10.11862/CJIC.2015.015
Abstract:
Two coordination polymers {[Co(1,3-bib)(MPA)(H2O)2]·H2O}n (1) and {[Co2(1,3-bib)2(MPA)2]·5H2O}n (2) based on mixed-ligands, 1,3-bib(1,3-bib =1,3-bis(imidazol-1-yl)benzene) and H2MPA (H2MPA=m-phthalic acid) have been synthesized by mild hydrothermal method and characterized by elemental analysis, IRspectra, TGA, and their crystal structure was determined by single-crystal X-ray diffraction. The coordination polymer 1 crystallizes in the orthorhombic system, space group Pnma and features a 1Dstructure. The coordination polymer 2 crystallizes in the triclinic system, space group P1 and features a dual-core 2Dstructure. Ultraviolet spectroscopy studies revealed that the complexes exhibits ultraviolet absorption in the solid state at room temperature. CCDC: 954321, 1; 1023812, 2.
Two coordination polymers {[Co(1,3-bib)(MPA)(H2O)2]·H2O}n (1) and {[Co2(1,3-bib)2(MPA)2]·5H2O}n (2) based on mixed-ligands, 1,3-bib(1,3-bib =1,3-bis(imidazol-1-yl)benzene) and H2MPA (H2MPA=m-phthalic acid) have been synthesized by mild hydrothermal method and characterized by elemental analysis, IRspectra, TGA, and their crystal structure was determined by single-crystal X-ray diffraction. The coordination polymer 1 crystallizes in the orthorhombic system, space group Pnma and features a 1Dstructure. The coordination polymer 2 crystallizes in the triclinic system, space group P1 and features a dual-core 2Dstructure. Ultraviolet spectroscopy studies revealed that the complexes exhibits ultraviolet absorption in the solid state at room temperature. CCDC: 954321, 1; 1023812, 2.
2015, (2): 309-316
doi: 10.11862/CJIC.2015.055
Abstract:
The Bi2MoO6 crystallites were synthesized by a simple hydrothermal method using (NH4)6Mo7O24·4H2Oand Bi(NO3)3·5H2O as source materials and the effect of the pHvalue was studied on preparation of Bi2MoO6 crystallites. The samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), low temperature nitrogen adsorption-desorption, X-ray photoelectron spectroscopy (XPS) and UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS). The results show that the pHvalue has great influence on the phase composition, morphology and photocatalytic performance of Bi2MoO6 crystallites. Pure Bi2MoO6 is obtained with pHvalues of 1 to 7 and Bi3.64Mo0.36O6.55 is produced when the pHvalue is 9 or 11. The morphology of Bi2MoO6 can be controlled from nanorods, nanosheets to nanoparticles by adjusting the pHvalue. The photocatalytic activity under visible light (λ≥420 nm) and the effect of the pHvalue on the activity were evaluated using photocatalytic degradation of the Rhodamine B (RhB). The results indicate that the highest photocatalytic activity is obtained with the pHvalue of 7. Under visible light irradiation, the degradation rate of 5 mg·L-1 RhBwithin 50 min is 85%.
The Bi2MoO6 crystallites were synthesized by a simple hydrothermal method using (NH4)6Mo7O24·4H2Oand Bi(NO3)3·5H2O as source materials and the effect of the pHvalue was studied on preparation of Bi2MoO6 crystallites. The samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), low temperature nitrogen adsorption-desorption, X-ray photoelectron spectroscopy (XPS) and UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS). The results show that the pHvalue has great influence on the phase composition, morphology and photocatalytic performance of Bi2MoO6 crystallites. Pure Bi2MoO6 is obtained with pHvalues of 1 to 7 and Bi3.64Mo0.36O6.55 is produced when the pHvalue is 9 or 11. The morphology of Bi2MoO6 can be controlled from nanorods, nanosheets to nanoparticles by adjusting the pHvalue. The photocatalytic activity under visible light (λ≥420 nm) and the effect of the pHvalue on the activity were evaluated using photocatalytic degradation of the Rhodamine B (RhB). The results indicate that the highest photocatalytic activity is obtained with the pHvalue of 7. Under visible light irradiation, the degradation rate of 5 mg·L-1 RhBwithin 50 min is 85%.
2015, (2): 317-322
doi: 10.11862/CJIC.2015.044
Abstract:
Ahydrazone Schiff base monohydrate, C17H20N4O2·H2O (1), was synthesized by rection of 4-diethylamino -salicylaldehyde and isoniazide, and its zinc(Ⅱ) coordination polymer, [Zn(L)(Phen)]∞ (2) with double helix structure, was prepared. They have been characterized by elemental analysis, IR, UV-vis spectra and X-ray diffraction single crystal analysis and the fluorescence property of the compounds were investigated, which result showed that the crystal of 1 belongs to the triclinic system,space group P1 with cell parameters a=0.71058(4) nm, b=1.0045(2) nm, c=1.3054(3) nm, α=97.383(11)°, β=102.989(12)°, γ=104.038(10)°, V=8.641(3) nm3, Z=2, Mr=330.39, Dc=1.270 g·cm-3 and the crystal of 2 belongs to the trigonal system,space group P32 with cell parameters a=1.68654(12) nm, b=1.68654(12) nm, c=0.79656(12) nm, V=1.9622(5) nm3, Z=3, Mr=555.93, Dc=1.411 g·cm-3. The compounds 1 and 2 exhibit luminescence with emission maximum at 524 and 535 nm at room temperature, respectively. CCDC: 995121, 1; 994066, 2.
Ahydrazone Schiff base monohydrate, C17H20N4O2·H2O (1), was synthesized by rection of 4-diethylamino -salicylaldehyde and isoniazide, and its zinc(Ⅱ) coordination polymer, [Zn(L)(Phen)]∞ (2) with double helix structure, was prepared. They have been characterized by elemental analysis, IR, UV-vis spectra and X-ray diffraction single crystal analysis and the fluorescence property of the compounds were investigated, which result showed that the crystal of 1 belongs to the triclinic system,space group P1 with cell parameters a=0.71058(4) nm, b=1.0045(2) nm, c=1.3054(3) nm, α=97.383(11)°, β=102.989(12)°, γ=104.038(10)°, V=8.641(3) nm3, Z=2, Mr=330.39, Dc=1.270 g·cm-3 and the crystal of 2 belongs to the trigonal system,space group P32 with cell parameters a=1.68654(12) nm, b=1.68654(12) nm, c=0.79656(12) nm, V=1.9622(5) nm3, Z=3, Mr=555.93, Dc=1.411 g·cm-3. The compounds 1 and 2 exhibit luminescence with emission maximum at 524 and 535 nm at room temperature, respectively. CCDC: 995121, 1; 994066, 2.
2015, (2): 323-328
doi: 10.11862/CJIC.2015.049
Abstract:
Two coordination polymers, [Cu(H2dpcp)2]n (1) and [Mn2(Hdpcp)2(H2O)2·2H2O]n (2) [H3dpcp=5-(2,4-dicarboxylphenyl)-2-carboxylpyridine] have been synthesized under hydrothermal conditions, and the H3dpcp ligand was formed in situ via decarboxylation of the initial 3-(2,4-dicarboxylphenyl)-2,6-dicarboxylpyridine (H4dpdp). Crystal structural analyses indicate that two complexes crystallize in the same monoclinic system, and space group P21/c for complex 1 with a=0.639(13) nm, b=1.835(4) nm, c=1.115(2) nm, β=102.29(3)°, Z=2, and space group C2/c for complex 2 with a=3.126(6) nm, b=1.004(2) nm, c=1.080(2) nm, β=93.73(3)°, Z=4. For 1, Cu(Ⅱ) were bridged by H2dpcp-ligands to form a 1Dchain structure. For 2, Mn(Ⅱ) were linked by Hdpcp2-ligands to form 2Dlayers and further extend to a 3Dstructure through the hydrogen bonding interaction. The negative value of θ shows the existence of antiferromagnetic coupling in 2. CCDC: 1021238, 1; 1021239, 2.
Two coordination polymers, [Cu(H2dpcp)2]n (1) and [Mn2(Hdpcp)2(H2O)2·2H2O]n (2) [H3dpcp=5-(2,4-dicarboxylphenyl)-2-carboxylpyridine] have been synthesized under hydrothermal conditions, and the H3dpcp ligand was formed in situ via decarboxylation of the initial 3-(2,4-dicarboxylphenyl)-2,6-dicarboxylpyridine (H4dpdp). Crystal structural analyses indicate that two complexes crystallize in the same monoclinic system, and space group P21/c for complex 1 with a=0.639(13) nm, b=1.835(4) nm, c=1.115(2) nm, β=102.29(3)°, Z=2, and space group C2/c for complex 2 with a=3.126(6) nm, b=1.004(2) nm, c=1.080(2) nm, β=93.73(3)°, Z=4. For 1, Cu(Ⅱ) were bridged by H2dpcp-ligands to form a 1Dchain structure. For 2, Mn(Ⅱ) were linked by Hdpcp2-ligands to form 2Dlayers and further extend to a 3Dstructure through the hydrogen bonding interaction. The negative value of θ shows the existence of antiferromagnetic coupling in 2. CCDC: 1021238, 1; 1021239, 2.
2015, (2): 329-337
doi: 10.11862/CJIC.2015.042
Abstract:
Ahighly efficient photocatalyst consisting of Ag@AgBr nanoparticles decorated by three-dimensional flower-like hierarchical BiOBr (Ag@AgBr/BiOBr) were synthesized via a facile oil-in-water self-assembly method and applied to decontaminate methylene blue (MB) solution. The photocatalysts were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Energy dispersive X-ray (EDX), UV-Vis diffuse reflectance spectroscopy (DRS) and X-ray photoelectron spectroscopy (XPS), photoluminescence (PL) photocurrent and electrochemical impedance spectra (EIS) measurement. The results showed that the Ag@AgBr nanoparticles possessed average diameters of 20 nm, and were tightly adhered to the surface of the BiOBr. Ag@AgBr/BiOBr composites enhanced the visible light absorption efficiency and efficiently accelerated the separation of the photogenerated charge carriers due to the surface plasmonic resonance. Meanwhile, the Ag@AgBr(15wt%)/BiOBr composite photocatalyst showed the highest degradation rate, and about 90% of MBcould be degraded under visible light irradiation for 30 min. Additionally, studies performed using radical scavengers indicated that ·O2-, h+ and Br0 acted as the main reactive species. On the basis of experimental and theoretical results, the photocatalytic mechanism was proposed.
Ahighly efficient photocatalyst consisting of Ag@AgBr nanoparticles decorated by three-dimensional flower-like hierarchical BiOBr (Ag@AgBr/BiOBr) were synthesized via a facile oil-in-water self-assembly method and applied to decontaminate methylene blue (MB) solution. The photocatalysts were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Energy dispersive X-ray (EDX), UV-Vis diffuse reflectance spectroscopy (DRS) and X-ray photoelectron spectroscopy (XPS), photoluminescence (PL) photocurrent and electrochemical impedance spectra (EIS) measurement. The results showed that the Ag@AgBr nanoparticles possessed average diameters of 20 nm, and were tightly adhered to the surface of the BiOBr. Ag@AgBr/BiOBr composites enhanced the visible light absorption efficiency and efficiently accelerated the separation of the photogenerated charge carriers due to the surface plasmonic resonance. Meanwhile, the Ag@AgBr(15wt%)/BiOBr composite photocatalyst showed the highest degradation rate, and about 90% of MBcould be degraded under visible light irradiation for 30 min. Additionally, studies performed using radical scavengers indicated that ·O2-, h+ and Br0 acted as the main reactive species. On the basis of experimental and theoretical results, the photocatalytic mechanism was proposed.
2015, (2): 338-344
doi: 10.11862/CJIC.2015.057
Abstract:
Two coordination compounds, namely {[Zn2(bptc)(DMF)2(H2O)]·DMF·H2O}n(1) and{[Zn(bte)(bptc)0.5]·DMF·0.5H2O}n(2) (bte=bis(1,2,4-triazol-1-yl)ethane, H4bptc=biphenyl-3,3',5,5'-tetracarboxylic acid), have been synthesized and structurally characterized. 1 features a 3Dframework with PtS-type topology, in which each binuclear second-building-unit (SBU){Zn2(O2CR)4} is linked to four biphenyl connectors (and vice versa). 2 is 2Dlayers, which are interconnected by weak C-H…Ointeractions to lead to 3Dsupramolecular framework. The thermal stability, and fluorescent emission of the two complexes have also been discussed. CCDC:1018691, 1; 1018790, 2.
Two coordination compounds, namely {[Zn2(bptc)(DMF)2(H2O)]·DMF·H2O}n(1) and{[Zn(bte)(bptc)0.5]·DMF·0.5H2O}n(2) (bte=bis(1,2,4-triazol-1-yl)ethane, H4bptc=biphenyl-3,3',5,5'-tetracarboxylic acid), have been synthesized and structurally characterized. 1 features a 3Dframework with PtS-type topology, in which each binuclear second-building-unit (SBU){Zn2(O2CR)4} is linked to four biphenyl connectors (and vice versa). 2 is 2Dlayers, which are interconnected by weak C-H…Ointeractions to lead to 3Dsupramolecular framework. The thermal stability, and fluorescent emission of the two complexes have also been discussed. CCDC:1018691, 1; 1018790, 2.
2015, (2): 345-352
doi: 10.11862/CJIC.2015.058
Abstract:
Reaction of W(CO)6 with (N-methylimidazol-2-yl)bis(3,5-dimethylpyrazol-1-yl)methane (L1), (pyridin-2-yl)bis(3,5-dimethylpyrazol-1-yl)methane (L2) and (pyridin-4-yl)bis(3,5-dimethylpyrazol-1-yl)methane (L3) yielded complexes LW(CO)5 (L=L1 or L3), LW(CO)4 (L=L1, L2 or L3) and LW(CO)3 (L=L1 or L2), respectively. NMR, IRand X-ray structural analyses indicated that these three ligands possessed variable coordination modes in these complexes. L1 and L3 acted as monodentate ligands through the imidazolyl nitrogen or the pyridyl nitrogen in LW(CO)5. A N,N'-chelating bidentate ligand through the imidazolyl nitrogen and one pyrazolyl nitrogen was observed in L1W(CO)4, while L2 and L3 acted as N,N-chelating bidentate ligands through two pyrazolyl nitrogens in L2W(CO)4 and L3W(CO)4. A tridentate N,N,N'-chelating ligand through two pyrazolyl nitrogens and the imidazolyl or 2-pyridyl nitrogen was observed in L1W(CO)3 and L2W(CO)3. The different donor ability of these imidazolyl, pyridyl and pyrazolyl nitrogens possibly plays important roles for the structural diversity. CCDC: 1030402, 2; 1030403, 4; 1030404, 7.
Reaction of W(CO)6 with (N-methylimidazol-2-yl)bis(3,5-dimethylpyrazol-1-yl)methane (L1), (pyridin-2-yl)bis(3,5-dimethylpyrazol-1-yl)methane (L2) and (pyridin-4-yl)bis(3,5-dimethylpyrazol-1-yl)methane (L3) yielded complexes LW(CO)5 (L=L1 or L3), LW(CO)4 (L=L1, L2 or L3) and LW(CO)3 (L=L1 or L2), respectively. NMR, IRand X-ray structural analyses indicated that these three ligands possessed variable coordination modes in these complexes. L1 and L3 acted as monodentate ligands through the imidazolyl nitrogen or the pyridyl nitrogen in LW(CO)5. A N,N'-chelating bidentate ligand through the imidazolyl nitrogen and one pyrazolyl nitrogen was observed in L1W(CO)4, while L2 and L3 acted as N,N-chelating bidentate ligands through two pyrazolyl nitrogens in L2W(CO)4 and L3W(CO)4. A tridentate N,N,N'-chelating ligand through two pyrazolyl nitrogens and the imidazolyl or 2-pyridyl nitrogen was observed in L1W(CO)3 and L2W(CO)3. The different donor ability of these imidazolyl, pyridyl and pyrazolyl nitrogens possibly plays important roles for the structural diversity. CCDC: 1030402, 2; 1030403, 4; 1030404, 7.
2015, (2): 353-360
doi: 10.11862/CJIC.2015.030
Abstract:
1,3-bis(2-formylphenoxy)-2-propanol underwent an ammonium acetate-catalyzed condensation reaction with dicyanomethane to afford the ligand 1,3-bis(2-(2,2-dicyanovinyl)phenoxy)-2-propanol (L). Further, the ligand Lwas made to react with hexafluoroantimonate(AgSbF6) which resulted in the formation of coordination polymer [AgLSbF6]n·nCHCl3 (1). Complex 1 so-obtained was characterized by Fourier transform infrared spectroscopy, elemental analysis, and single crystal X-ray diffraction. The results of X-ray crystallographic analysis indicated that the ligand L crystallized in the monoclinic system, space group P21/n, with the following crystal cell parameters: a=0.9902(11) nm, b=2.181(2) nm, c=1.0122(11) nm, β=109.374(10)°, V=2.062(4) nm3, Z=4, Dc=1.277 g·cm-3, Mr=396.40, μ=0.087 mm-1, F(000)=824, R1=0.0642, and wR2=0.1174 (observed reflections with I >2σ(I)). Complex 1 crystallized in the monoclinic system, space group P21/n, with the following crystallographic data: a=1.27057(11) nm, b=1.45644(13) nm, c=1.66985(14) nm, β=105.643(3)°, V=2.9756(4) nm 3, Z=4, Dc=1.918 g·cm-3, Mr=859.39, μ=1.907 mm-1, F(000)=1664, R1=0.0417, and wR2=0.1032 (observed reflections with I >2σ(I)). In the crystal structure, each ligand L acted as a tetradentate ligand coordinating four Ag(Ⅰ) centers, and each Ag(Ⅰ) was connected to four ligands L, forming two-dimensional layered structure. Moreover, the fluorescent properties of ligand L and complex 1 were investigated in the solid state at room temperature. CCDC:1008802, L; 1008804, 1.
1,3-bis(2-formylphenoxy)-2-propanol underwent an ammonium acetate-catalyzed condensation reaction with dicyanomethane to afford the ligand 1,3-bis(2-(2,2-dicyanovinyl)phenoxy)-2-propanol (L). Further, the ligand Lwas made to react with hexafluoroantimonate(AgSbF6) which resulted in the formation of coordination polymer [AgLSbF6]n·nCHCl3 (1). Complex 1 so-obtained was characterized by Fourier transform infrared spectroscopy, elemental analysis, and single crystal X-ray diffraction. The results of X-ray crystallographic analysis indicated that the ligand L crystallized in the monoclinic system, space group P21/n, with the following crystal cell parameters: a=0.9902(11) nm, b=2.181(2) nm, c=1.0122(11) nm, β=109.374(10)°, V=2.062(4) nm3, Z=4, Dc=1.277 g·cm-3, Mr=396.40, μ=0.087 mm-1, F(000)=824, R1=0.0642, and wR2=0.1174 (observed reflections with I >2σ(I)). Complex 1 crystallized in the monoclinic system, space group P21/n, with the following crystallographic data: a=1.27057(11) nm, b=1.45644(13) nm, c=1.66985(14) nm, β=105.643(3)°, V=2.9756(4) nm 3, Z=4, Dc=1.918 g·cm-3, Mr=859.39, μ=1.907 mm-1, F(000)=1664, R1=0.0417, and wR2=0.1032 (observed reflections with I >2σ(I)). In the crystal structure, each ligand L acted as a tetradentate ligand coordinating four Ag(Ⅰ) centers, and each Ag(Ⅰ) was connected to four ligands L, forming two-dimensional layered structure. Moreover, the fluorescent properties of ligand L and complex 1 were investigated in the solid state at room temperature. CCDC:1008802, L; 1008804, 1.
2015, (2): 361-368
doi: 10.11862/CJIC.2015.019
Abstract:
Abenzothiazole-derived fluorescent probe (YH1) has been synthesized and structurally characterized, and its response to different metal ions has been investigated by spectrometry. The results showed that YH1 exhibited good sensitivity and selectivity to Hg2+. Its interaction with Hg2+ caused the color of its solution changed from blue to colorless under UVirradiation. There was a good linear relationship between the fluorescence intensity of YH1 and the concentration of Hg2+ in the range of 1.4 μmol·L-1 to 8.8 μmol·L-1, and its detection limit for Hg2+ was 0.56 μmol·L-1. Moreover, the cell membrane penetration of YH1 had low cytotoxicity, and it can be applied to image intracellular Hg2+ in living HeLa cells. CCDC: 978108.
Abenzothiazole-derived fluorescent probe (YH1) has been synthesized and structurally characterized, and its response to different metal ions has been investigated by spectrometry. The results showed that YH1 exhibited good sensitivity and selectivity to Hg2+. Its interaction with Hg2+ caused the color of its solution changed from blue to colorless under UVirradiation. There was a good linear relationship between the fluorescence intensity of YH1 and the concentration of Hg2+ in the range of 1.4 μmol·L-1 to 8.8 μmol·L-1, and its detection limit for Hg2+ was 0.56 μmol·L-1. Moreover, the cell membrane penetration of YH1 had low cytotoxicity, and it can be applied to image intracellular Hg2+ in living HeLa cells. CCDC: 978108.
2015, (2): 369-376
doi: 10.11862/CJIC.2015.052
Abstract:
Two coordination polymers [Zn(EBLA)(2,2'-bipy)(H2O)] (1) and [Mn(EBSA)(im)2(H2O)]n (2) were synthesized by hydrothermal and evaporation methods using2,2'-dithiosalicylic acid(EBSA), 2,2'-dipyridyl, imidazole, Zn(NO3)2·6H2O and Mn(NO3)2·4H2O. And the complexes were characterized by elemental analysis, FT-IRand thermogravimetrie analysis (TGA), meanwhile the crystal structures and fluorescence properties of the complex 1 have been studied. In complex 1, 2,2'-dicarboxydiphenylthioether (EBLA) was prepared with 2,2'-dithiosalicylic acid(EBSA) in situ reaction by hydrothermal method. The complex 1 is a dinuclear structure and Zn2+ ion is five-coordination in a distorted square pyramidal geometry; The complex 2 is a one-dimensional infinite linear chain and Mn2+ ion is six-coordination in a distorted octahedral geometry. Hydrogen bonding and π-π interactions are observed in these complexes. CCDC: 998513, 1; 1000616, 2.
Two coordination polymers [Zn(EBLA)(2,2'-bipy)(H2O)] (1) and [Mn(EBSA)(im)2(H2O)]n (2) were synthesized by hydrothermal and evaporation methods using2,2'-dithiosalicylic acid(EBSA), 2,2'-dipyridyl, imidazole, Zn(NO3)2·6H2O and Mn(NO3)2·4H2O. And the complexes were characterized by elemental analysis, FT-IRand thermogravimetrie analysis (TGA), meanwhile the crystal structures and fluorescence properties of the complex 1 have been studied. In complex 1, 2,2'-dicarboxydiphenylthioether (EBLA) was prepared with 2,2'-dithiosalicylic acid(EBSA) in situ reaction by hydrothermal method. The complex 1 is a dinuclear structure and Zn2+ ion is five-coordination in a distorted square pyramidal geometry; The complex 2 is a one-dimensional infinite linear chain and Mn2+ ion is six-coordination in a distorted octahedral geometry. Hydrogen bonding and π-π interactions are observed in these complexes. CCDC: 998513, 1; 1000616, 2.
2015, (2): 377-384
doi: 10.11862/CJIC.2015.047
Abstract:
Two mixed metal-organic coordination polymers, namely {[Zn(4-PTZ)2Cl2]·4H2O}n (1) and {[Cd3(4-PTZ)2(H2O)2Cl6]·3H2O}n (2), were synthesized under hydrothermal condition using5-(4-pyridyl)tetrazolate (4-PTZ), which exhibited diverse coordination modes in two complexes. The two compounds are both crystallized in a monoclinic system. Compound 1: a=0.69175(8) nm; b=2.6688(3) nm; c=1.12266(12) nm; β=93.5350(10)°; V=2.0687(4) nm3; Z=4; R1=0.0318 for I>2σ(I); wR2=0.0829; space group P21/n. Compound 2: a=1.89713(13) nm; b=1.05579(7) nm; c=1.44649(10) nm; β=102.4890(10)°; V=2.8287(3) nm3; Z=4; R1=0.0262 for I>2σ(I); wR2=0.1343; space group C2/c. They are characterized by elemental analysis, IRspectroscopy and TGA. In addition, 1 and 2 have ultraviolet fluorescence emissions in the solid state at room temperature. CCDC: 984430, 1; 984429, 2.
Two mixed metal-organic coordination polymers, namely {[Zn(4-PTZ)2Cl2]·4H2O}n (1) and {[Cd3(4-PTZ)2(H2O)2Cl6]·3H2O}n (2), were synthesized under hydrothermal condition using5-(4-pyridyl)tetrazolate (4-PTZ), which exhibited diverse coordination modes in two complexes. The two compounds are both crystallized in a monoclinic system. Compound 1: a=0.69175(8) nm; b=2.6688(3) nm; c=1.12266(12) nm; β=93.5350(10)°; V=2.0687(4) nm3; Z=4; R1=0.0318 for I>2σ(I); wR2=0.0829; space group P21/n. Compound 2: a=1.89713(13) nm; b=1.05579(7) nm; c=1.44649(10) nm; β=102.4890(10)°; V=2.8287(3) nm3; Z=4; R1=0.0262 for I>2σ(I); wR2=0.1343; space group C2/c. They are characterized by elemental analysis, IRspectroscopy and TGA. In addition, 1 and 2 have ultraviolet fluorescence emissions in the solid state at room temperature. CCDC: 984430, 1; 984429, 2.
2015, (2): 385-398
doi: 10.11862/CJIC.2015.046
Abstract:
Fe2BiTaO7 powder photocatalyst was synthesized by a solid state reaction method. The structural and photocatalytic properties of Fe2BiTaO7 were characterized by XRD, SEM, TEMand UV-Vis diffuse reflectance spectroscopy. The results show that Fe2BiTaO7 crystallizes with the pyrochlore-type structure, cubic crystal system and space group Fd3m. The estimated band gap of Fe2BiTaO7 is 1.72 eV. The photocatalytic degradation of rhodamine Bover Fe2BiTaO7, P25 TiO2, N-doped TiO2 and Bi2InTaO7 was investigated under visible light irradiation. The photocatalytic efficiency with Fe2BiTaO7 catalyst is 1.5 times of N-doped TiO2 catalyst after 140 minutes under visible light irradiation. Fe2BiTaO7 has higher visible-light photocatalytic performance and shows much better activity than that of other photocatalysts. The photocatalytic degradation of rhodamine Bfollows the first-order reaction kinetics, and the first-order rate constant is 0.02293 min-1 for Fe2BiTaO7. The possible photocatalytic degradation pathway of rhodamine Bunder visible light irradiation is suggested. In addition, the photocatalytic degradation of phenol over Fe2BiTaO7 catalyst was investigated under visible light irradiation. Fe2BiTaO7 (visible light) photocatalysis system is confirmed to be suitable for textile industry wastewater treatment.
Fe2BiTaO7 powder photocatalyst was synthesized by a solid state reaction method. The structural and photocatalytic properties of Fe2BiTaO7 were characterized by XRD, SEM, TEMand UV-Vis diffuse reflectance spectroscopy. The results show that Fe2BiTaO7 crystallizes with the pyrochlore-type structure, cubic crystal system and space group Fd3m. The estimated band gap of Fe2BiTaO7 is 1.72 eV. The photocatalytic degradation of rhodamine Bover Fe2BiTaO7, P25 TiO2, N-doped TiO2 and Bi2InTaO7 was investigated under visible light irradiation. The photocatalytic efficiency with Fe2BiTaO7 catalyst is 1.5 times of N-doped TiO2 catalyst after 140 minutes under visible light irradiation. Fe2BiTaO7 has higher visible-light photocatalytic performance and shows much better activity than that of other photocatalysts. The photocatalytic degradation of rhodamine Bfollows the first-order reaction kinetics, and the first-order rate constant is 0.02293 min-1 for Fe2BiTaO7. The possible photocatalytic degradation pathway of rhodamine Bunder visible light irradiation is suggested. In addition, the photocatalytic degradation of phenol over Fe2BiTaO7 catalyst was investigated under visible light irradiation. Fe2BiTaO7 (visible light) photocatalysis system is confirmed to be suitable for textile industry wastewater treatment.
2015, (2): 399-404
doi: 10.11862/CJIC.2015.028
Abstract:
Two copper(Ⅱ) Schiff base complexes [Cu(HL1)ClO4]n (1) and [Cu(HL2)NO3]n (2) (H2L1=N-[(2-oxy-acetate)benzyl]-2-amino ethanol, H2L2=N-salicylidene-3-amino propanol) have been synthesized and explored as photo-Fenton-like catalysts for the degradation of methyl orange (MO) without acidification process. 1 and 2 show 1Dchain motifs and each copper(Ⅱ) ion is six-coordinated in elongated octahedral environment. They are the first 1Dchains of copper(Ⅱ) Schiff base complexes with excellent photocatalytic performance. 1 has advantages on catalyzing efficient MOdegradation through homogeneous photo-Fenton-like reaction. The results indicate that the coordinated ligands have some effect on the photocatalytic activity of copper(Ⅱ) complexes in this study. CCDC: 996021, 1; 996020, 2.
Two copper(Ⅱ) Schiff base complexes [Cu(HL1)ClO4]n (1) and [Cu(HL2)NO3]n (2) (H2L1=N-[(2-oxy-acetate)benzyl]-2-amino ethanol, H2L2=N-salicylidene-3-amino propanol) have been synthesized and explored as photo-Fenton-like catalysts for the degradation of methyl orange (MO) without acidification process. 1 and 2 show 1Dchain motifs and each copper(Ⅱ) ion is six-coordinated in elongated octahedral environment. They are the first 1Dchains of copper(Ⅱ) Schiff base complexes with excellent photocatalytic performance. 1 has advantages on catalyzing efficient MOdegradation through homogeneous photo-Fenton-like reaction. The results indicate that the coordinated ligands have some effect on the photocatalytic activity of copper(Ⅱ) complexes in this study. CCDC: 996021, 1; 996020, 2.
2015, (2): 405-412
doi: 10.11862/CJIC.2015.062
Abstract:
Two complexes [Cu2L2Cl4]·2H2O (1) and [Cd3L2( μ2-Cl)6]n·2nCH3CN (2) were obtained by the reaction of 3-phenoxymethyl-4-(4-methyphenyl)-5-(2-pyridyl)-1,2,4-triazole (L) with Copper(Ⅱ) chloride and cadmium(Ⅱ) chloride respectively. The complexes have been characterized by IR, UV, TGA, powder XRD, elemental analyses and crystal structures. The complexes 1 and 2 crystallize in the triclinic space group P1. Crystallographic studies reveal that 1 has a distorted trigonal bipyramidal [CuN3Cl2] coordination. 2 is a polymeric complex. every repeat unit has three cadmium(Ⅱ) atoms and two different cadmium(Ⅱ) centers. Cd1(Ⅱ) atom possesses a centrosymmetric distorted-octahedral geometry with [CdCl2Cl'2N2], and Cd2(Ⅱ) atom has a distorted-octahedral geometries with [CdCl2Cl'Cl″NN']. CCDC: 1015366, L; 1015367, 1; 1015368, 2.
Two complexes [Cu2L2Cl4]·2H2O (1) and [Cd3L2( μ2-Cl)6]n·2nCH3CN (2) were obtained by the reaction of 3-phenoxymethyl-4-(4-methyphenyl)-5-(2-pyridyl)-1,2,4-triazole (L) with Copper(Ⅱ) chloride and cadmium(Ⅱ) chloride respectively. The complexes have been characterized by IR, UV, TGA, powder XRD, elemental analyses and crystal structures. The complexes 1 and 2 crystallize in the triclinic space group P1. Crystallographic studies reveal that 1 has a distorted trigonal bipyramidal [CuN3Cl2] coordination. 2 is a polymeric complex. every repeat unit has three cadmium(Ⅱ) atoms and two different cadmium(Ⅱ) centers. Cd1(Ⅱ) atom possesses a centrosymmetric distorted-octahedral geometry with [CdCl2Cl'2N2], and Cd2(Ⅱ) atom has a distorted-octahedral geometries with [CdCl2Cl'Cl″NN']. CCDC: 1015366, L; 1015367, 1; 1015368, 2.
2015, (2): 413-419
doi: 10.11862/CJIC.2015.054
Abstract:
1,10-Phenanthroline-5,6-dione based molecules (1 and 2), extended by two thiophene rings at 2 and 9 positions, have been designed and prepared successfully. It is interesting to mention that the study of coordination chemistry of this large steric ligand 2 with some transition-metal ions reveals that only a Cu(Ⅱ) complex 3·H2Ocan be yielded. The conformation of ligand 2 undergoes great alteration after Cu(Ⅱ) ion complexation, where the dihedral angles between the central 1,10-phenanthroline-5,6-dione and its neighboring two thiophene rings are significantly increased from 1.9(2)°/5.6(2)° in 2 and 5.2(6)°/6.5(6)° in 2·CHCl3 to 25.3(3)°/27.2(3)° and 34.9(3)°/38.2(3)° in 3·H2O in order to meet the geometric requirement of four-coordinate Cu(Ⅱ) centre. CCDC: 1013452, 2; 1013453, 2·CHCl3; 1013454, 3·H2O.
1,10-Phenanthroline-5,6-dione based molecules (1 and 2), extended by two thiophene rings at 2 and 9 positions, have been designed and prepared successfully. It is interesting to mention that the study of coordination chemistry of this large steric ligand 2 with some transition-metal ions reveals that only a Cu(Ⅱ) complex 3·H2Ocan be yielded. The conformation of ligand 2 undergoes great alteration after Cu(Ⅱ) ion complexation, where the dihedral angles between the central 1,10-phenanthroline-5,6-dione and its neighboring two thiophene rings are significantly increased from 1.9(2)°/5.6(2)° in 2 and 5.2(6)°/6.5(6)° in 2·CHCl3 to 25.3(3)°/27.2(3)° and 34.9(3)°/38.2(3)° in 3·H2O in order to meet the geometric requirement of four-coordinate Cu(Ⅱ) centre. CCDC: 1013452, 2; 1013453, 2·CHCl3; 1013454, 3·H2O.
2015, (2): 420-428
doi: 10.11862/CJIC.2015.025
Abstract:
Two complexes, [Cd(L1)(HL1)I] (1, HL1=4-(1H-imidazol-4-yl)benzoic acid) and [Co2(L1)4(H2O)8] (2), have been hydrothermally prepared and characterized by single-crystal X-ray diffraction, elemental analysis, IRspectroscopy, photoluminescence property, TGand PXRD. Complex 1 crystallizes in monoclinic, space group P21/c. The L1-ligands link Cd(Ⅱ) atoms to form one-dimensional chains, which are further bridged to form a three-dimensional three-fold interpenetrating α-Po supramolecular polymer by hydrogen bonds. X-ray diffraction analysis revealed three different kinds of Co(Ⅱ) centre mononuclear molecules in the asymmetric unit. The independent mononuclear units are bridged to form a three-dimensional supramolecular polymer by extensive hydrogen bonds interactions. Solid state luminescent property of 1 and sorption property of 2 have been investigated. CCDC: 983657, 1; 1027672, 2.
Two complexes, [Cd(L1)(HL1)I] (1, HL1=4-(1H-imidazol-4-yl)benzoic acid) and [Co2(L1)4(H2O)8] (2), have been hydrothermally prepared and characterized by single-crystal X-ray diffraction, elemental analysis, IRspectroscopy, photoluminescence property, TGand PXRD. Complex 1 crystallizes in monoclinic, space group P21/c. The L1-ligands link Cd(Ⅱ) atoms to form one-dimensional chains, which are further bridged to form a three-dimensional three-fold interpenetrating α-Po supramolecular polymer by hydrogen bonds. X-ray diffraction analysis revealed three different kinds of Co(Ⅱ) centre mononuclear molecules in the asymmetric unit. The independent mononuclear units are bridged to form a three-dimensional supramolecular polymer by extensive hydrogen bonds interactions. Solid state luminescent property of 1 and sorption property of 2 have been investigated. CCDC: 983657, 1; 1027672, 2.
