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2014 Volume 30 Issue 3
2014, 30(3): 473-480
doi: 10.11862/CJIC.2014.122
Abstract:
In the present work, three different cucurbit[6]urils (Q[6]s), the unsubstituted cucurbit[6]uril, 1,3,5-hexamethylcucurbit[6]uril, and symmetric tetramethyl cucurbit[6]uril were selected as the building blocks or the construction of Q[6]s-based coordination polymers. Four compounds based on the Q[6]s-Sr(Ⅱ) complexes were synthesized and characterized by single crystal X-ray diffraction. The crystal structures of the obtained compounds show a common feature of Q[6]s-Sr(Ⅱ) complex-based one dimensional supramolecular chain. In the presence of Cl- anion as a counter ion, the supramolecular chains are typical coordination polymers, while in the presence of NO3- anion as a counter ion, the formation of chain is based on share of coordinated water molecules.CCDC: 653909, 1; 977776, 2; 977778 3; 977777, 4.
In the present work, three different cucurbit[6]urils (Q[6]s), the unsubstituted cucurbit[6]uril, 1,3,5-hexamethylcucurbit[6]uril, and symmetric tetramethyl cucurbit[6]uril were selected as the building blocks or the construction of Q[6]s-based coordination polymers. Four compounds based on the Q[6]s-Sr(Ⅱ) complexes were synthesized and characterized by single crystal X-ray diffraction. The crystal structures of the obtained compounds show a common feature of Q[6]s-Sr(Ⅱ) complex-based one dimensional supramolecular chain. In the presence of Cl- anion as a counter ion, the supramolecular chains are typical coordination polymers, while in the presence of NO3- anion as a counter ion, the formation of chain is based on share of coordinated water molecules.CCDC: 653909, 1; 977776, 2; 977778 3; 977777, 4.
2014, 30(3): 481-486
doi: 10.11862/CJIC.2014.053
Abstract:
TiO2 nanotube supported Pd-Ag catalysts were prepared by the photodeposition and impregnation methods, and the catalystic hydrodechlorination of 1, 2-dichloroethane was investigated. The characterization results of UV-Vis, XRD and XPS showed that given similar Ag loading amount, much higher Ag enrichment was identified on the catalyst prepared by the photodeposition method than by the impregnation method. Accordingly, the catalyst prepared by the photodeposition method exhibit markedly enhanced ethylene selectivity for the hydrodechlorination of 1, 2-dichloroethane. Additionally, the ethylene selectivity was gradually increased with the Ag loading content.
TiO2 nanotube supported Pd-Ag catalysts were prepared by the photodeposition and impregnation methods, and the catalystic hydrodechlorination of 1, 2-dichloroethane was investigated. The characterization results of UV-Vis, XRD and XPS showed that given similar Ag loading amount, much higher Ag enrichment was identified on the catalyst prepared by the photodeposition method than by the impregnation method. Accordingly, the catalyst prepared by the photodeposition method exhibit markedly enhanced ethylene selectivity for the hydrodechlorination of 1, 2-dichloroethane. Additionally, the ethylene selectivity was gradually increased with the Ag loading content.
2014, 30(3): 487-491
doi: 10.11862/CJIC.2014.022
Abstract:
The benzyl dimethyl dodecyl ammonium chloride (BDMDAC) can react with Au(CN)2- to the ionic complex and the compound can be extracted quantitatively. At the same time, It can be enriched highly by solid phase extraction column of reversed phase bonded silica gel. Therefore, we proposed a new method of extracting gold with high enrichment multiple. What enriched by the solid phase extraction column can be eluted by ethanol and the gold in the eluent can be determinated with spectrophotometry. The solid phase extraction column was not easily damaged and it can repeat using. The method is used to extract trace amounts of gold from alkaline cyanide solution and the recovery rate of gold is higher than 98% under the optimal experimental condition.
The benzyl dimethyl dodecyl ammonium chloride (BDMDAC) can react with Au(CN)2- to the ionic complex and the compound can be extracted quantitatively. At the same time, It can be enriched highly by solid phase extraction column of reversed phase bonded silica gel. Therefore, we proposed a new method of extracting gold with high enrichment multiple. What enriched by the solid phase extraction column can be eluted by ethanol and the gold in the eluent can be determinated with spectrophotometry. The solid phase extraction column was not easily damaged and it can repeat using. The method is used to extract trace amounts of gold from alkaline cyanide solution and the recovery rate of gold is higher than 98% under the optimal experimental condition.
2014, 30(3): 492-498
doi: 10.11862/CJIC.2014.057
Abstract:
Silver-modified BiFeO3 nanoparticles were prepared by the sol-gel and photodeposition method. The composites were characterized by FESEM, XRD, XPS, FTIR, UV-Vis/DRS. The effect of the space selective photochemical reaction of ferromagnetic material was investigated on structure, morphology and spectral properties of the composites under light irradiation (λ≥365 nm). The photocatalytic activity of the nanoparticle was tested using rhodamine B as the model reaction under visible-light irradiation. The results show that the modification not only enhances the ultraviolet-visible light response of BiFeO3, but also inhibits the photocorrosion phenomenon of BiFeO3 and improves the stability of the catalyst. The decolorization of rhodamine B is 74% with fresh pure BiFeO3 under visible light within 12 h, however, the decolorization of rhodamine B is about 90% with Ag-BiFeO3 nano-composites within 6 h, and the catalytic performance of Ag-BiFeO3 nano-composites remains almost the same after three cycles.
Silver-modified BiFeO3 nanoparticles were prepared by the sol-gel and photodeposition method. The composites were characterized by FESEM, XRD, XPS, FTIR, UV-Vis/DRS. The effect of the space selective photochemical reaction of ferromagnetic material was investigated on structure, morphology and spectral properties of the composites under light irradiation (λ≥365 nm). The photocatalytic activity of the nanoparticle was tested using rhodamine B as the model reaction under visible-light irradiation. The results show that the modification not only enhances the ultraviolet-visible light response of BiFeO3, but also inhibits the photocorrosion phenomenon of BiFeO3 and improves the stability of the catalyst. The decolorization of rhodamine B is 74% with fresh pure BiFeO3 under visible light within 12 h, however, the decolorization of rhodamine B is about 90% with Ag-BiFeO3 nano-composites within 6 h, and the catalytic performance of Ag-BiFeO3 nano-composites remains almost the same after three cycles.
2014, 30(3): 499-505
doi: 10.11862/CJIC.2014.059
Abstract:
The pyridine substituent vanillins (1a and 1b) were synthesized by still coupling reaction. New unsymmetrical metallo Salophen complexes (3a, 3b and 3c) derived from the condensation of monoamine 2 and pyridine substituent salicylaldehyde in the presence of transition metal ions (Zn2+, Ni2+) as template have been synthesized and characterized. The linear and third-order non-linear optical (two photon absorption, TPA) properties of the complexes have been measured. The emission of (3a and 3c) were in the visible range(504~516 nm) with lifetime between 4.51 to 5.18 ns and quantum yields (Φem) between 4.3% to 5.3%. Decay times with nano-second scale indicate the emissions come from the singlet states. Complexes 3a, 3b and 3c are thermally stable with onset decomposition temperatures (Td) within the range of 333 to 374 ℃. 100 fs laser pulses with the open-aperture Z-scan method was used to measure the TPA cross-sections σ(2) of 3a, 3b and 3c at 800 nm. The σ(2) could reach to 1 403 GM, which is among the largest value known for metalloSalophen complexes to date. In general, these Salophen complexes show moderate fluorescence quantum yields, larger σ(2), low cytotoxicity of zinc complexes and thermal stability. Hence, they are potentially good TPA candidates for tissue imaging work and excitation by NIR or longer-wavelength radiation is possible to increase penetration depth and reduce cell damage.
The pyridine substituent vanillins (1a and 1b) were synthesized by still coupling reaction. New unsymmetrical metallo Salophen complexes (3a, 3b and 3c) derived from the condensation of monoamine 2 and pyridine substituent salicylaldehyde in the presence of transition metal ions (Zn2+, Ni2+) as template have been synthesized and characterized. The linear and third-order non-linear optical (two photon absorption, TPA) properties of the complexes have been measured. The emission of (3a and 3c) were in the visible range(504~516 nm) with lifetime between 4.51 to 5.18 ns and quantum yields (Φem) between 4.3% to 5.3%. Decay times with nano-second scale indicate the emissions come from the singlet states. Complexes 3a, 3b and 3c are thermally stable with onset decomposition temperatures (Td) within the range of 333 to 374 ℃. 100 fs laser pulses with the open-aperture Z-scan method was used to measure the TPA cross-sections σ(2) of 3a, 3b and 3c at 800 nm. The σ(2) could reach to 1 403 GM, which is among the largest value known for metalloSalophen complexes to date. In general, these Salophen complexes show moderate fluorescence quantum yields, larger σ(2), low cytotoxicity of zinc complexes and thermal stability. Hence, they are potentially good TPA candidates for tissue imaging work and excitation by NIR or longer-wavelength radiation is possible to increase penetration depth and reduce cell damage.
2014, 30(3): 506-510
doi: 10.11862/CJIC.2014.050
Abstract:
With the discovery of graphene, two dimensional nanosheets are of great interest due to their novel physics. Among these 2D systems, transition metal sulficid nanosheets with strong correlated nature and ample compositional variations attract more and more attention. Here, by using density functional theory calculations and semi-classic Boltzmann transport equations, we investigated the influence of layer thickness on thermoelectric properties of TiS2 nanosheets, whose courtpart bulk material already shows some promising thermoelectric performance. Our theoretical results show that when the thickness is greater than the critical thickness for electronic quantum confinement and also is smaller than the critical thickness for phonon confinement, the TiS2 nanosheets will have better thermoelectric performance than its counterpart bulk. These finding is helpful for design novel high performance thermoelectric materials.
With the discovery of graphene, two dimensional nanosheets are of great interest due to their novel physics. Among these 2D systems, transition metal sulficid nanosheets with strong correlated nature and ample compositional variations attract more and more attention. Here, by using density functional theory calculations and semi-classic Boltzmann transport equations, we investigated the influence of layer thickness on thermoelectric properties of TiS2 nanosheets, whose courtpart bulk material already shows some promising thermoelectric performance. Our theoretical results show that when the thickness is greater than the critical thickness for electronic quantum confinement and also is smaller than the critical thickness for phonon confinement, the TiS2 nanosheets will have better thermoelectric performance than its counterpart bulk. These finding is helpful for design novel high performance thermoelectric materials.
2014, 30(3): 511-516
doi: 10.11862/CJIC.2014.096
Abstract:
Two coordination polymers, {[Zn3(H2O)7(bpta)2]·5H2O}n (1) (H3bpta=biphenyl-3,3',5-tricarboxylic acid) and {[Zn2Cl(bpta)(bip)2]·2H2O}n (2) [bip=2,6-bis(imidazole-1-yl)pyridine], have been synthesized under hydrothermal conditions and characterized by elemental analysis, FT-IR and single crystal X-ray diffraction. Complex 1 crystallizes in monoclinic system, space group C2/c with a=3.317 1(11) nm, b=1.495 7(5) nm, c=0.695 1(2) nm, β=91.50°, Z=4. Complex 2 crystallizes in monoclinic, space group P2/c with a=1.960 4(4) nm, b=1.035 7(2) nm, c=1.998 7(4) nm, β=101.97(3)°, Z=4. For 1, Zn(Ⅱ) bridged by bpta ligands to form a 1D chain, through the hydrogen bonding interaction between water molecules and carboxylate oxygen atoms, further extend 1D chains into a 3D structure. For 2, Zn(Ⅱ) were linked by bip ligands to form a 1D helical chain, and 1D chains further connected by bpta ligands to form 2D network. In addition, TG and luminescent properties of two complexes have also been investigated.CCDC: 929651, 1; CCDC: 929652, 2.
Two coordination polymers, {[Zn3(H2O)7(bpta)2]·5H2O}n (1) (H3bpta=biphenyl-3,3',5-tricarboxylic acid) and {[Zn2Cl(bpta)(bip)2]·2H2O}n (2) [bip=2,6-bis(imidazole-1-yl)pyridine], have been synthesized under hydrothermal conditions and characterized by elemental analysis, FT-IR and single crystal X-ray diffraction. Complex 1 crystallizes in monoclinic system, space group C2/c with a=3.317 1(11) nm, b=1.495 7(5) nm, c=0.695 1(2) nm, β=91.50°, Z=4. Complex 2 crystallizes in monoclinic, space group P2/c with a=1.960 4(4) nm, b=1.035 7(2) nm, c=1.998 7(4) nm, β=101.97(3)°, Z=4. For 1, Zn(Ⅱ) bridged by bpta ligands to form a 1D chain, through the hydrogen bonding interaction between water molecules and carboxylate oxygen atoms, further extend 1D chains into a 3D structure. For 2, Zn(Ⅱ) were linked by bip ligands to form a 1D helical chain, and 1D chains further connected by bpta ligands to form 2D network. In addition, TG and luminescent properties of two complexes have also been investigated.CCDC: 929651, 1; CCDC: 929652, 2.
2014, 30(3): 517-521
doi: 10.11862/CJIC.2014.117
Abstract:
A 1D cadmium(Ⅱ) coordination polymer, {[Cd2(dhns)(imdz)4]·H2O}n (1), was synthesized by reaction of disodium 3,6-dihydroxy-naphthalene-2,7-disulfonate (Na2H2dhns), imidazole (imdz) and Cd(NO3)2·4H2O in a water-methanol solution, and characterized by elemental analysis, IR, UV, PL, TG and single crystal X -ray diffraction. The complex crystallizes in the monoclinic system, space group C2/m, a=1.245 97(6) nm, b=1.558 33(9) nm, c=1.629 99(10) nm, β=90.258(6)°, V=3.164 8(3) nm3, Z=4, Mr=831.39, Dc=1.745 g·cm-3, μ=1.534 mm-1, F(000)=1 640, R=0.056 4, wR2=0.140 5, S=1.09. In 1, dhns4-ligands bridge two edge shared distorted octahedrons, in which Cd(Ⅱ) ions are in the center, forming 1D chains that are further connected by intermolecular hydrogen-bonding interactions, generating a 3D supramolecular network. CCDC: 939692.
A 1D cadmium(Ⅱ) coordination polymer, {[Cd2(dhns)(imdz)4]·H2O}n (1), was synthesized by reaction of disodium 3,6-dihydroxy-naphthalene-2,7-disulfonate (Na2H2dhns), imidazole (imdz) and Cd(NO3)2·4H2O in a water-methanol solution, and characterized by elemental analysis, IR, UV, PL, TG and single crystal X -ray diffraction. The complex crystallizes in the monoclinic system, space group C2/m, a=1.245 97(6) nm, b=1.558 33(9) nm, c=1.629 99(10) nm, β=90.258(6)°, V=3.164 8(3) nm3, Z=4, Mr=831.39, Dc=1.745 g·cm-3, μ=1.534 mm-1, F(000)=1 640, R=0.056 4, wR2=0.140 5, S=1.09. In 1, dhns4-ligands bridge two edge shared distorted octahedrons, in which Cd(Ⅱ) ions are in the center, forming 1D chains that are further connected by intermolecular hydrogen-bonding interactions, generating a 3D supramolecular network. CCDC: 939692.
2014, 30(3): 522-528
doi: 10.11862/CJIC.2014.111
Abstract:
In this paper, a tetranuclear Mn cluster containing mixed multidentate chelating ligands, Na2[Mn2ⅢMn2Ⅱ(pdmH)2(L)2(N3)2]·2CH3OH·2H2O(1·2CH3OH·2H2O, pdmH2 is 2, 6-pyridinedimethanol and H2L is the production of dehydration condensation between pdmH2 and the gem-diol form of di-2-pyridylketone) has been reported. The obtained complex was fully characterized by X-ray single crystal structural diffraction, IR, elemental analysis and magnetic investigation. The structural analysis indicates that the complex crystallizes in the triclinic system, P1 space group, and in the complex, two Mn2+ ions, two Mn3+ ions and six O atoms from pdmH- or L2- ligands comprise a double-cuboidal core. Magnetic studies indicate that within the cluster, while the magnetic coupling interactions between Mn2+ and Mn3+ are weak antiferromagnetic with the values being J1=-0.89 cm-1 and J2=-1.13 cm-1, the magnetic interaction between Mn3+ ions is slightly strong ferromagnetic with the value being J3=3.20 cm-1. The value of the ground state S is 2, and from ac magnetic susceptibility investigation, the complex do not possess frequency-dependent that the single molecule magnets possess. CCDC: 957203.
In this paper, a tetranuclear Mn cluster containing mixed multidentate chelating ligands, Na2[Mn2ⅢMn2Ⅱ(pdmH)2(L)2(N3)2]·2CH3OH·2H2O(1·2CH3OH·2H2O, pdmH2 is 2, 6-pyridinedimethanol and H2L is the production of dehydration condensation between pdmH2 and the gem-diol form of di-2-pyridylketone) has been reported. The obtained complex was fully characterized by X-ray single crystal structural diffraction, IR, elemental analysis and magnetic investigation. The structural analysis indicates that the complex crystallizes in the triclinic system, P1 space group, and in the complex, two Mn2+ ions, two Mn3+ ions and six O atoms from pdmH- or L2- ligands comprise a double-cuboidal core. Magnetic studies indicate that within the cluster, while the magnetic coupling interactions between Mn2+ and Mn3+ are weak antiferromagnetic with the values being J1=-0.89 cm-1 and J2=-1.13 cm-1, the magnetic interaction between Mn3+ ions is slightly strong ferromagnetic with the value being J3=3.20 cm-1. The value of the ground state S is 2, and from ac magnetic susceptibility investigation, the complex do not possess frequency-dependent that the single molecule magnets possess. CCDC: 957203.
2014, 30(3): 529-535
doi: 10.11862/CJIC.2014.005
Abstract:
LiNi0.8Co0.15Al0.05O2 cathode material was successfully fabricated by co-precipitation. CeO2 coating use by sol-gel and subsequent heat treatment at 600 ℃ for 4 h, the CeO2 surface modification can improve cycle and storage performance. When CeO2 coating is 0.02% (molar ratio), contrast to pristine NCA, the CeO2-coated LiNi0.8Co0.15Al0.05O2 cathode exhibits no decrease in its initial specific capacity of 182.44 mAh·g-1 at 0.2C and excellent capacity retention (85.96% of its initial capacity) between 4.3 and 2.75 V at 0.5C after 100th cycles. The results indicate that the surface treatment should be an effective way to improve cycle properties due to CeO2 inhibit the electrodes and the electrolyte side effects. CeO2 coating layer with highly oxidability can react with the electrolyte in advance to consume trace amounts of water and HF in the electrolyte, and protect the internal active material.
LiNi0.8Co0.15Al0.05O2 cathode material was successfully fabricated by co-precipitation. CeO2 coating use by sol-gel and subsequent heat treatment at 600 ℃ for 4 h, the CeO2 surface modification can improve cycle and storage performance. When CeO2 coating is 0.02% (molar ratio), contrast to pristine NCA, the CeO2-coated LiNi0.8Co0.15Al0.05O2 cathode exhibits no decrease in its initial specific capacity of 182.44 mAh·g-1 at 0.2C and excellent capacity retention (85.96% of its initial capacity) between 4.3 and 2.75 V at 0.5C after 100th cycles. The results indicate that the surface treatment should be an effective way to improve cycle properties due to CeO2 inhibit the electrodes and the electrolyte side effects. CeO2 coating layer with highly oxidability can react with the electrolyte in advance to consume trace amounts of water and HF in the electrolyte, and protect the internal active material.
2014, 30(3): 536-542
doi: 10.11862/CJIC.2014.066
Abstract:
The SrHfO3:Ce ultramicroballoon particles were prepared by unitary alcohol-thermal method, by using Sr(NO3)2 and HfOCl2·8H2O as raw materials, using C2H5OH/H2O as solvent, adding KOH aqueous solution as mineralier and Ce(NO3)3·6H2O as activator. The phase transformation and the morphology of powders were studied by XRD and SEM. The excitation and emission spectra of samples were analyzed by the fluorophotometer. The results show that the powders of SrHfO3:Ce are spherical particles with the size of about 900 nm and good dispersibility under the condition of nSr:nHf=1:1, VC2H5OH:VH2O=4:1, pH=13.5, reacted at 140 ℃ for 4 h. The maximum luminous was obtained at doping of 0.7mol% Ce.
The SrHfO3:Ce ultramicroballoon particles were prepared by unitary alcohol-thermal method, by using Sr(NO3)2 and HfOCl2·8H2O as raw materials, using C2H5OH/H2O as solvent, adding KOH aqueous solution as mineralier and Ce(NO3)3·6H2O as activator. The phase transformation and the morphology of powders were studied by XRD and SEM. The excitation and emission spectra of samples were analyzed by the fluorophotometer. The results show that the powders of SrHfO3:Ce are spherical particles with the size of about 900 nm and good dispersibility under the condition of nSr:nHf=1:1, VC2H5OH:VH2O=4:1, pH=13.5, reacted at 140 ℃ for 4 h. The maximum luminous was obtained at doping of 0.7mol% Ce.
2014, 30(3): 543-549
doi: 10.11862/CJIC.2014.058
Abstract:
With SiO2 acting as an interlinker, multiwalled carbon nanotubes (MWCNTs) were grafted with Ag nanoparticles to form CNTs@SiO2@Ag nancomposites. The microstructure, morphology and composition of the nanocomposites were characterized by TEM, XRD, UV-Vis, XPS. Meanwhile, surface-enhanced Raman scattering (SERS) effect of the nanocomposites was also studied. The results show that Ag nanoparticles effectively improve SERS activity of CNTs, and compared with the pure CNTs, the Raman peak intensities of the nanocomposite increase by 5 times. Furthermore, the SERS activity of the nanocomposite was investigated using Rhodamine 6G (R6G) as the probe molecules. It is found that the SERS signal intensity and quality of the R6G molecules are obviously improved. The high SERS sensitivity of the nanocomposite make it a suitable substrate for noninvasive biomedical detection.
With SiO2 acting as an interlinker, multiwalled carbon nanotubes (MWCNTs) were grafted with Ag nanoparticles to form CNTs@SiO2@Ag nancomposites. The microstructure, morphology and composition of the nanocomposites were characterized by TEM, XRD, UV-Vis, XPS. Meanwhile, surface-enhanced Raman scattering (SERS) effect of the nanocomposites was also studied. The results show that Ag nanoparticles effectively improve SERS activity of CNTs, and compared with the pure CNTs, the Raman peak intensities of the nanocomposite increase by 5 times. Furthermore, the SERS activity of the nanocomposite was investigated using Rhodamine 6G (R6G) as the probe molecules. It is found that the SERS signal intensity and quality of the R6G molecules are obviously improved. The high SERS sensitivity of the nanocomposite make it a suitable substrate for noninvasive biomedical detection.
2014, 30(3): 550-556
doi: 10.11862/CJIC.2014.056
Abstract:
Two cadmium complexes, [CdCl2(EATA)]n(1) and [CdCl2(EATA)2](2), have been synthesized by the reaction between CdCl2·2.5H2O and ethyl 2-amino-4-thiazoleacetate (EATA), and characterized by single-crystal X-ray diffraction, elemental analysis, infrared and photoluminescence spectra. Single crystal X-ray diffraction analysis reveals that, complex 1 crystallizes in monoclinic with space group P21/c, a=1.765 1(5) nm, b=0.927 7(3) nm, c=0.715 0(2) nm, β=92.072(5)°, V=1.170 0(6) nm3, Z=4, R1=0.0363, wR2=0.0762, S=1.082. The title complex 2 also belongs to the monoclinic system, space group Cc with a=1.686 0(3) nm, b=1.663 0(3) nm, c=1.622 0(3) nm, β=105.41(3)°, V=4.384 3(15) nm3, Z=8, R1=0.0215, wR2=0.0483, S=1.021. For either complexes 1 or 2, the central metal ion (Cd2+) displays a distorted six-coordinated octahedral geometry. In complex 1, two adjacent octahedral units are connected by two bridging μ2-Cl- anions, resulting in the formation of one-dimensional chain. These one-dimensional chains are further assembled into a three-dimensional network structure by intermolecular N-H…Cl hydrogen bonds interactions. In complex 2, two-dimensional supramolecular structure is generated via a large number of intermolecular N-H…Cl and C-H…Cl hydrogen bonds. Solid-state photoluminescence spectrum shows that complexes 1 and 2 have similar fluorescence behaviors, and both of which can be attributed to the ligand-to-metal charge transition (LMCT). CCDC: 837325, 1; 837326, 2.
Two cadmium complexes, [CdCl2(EATA)]n(1) and [CdCl2(EATA)2](2), have been synthesized by the reaction between CdCl2·2.5H2O and ethyl 2-amino-4-thiazoleacetate (EATA), and characterized by single-crystal X-ray diffraction, elemental analysis, infrared and photoluminescence spectra. Single crystal X-ray diffraction analysis reveals that, complex 1 crystallizes in monoclinic with space group P21/c, a=1.765 1(5) nm, b=0.927 7(3) nm, c=0.715 0(2) nm, β=92.072(5)°, V=1.170 0(6) nm3, Z=4, R1=0.0363, wR2=0.0762, S=1.082. The title complex 2 also belongs to the monoclinic system, space group Cc with a=1.686 0(3) nm, b=1.663 0(3) nm, c=1.622 0(3) nm, β=105.41(3)°, V=4.384 3(15) nm3, Z=8, R1=0.0215, wR2=0.0483, S=1.021. For either complexes 1 or 2, the central metal ion (Cd2+) displays a distorted six-coordinated octahedral geometry. In complex 1, two adjacent octahedral units are connected by two bridging μ2-Cl- anions, resulting in the formation of one-dimensional chain. These one-dimensional chains are further assembled into a three-dimensional network structure by intermolecular N-H…Cl hydrogen bonds interactions. In complex 2, two-dimensional supramolecular structure is generated via a large number of intermolecular N-H…Cl and C-H…Cl hydrogen bonds. Solid-state photoluminescence spectrum shows that complexes 1 and 2 have similar fluorescence behaviors, and both of which can be attributed to the ligand-to-metal charge transition (LMCT). CCDC: 837325, 1; 837326, 2.
2014, 30(3): 557-562
doi: 10.11862/CJIC.2014.032
Abstract:
A Cu4 cluster compound, Cu4(HL)4·2H2O, (H2L=N-ethoxycarbonyl-N'-o-nitrophenylthiourea), was synthesized in the way of component assembly. Structures and chemical compositions of the cluster compound and its corresponding component were determined by single crystal X-ray diffraction analysis, elemental analysis, FTIR, 1H NMR etc., and its electro-catalysis was also characterized. The experimental results show that the core of the cluster compound is composed by four Cu(I) linked with M-M bonds, and the Cu(I) are coordinated by 4 thiourea ligands with thiocarbonyl sulfur atom and nitrogen atom, respectively. DPV Electro-catalysis shows that the cluster compound is of high O2 catalysis activation. CCDC: 945182, Cu(H2L)2Cl·H2O; 602859, Cu4(HL)4·2H2O.
A Cu4 cluster compound, Cu4(HL)4·2H2O, (H2L=N-ethoxycarbonyl-N'-o-nitrophenylthiourea), was synthesized in the way of component assembly. Structures and chemical compositions of the cluster compound and its corresponding component were determined by single crystal X-ray diffraction analysis, elemental analysis, FTIR, 1H NMR etc., and its electro-catalysis was also characterized. The experimental results show that the core of the cluster compound is composed by four Cu(I) linked with M-M bonds, and the Cu(I) are coordinated by 4 thiourea ligands with thiocarbonyl sulfur atom and nitrogen atom, respectively. DPV Electro-catalysis shows that the cluster compound is of high O2 catalysis activation. CCDC: 945182, Cu(H2L)2Cl·H2O; 602859, Cu4(HL)4·2H2O.
2014, 30(3): 563-572
doi: 10.11862/CJIC.2014.061
Abstract:
Keggin-type polyoxometalate catalysts Mx/nH0.6PW(Zr0.6H0.6PW, Al0.8H0.6PW, Zn1.2H0.6PW, Fe0.8 H0.6PW, Ti0.6H0.6PW and Sn0.6H0.6PW) and Alx/3H3-xPW(AlPW, Al0.8H0.6PW, Al0.5H1.5PW, Al0.3H2.1PW and Al0.1H2.7PW) were prepared using 6 metal salts and phosphotungstate. The prepared catalysts were characterized by FTIR, XRD, DSC/TGA and ICP. Al0.5H1.5PW is the best catalyst based on the catalytic activity screening results. The catalytic oxidation extraction for fuel ultra-deep desulfurization was studied using hydrogen peroxide as the oxidant and MeCN as the extractant. The effect of catalyst dosage, O/S molar ratio, pre-immersion time of the catalyst in H2O2 solution, reaction temperature and initial sulfur content on the desulfurization efficiency was studied. The results show that the sulfur content of simulated diesel is reduced from 350 mg·L-1 to 2.45 mg·L-1 with a desulfurization efficiency of 99.3% at 60 min under the following operating conditions: Al0.5H1.5PW catalyst/simulated diesel, 0.25%(m/m); molar ratio of O/S=10; pre-immersion time of the catalyst in H2O2 solution, 8 min; reaction temperature, 60 ℃; initial sulfur content, 350 mg·L-1. The efficiency of the oxidation extraction desulfurization is much higher than that of extraction only (45.3% higher). Moreover, very good desulfurization efficiency is obtained for real gasoline and diesel catalytic oxidative desulfurization over Al0.5H1.5PW catalyst, and the desulfurization efficiency is not reduced obviously after 5 cycles.
Keggin-type polyoxometalate catalysts Mx/nH0.6PW(Zr0.6H0.6PW, Al0.8H0.6PW, Zn1.2H0.6PW, Fe0.8 H0.6PW, Ti0.6H0.6PW and Sn0.6H0.6PW) and Alx/3H3-xPW(AlPW, Al0.8H0.6PW, Al0.5H1.5PW, Al0.3H2.1PW and Al0.1H2.7PW) were prepared using 6 metal salts and phosphotungstate. The prepared catalysts were characterized by FTIR, XRD, DSC/TGA and ICP. Al0.5H1.5PW is the best catalyst based on the catalytic activity screening results. The catalytic oxidation extraction for fuel ultra-deep desulfurization was studied using hydrogen peroxide as the oxidant and MeCN as the extractant. The effect of catalyst dosage, O/S molar ratio, pre-immersion time of the catalyst in H2O2 solution, reaction temperature and initial sulfur content on the desulfurization efficiency was studied. The results show that the sulfur content of simulated diesel is reduced from 350 mg·L-1 to 2.45 mg·L-1 with a desulfurization efficiency of 99.3% at 60 min under the following operating conditions: Al0.5H1.5PW catalyst/simulated diesel, 0.25%(m/m); molar ratio of O/S=10; pre-immersion time of the catalyst in H2O2 solution, 8 min; reaction temperature, 60 ℃; initial sulfur content, 350 mg·L-1. The efficiency of the oxidation extraction desulfurization is much higher than that of extraction only (45.3% higher). Moreover, very good desulfurization efficiency is obtained for real gasoline and diesel catalytic oxidative desulfurization over Al0.5H1.5PW catalyst, and the desulfurization efficiency is not reduced obviously after 5 cycles.
2014, 30(3): 573-578
doi: 10.11862/CJIC.2014.026
Abstract:
By using hydrogen titanate nanotubes as support and titanium sol containing copper(Ⅱ) acetate as modifying agent, CuO modified-TiO2 nanotubes (CuO/TiO2 NTs) with high thermal stability were prepared by impregnation method. The prepared materials were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS), N2 absorption-desorption (BET), and temperature programed desorption (TPD). The catalytic performances for CO oxidation of the obtained samples were evaluated. Obtained results show that not only is the copper component coated on the nanotubes, but also the thermal stability of the tubular support is improved after the impregnation process. The influences of support form, atomic ratio of Cu to Ti, and calcination temperature on the catalytic performance of the prepared catalysts were also investigated. Obtained results also indicate that the CuO/TiO2 NTs (nCu:nTi=1:5) calcined at 400 ℃ exhibit the best catalytic performance.
By using hydrogen titanate nanotubes as support and titanium sol containing copper(Ⅱ) acetate as modifying agent, CuO modified-TiO2 nanotubes (CuO/TiO2 NTs) with high thermal stability were prepared by impregnation method. The prepared materials were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS), N2 absorption-desorption (BET), and temperature programed desorption (TPD). The catalytic performances for CO oxidation of the obtained samples were evaluated. Obtained results show that not only is the copper component coated on the nanotubes, but also the thermal stability of the tubular support is improved after the impregnation process. The influences of support form, atomic ratio of Cu to Ti, and calcination temperature on the catalytic performance of the prepared catalysts were also investigated. Obtained results also indicate that the CuO/TiO2 NTs (nCu:nTi=1:5) calcined at 400 ℃ exhibit the best catalytic performance.
2014, 30(3): 579-584
doi: 10.11862/CJIC.2014.009
Abstract:
A series of Zeolitic Imidazolate Framework-8(ZIF-8) samples was synthesized in a mixture of methanol and aqueous ammonia, methanol, and DMF, respectively (denoted as ZIF-8(NH4OH), ZIF-8(MeOH) and ZIF-8(DMF)) with 2-methylimidazole as an organic linker and Zn(OH)2 or Zn(NO3)2·6H2O as Zn source. The physicochemical properties and catalytic performance of the samples were characterized by XRD, FTIR, N2 adsorption, SEM, TPD and Knoevenagel reaction. The results show that ZIF-8 can be synthesized by three methods and the samples synthesized by different methods have similar morphologies, but different particle sizes and acid-base properties. ZIF-8(MeOH) has much narrower particle size distribution, smaller particle size as well as more acid and base centers than those of ZIF-8(NH4OH) and ZIF-8(DMF). The ZIF-8 samples exhibit significant difference in catalytic performance for Knoevenagel reaction from benzaldehyde and malononitrile. ZIF-8(MeOH) is the most effective catalyst. The higher catalytic activity of the ZIF-8(MeOH) sample is closely related with its higher external surface area and acid-base properties.
A series of Zeolitic Imidazolate Framework-8(ZIF-8) samples was synthesized in a mixture of methanol and aqueous ammonia, methanol, and DMF, respectively (denoted as ZIF-8(NH4OH), ZIF-8(MeOH) and ZIF-8(DMF)) with 2-methylimidazole as an organic linker and Zn(OH)2 or Zn(NO3)2·6H2O as Zn source. The physicochemical properties and catalytic performance of the samples were characterized by XRD, FTIR, N2 adsorption, SEM, TPD and Knoevenagel reaction. The results show that ZIF-8 can be synthesized by three methods and the samples synthesized by different methods have similar morphologies, but different particle sizes and acid-base properties. ZIF-8(MeOH) has much narrower particle size distribution, smaller particle size as well as more acid and base centers than those of ZIF-8(NH4OH) and ZIF-8(DMF). The ZIF-8 samples exhibit significant difference in catalytic performance for Knoevenagel reaction from benzaldehyde and malononitrile. ZIF-8(MeOH) is the most effective catalyst. The higher catalytic activity of the ZIF-8(MeOH) sample is closely related with its higher external surface area and acid-base properties.
2014, 30(3): 585-590
doi: 10.11862/CJIC.2014.095
Abstract:
A novel Schiff base ligand which called 2-furancarbaldehyde-4-methoxy-benzoylhydrazone (HL) has been synthesized from 2-furancarbaldehyde and 4-methoxybenzoylhydrazine. Two different configurations metal complexes of the ligand which named NiL2 and Mn(HL)2Cl2 were also synthesized in mixed solvent of ethanol and acetone with Ni(NO3)2·6H2O and MnCl2·4H2O. The single crystal of HL, NiL2 and Mn(HL)2Cl2 were obtained through solvent evaporation method. Complex NiL2 and Mn(HL)2Cl2 were characterized by using X-ray, EA, FT-IR and 1H NMR methods. Structure analysis shows the ligand HL crystallizes in the trigonal system, space group R3 with a=2.442(2) nm, b=2.442(2) nm, c=1.135 4(10) nm parameters, γ=120°, Z=18. Complex NiL2 and Mn(HL)2Cl2 crystall-izes both in the monoclinic system. Complex NiL2 has square planar configuration in space group P21/n with a=1.206 7(8) nm, b=0.577 4(4) nm, c=1.841 8(13) nm parameters, β=107.122(11)°, Z=2; Complex Mn(HL)2Cl2 has distorted octahedral configuration in space group P21/c with a=0.915 5(4) nm, b=0.721 7(4) nm, c=2.033 6(9) nm parameters, β=96.047(9)°, Z=2. The ligand and its metal complexes have been screened for their antibacterial activities by agar diffusion method. The result shows that complex NiL2 has very significant antibacterial activity to Staphylococcus aureus. CCDC: 926194, HL; 926193, NiL2; 926195, Mn(HL)2Cl2.
A novel Schiff base ligand which called 2-furancarbaldehyde-4-methoxy-benzoylhydrazone (HL) has been synthesized from 2-furancarbaldehyde and 4-methoxybenzoylhydrazine. Two different configurations metal complexes of the ligand which named NiL2 and Mn(HL)2Cl2 were also synthesized in mixed solvent of ethanol and acetone with Ni(NO3)2·6H2O and MnCl2·4H2O. The single crystal of HL, NiL2 and Mn(HL)2Cl2 were obtained through solvent evaporation method. Complex NiL2 and Mn(HL)2Cl2 were characterized by using X-ray, EA, FT-IR and 1H NMR methods. Structure analysis shows the ligand HL crystallizes in the trigonal system, space group R3 with a=2.442(2) nm, b=2.442(2) nm, c=1.135 4(10) nm parameters, γ=120°, Z=18. Complex NiL2 and Mn(HL)2Cl2 crystall-izes both in the monoclinic system. Complex NiL2 has square planar configuration in space group P21/n with a=1.206 7(8) nm, b=0.577 4(4) nm, c=1.841 8(13) nm parameters, β=107.122(11)°, Z=2; Complex Mn(HL)2Cl2 has distorted octahedral configuration in space group P21/c with a=0.915 5(4) nm, b=0.721 7(4) nm, c=2.033 6(9) nm parameters, β=96.047(9)°, Z=2. The ligand and its metal complexes have been screened for their antibacterial activities by agar diffusion method. The result shows that complex NiL2 has very significant antibacterial activity to Staphylococcus aureus. CCDC: 926194, HL; 926193, NiL2; 926195, Mn(HL)2Cl2.
2014, 30(3): 591-596
doi: 10.11862/CJIC.2014.003
Abstract:
Reaction of CdCl2 with mixed-ligands of imidazole-4,5-dicarboxylic acid (H3IDC) and 1,4-benzenedicar-boxylic acid (H2BDC) under hydrothermal condition, yielded a new 3D cadmium(Ⅱ) coordination polymer of[Cd2(HIDC)(BDC)(H2O)]n(1), which was structurally characterized by elemental analysis, infrared spectroscopy, powder X-ray diffraction, and single-crystal X-ray diffraction. The result of single-crystal X-ray diffraction analysis reveals that complex 1 crystallizes in the monoclinic crystal system with P21/n space group, a=0.884 34(2) nm, b=1.577 50(3) nm, c=1.071 58(3) nm, β=97.227(2), V=1.483 03(6) nm3, Z=4, Dc=2.513 g·cm-3, F(000)=1 072, the final R1=0.031 5, wR2=0.053 1 for 2 674 observed reflections with I>2σ(I). In complex 1, the interconnection of Cd(Ⅱ) ions by carboxylate oxygen atoms from BDC2- ligands result in an infinite 1D polymeric chain of {[Cd2(CO2)]2(CO2)2}n along a axis. The polymeric chains are further connected by HIDC2- and BDC2- bridging ligands to form a complicated 3D metal-organic framework architecture. Furthermore, its thermal stability and luminescent property at room temperature in the solid state were also investigated. CCDC: 923674.
Reaction of CdCl2 with mixed-ligands of imidazole-4,5-dicarboxylic acid (H3IDC) and 1,4-benzenedicar-boxylic acid (H2BDC) under hydrothermal condition, yielded a new 3D cadmium(Ⅱ) coordination polymer of[Cd2(HIDC)(BDC)(H2O)]n(1), which was structurally characterized by elemental analysis, infrared spectroscopy, powder X-ray diffraction, and single-crystal X-ray diffraction. The result of single-crystal X-ray diffraction analysis reveals that complex 1 crystallizes in the monoclinic crystal system with P21/n space group, a=0.884 34(2) nm, b=1.577 50(3) nm, c=1.071 58(3) nm, β=97.227(2), V=1.483 03(6) nm3, Z=4, Dc=2.513 g·cm-3, F(000)=1 072, the final R1=0.031 5, wR2=0.053 1 for 2 674 observed reflections with I>2σ(I). In complex 1, the interconnection of Cd(Ⅱ) ions by carboxylate oxygen atoms from BDC2- ligands result in an infinite 1D polymeric chain of {[Cd2(CO2)]2(CO2)2}n along a axis. The polymeric chains are further connected by HIDC2- and BDC2- bridging ligands to form a complicated 3D metal-organic framework architecture. Furthermore, its thermal stability and luminescent property at room temperature in the solid state were also investigated. CCDC: 923674.
2014, 30(3): 597-602
doi: 10.11862/CJIC.2014.088
Abstract:
GaN micron films were prepared on Si(100) substrate with Al, Ni and Fe metal buffer layer by chemical vapor deposition method (CVD), in which metal Ga and NH3 as source materials. The GaN micron films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), photoluminescence (PL) and hall effect measurement system (HMS-3000) etc. The results indicate that all samples are hexagonal wurtzite structure, show strong near-band-edge UV emission peaks and red light emission peaks with center wavelength of 672 nm. The electrical properties of samples are quite different. Finally the possible formation mechanisms of GaN micron films were proposed.
GaN micron films were prepared on Si(100) substrate with Al, Ni and Fe metal buffer layer by chemical vapor deposition method (CVD), in which metal Ga and NH3 as source materials. The GaN micron films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), photoluminescence (PL) and hall effect measurement system (HMS-3000) etc. The results indicate that all samples are hexagonal wurtzite structure, show strong near-band-edge UV emission peaks and red light emission peaks with center wavelength of 672 nm. The electrical properties of samples are quite different. Finally the possible formation mechanisms of GaN micron films were proposed.
2014, 30(3): 603-608
doi: 10.11862/CJIC.2014.103
Abstract:
The SiO2 composite aerogels enhanced by the self growing nano-fibers were prepared using sol-gel techniques and supercritical fluid drying, and converted to the high-strength composite aerogels after 1 200 ℃ high temperature heat treatment process. The structures and properties of composite aerogels were analyzed by means of SEM, TEM, XRD, TG, BET, and the compressive strengths and the true density were also measured. The experimental results showed that the as-synthesized ZrOX/SiO2 composite aerogels exhibited well-proportioned multihole network structure, and the Zirconium oxide nano-fibers alternated in the composite aerogels by the chemical bond. The mechanical strength and the insulation properties were improved evidently. The specific surface area, the compressive strengths and the true density of the ZrOX/SiO2 composite aerogels after 1 200 ℃ high temperature heat treatment process were 827.22 m2·g-1, 9.68 MPa, 0.23 g·cm-3, respectively.
The SiO2 composite aerogels enhanced by the self growing nano-fibers were prepared using sol-gel techniques and supercritical fluid drying, and converted to the high-strength composite aerogels after 1 200 ℃ high temperature heat treatment process. The structures and properties of composite aerogels were analyzed by means of SEM, TEM, XRD, TG, BET, and the compressive strengths and the true density were also measured. The experimental results showed that the as-synthesized ZrOX/SiO2 composite aerogels exhibited well-proportioned multihole network structure, and the Zirconium oxide nano-fibers alternated in the composite aerogels by the chemical bond. The mechanical strength and the insulation properties were improved evidently. The specific surface area, the compressive strengths and the true density of the ZrOX/SiO2 composite aerogels after 1 200 ℃ high temperature heat treatment process were 827.22 m2·g-1, 9.68 MPa, 0.23 g·cm-3, respectively.
2014, 30(3): 609-614
doi: 10.11862/CJIC.2014.114
Abstract:
Graphene/nickel oxide composites (RG/NiO) were prepared by microwave-assisted in-situ synthesis of nano-particles NiO on the defects of thermal expansion graphene (RG). The structure, morphology and the NiO content of the composites were characterized by X-ray diffraction (XRD), Raman spectra (Raman), Fourier transform infrared (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermogravimetry-differential thermal analysis (TGA-DSC). The results show that the number of high-defects graphene layers is about 7~8 and the interlay spacing is around 0.35 nm. After hydrothermal reaction and microwave irradiation, the oxidation resistance of graphene became poor obviously. The nanoparticles NiO with an average diameter of 25 nm evenly and densely coated on the graphene sheet. Simultaneously the weight percentage of NiO in the RG/NiO composites is estimated to be 19.8wt%.
Graphene/nickel oxide composites (RG/NiO) were prepared by microwave-assisted in-situ synthesis of nano-particles NiO on the defects of thermal expansion graphene (RG). The structure, morphology and the NiO content of the composites were characterized by X-ray diffraction (XRD), Raman spectra (Raman), Fourier transform infrared (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermogravimetry-differential thermal analysis (TGA-DSC). The results show that the number of high-defects graphene layers is about 7~8 and the interlay spacing is around 0.35 nm. After hydrothermal reaction and microwave irradiation, the oxidation resistance of graphene became poor obviously. The nanoparticles NiO with an average diameter of 25 nm evenly and densely coated on the graphene sheet. Simultaneously the weight percentage of NiO in the RG/NiO composites is estimated to be 19.8wt%.
2014, 30(3): 615-620
doi: 10.11862/CJIC.2014.104
Abstract:
The electronic structure and diffusion barriers of lithium ions in pure LiFePO4 and doped LiFe1-xMoxPO4(x=0.005, 0.01, 0.015, 0.02, and 0.025) have been calculated based on the first-principle density functional theory (DFT). The calculated results show that the LiFe0.99Mo0.01PO4 has the largest interplanar distance of (101) crystal plane, suggesting the widest Li ion diffusion pathway in [010] direction. Pure LiFePO4 has diffusion energy barrier of 4.289 eV for lithium ions, while the LiFe0.99Mo0.01PO4 has lower diffusion energy barrier of 4.274 eV. The calculated diffusion coefficient of LiFe0.99Mo0.01PO4 is 1.79 times as large as that of pure LiFePO4, indicating that Mo doping is beneficial to lithium ion diffusivity of LiFePO4. The intensity of the partial density of states (PDOS) near the bottom of conduction bands (CBs) becomes stronger after doping with Mo. According to the analysis above, Mo doping is beneficial to improve the electronic conductivity and lithium ion diffusivity of LiFePO4. Lithium ion diffusivity plays more important roles than electronic conductivity on improving the electrochemical performance of LiFePO4 by doping with Mo.
The electronic structure and diffusion barriers of lithium ions in pure LiFePO4 and doped LiFe1-xMoxPO4(x=0.005, 0.01, 0.015, 0.02, and 0.025) have been calculated based on the first-principle density functional theory (DFT). The calculated results show that the LiFe0.99Mo0.01PO4 has the largest interplanar distance of (101) crystal plane, suggesting the widest Li ion diffusion pathway in [010] direction. Pure LiFePO4 has diffusion energy barrier of 4.289 eV for lithium ions, while the LiFe0.99Mo0.01PO4 has lower diffusion energy barrier of 4.274 eV. The calculated diffusion coefficient of LiFe0.99Mo0.01PO4 is 1.79 times as large as that of pure LiFePO4, indicating that Mo doping is beneficial to lithium ion diffusivity of LiFePO4. The intensity of the partial density of states (PDOS) near the bottom of conduction bands (CBs) becomes stronger after doping with Mo. According to the analysis above, Mo doping is beneficial to improve the electronic conductivity and lithium ion diffusivity of LiFePO4. Lithium ion diffusivity plays more important roles than electronic conductivity on improving the electrochemical performance of LiFePO4 by doping with Mo.
2014, 30(3): 621-626
doi: 10.11862/CJIC.2014.108
Abstract:
Two copper complexes [CuL41Cl2] (1) and [CuL42Cl2·4H2O] (2) (L1=Uniconazole,L2=Paclobutrazol) were synthesized with triazole pesticides ligands uniconazole and paclobutrazol by solvothermal condition and structurally characterized by element analysis, IR and single crystal X-ray diffraction. Complex 1 is the Triclinic system, space group P1 with a=0.895 6(3) nm, b=1.326 7(4) nm, c=1.491 8(4) nm, α=94.828(3)°, β=97.774(3)°, γ=105.280(3)°, V=1.680 8(9) nm3. Complex 2 is the Triclinic system, space group P1 with a=1.021 89(19) nm, b=1.329(3) nm, c=1.366 4(3) nm, α=81.564(2)°, β=79.508(2)°, γ=79.185(2)°, V=1.785 3(7) nm3. In two complexes, Each six-coordinated Cu(Ⅱ) adopts a distorted octahedral geometry with four nitrogen atoms from triazole ligands and two Cl ions. 1 and 2 was linked into a one dimensional chain by intermolecular hydrogen bonds. Antibacterial activities of complex 1 and 2 increased significantly than corresponding ligands. CCDC: 931901, 1; 932228, 2.
Two copper complexes [CuL41Cl2] (1) and [CuL42Cl2·4H2O] (2) (L1=Uniconazole,L2=Paclobutrazol) were synthesized with triazole pesticides ligands uniconazole and paclobutrazol by solvothermal condition and structurally characterized by element analysis, IR and single crystal X-ray diffraction. Complex 1 is the Triclinic system, space group P1 with a=0.895 6(3) nm, b=1.326 7(4) nm, c=1.491 8(4) nm, α=94.828(3)°, β=97.774(3)°, γ=105.280(3)°, V=1.680 8(9) nm3. Complex 2 is the Triclinic system, space group P1 with a=1.021 89(19) nm, b=1.329(3) nm, c=1.366 4(3) nm, α=81.564(2)°, β=79.508(2)°, γ=79.185(2)°, V=1.785 3(7) nm3. In two complexes, Each six-coordinated Cu(Ⅱ) adopts a distorted octahedral geometry with four nitrogen atoms from triazole ligands and two Cl ions. 1 and 2 was linked into a one dimensional chain by intermolecular hydrogen bonds. Antibacterial activities of complex 1 and 2 increased significantly than corresponding ligands. CCDC: 931901, 1; 932228, 2.
2014, 30(3): 627-632
doi: 10.11862/CJIC.2014.093
Abstract:
SnS2 nanomaterials with different morphologies were synthesized by hydrothermal method using different surfactants and different sulfur sources. The influence of reaction condition on morphology and property was discussed. The structure and composition of the as-prepared SnS2 nanomaterials were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and Brunauer-Emmett-Teller (BET) surface area analysis. The photocatalytic performance of the as-synthesized SnS2 was evaluated by catalytic degradation of Rhodamine B (RhB). The results show that the surfactant and sulfur source play an important role in the structure and morphology of SnS2. When the molar ratio of Sn4+ to Surfactant is 1:1, the samples are all pure hexagonal phase SnS2. The obtained SnS2 nanoplates employing sodium citrate as surfactant and thiourea as sulfur source show the best photocatalytic performance and the larger BET surface area.
SnS2 nanomaterials with different morphologies were synthesized by hydrothermal method using different surfactants and different sulfur sources. The influence of reaction condition on morphology and property was discussed. The structure and composition of the as-prepared SnS2 nanomaterials were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and Brunauer-Emmett-Teller (BET) surface area analysis. The photocatalytic performance of the as-synthesized SnS2 was evaluated by catalytic degradation of Rhodamine B (RhB). The results show that the surfactant and sulfur source play an important role in the structure and morphology of SnS2. When the molar ratio of Sn4+ to Surfactant is 1:1, the samples are all pure hexagonal phase SnS2. The obtained SnS2 nanoplates employing sodium citrate as surfactant and thiourea as sulfur source show the best photocatalytic performance and the larger BET surface area.
2014, 30(3): 633-639
doi: 10.11862/CJIC.2014.107
Abstract:
Two new Zn(Ⅱ) compounds, [Zn(L)2(bpy)] (1) and {[Zn(L)2(bpp)]}n (2) (L=sulfonamide pyrimidine, bpy=2,2'-bipyridine, bpp=1,3-bis(4-pyridyl)propane), have been synthesized and characterized by single crystal X-ray diffraction, powder X-ray diffraction (PXRD), thermal analysis, elemental analysis, IR, UV-Vis and fluorescence. Single crystal X-ray analysis reveals that complex 1 is a mononuclear structure and the Zn(Ⅱ) ion exhibits a tetragonal pyramidal coordination geometry. Complex 2 is a one-dimensional structure and the Zn(Ⅱ) ion is a tetrahedral coordination geometry. Thermal analyses show that complex 1 and 2 have high thermal stability. CCDC: 935049, 1; 935050, 2.
Two new Zn(Ⅱ) compounds, [Zn(L)2(bpy)] (1) and {[Zn(L)2(bpp)]}n (2) (L=sulfonamide pyrimidine, bpy=2,2'-bipyridine, bpp=1,3-bis(4-pyridyl)propane), have been synthesized and characterized by single crystal X-ray diffraction, powder X-ray diffraction (PXRD), thermal analysis, elemental analysis, IR, UV-Vis and fluorescence. Single crystal X-ray analysis reveals that complex 1 is a mononuclear structure and the Zn(Ⅱ) ion exhibits a tetragonal pyramidal coordination geometry. Complex 2 is a one-dimensional structure and the Zn(Ⅱ) ion is a tetrahedral coordination geometry. Thermal analyses show that complex 1 and 2 have high thermal stability. CCDC: 935049, 1; 935050, 2.
2014, 30(3): 640-648
doi: 10.11862/CJIC.2014.106
Abstract:
Two new Schiff base vanadium complexes containing acetohydroxamate ligands, [VⅢL1(HAHA)] (1) and [VⅤOL2(AHA)] (2), where L1 is the dianionic form of N,N'-bis(5-methylsalicylidene)ethane-1, 2-diamine, L2 is the monoanionic form of 2-{[2-(2-hydroxyethylamino)ethylimino]methyl}-6-methylphenol, HAHA and AHA are the mono-anionic and di-anionic forms of acetohydroxamic acid, have been synthesized and characterized by physico-chemical methods and single-crystal X-ray diffraction. The V atoms in the complexes adopt octahedral coordination. Thermal stability and urease inhibitory activities of the complexes were studied. The percent inhibition of complexes 1 and 2 at the concentration of 100 μmol·L-1 on Helicobacter pylori urease are 37.2% and 81.5%, respectively. Complex 2 has IC50 value of 21.5 μmol·L-1. Molecular docking study indicates that there form effective interactions between complex 2 and the active site of the urease. CCDC: 961635, 1; 961636, 2.
Two new Schiff base vanadium complexes containing acetohydroxamate ligands, [VⅢL1(HAHA)] (1) and [VⅤOL2(AHA)] (2), where L1 is the dianionic form of N,N'-bis(5-methylsalicylidene)ethane-1, 2-diamine, L2 is the monoanionic form of 2-{[2-(2-hydroxyethylamino)ethylimino]methyl}-6-methylphenol, HAHA and AHA are the mono-anionic and di-anionic forms of acetohydroxamic acid, have been synthesized and characterized by physico-chemical methods and single-crystal X-ray diffraction. The V atoms in the complexes adopt octahedral coordination. Thermal stability and urease inhibitory activities of the complexes were studied. The percent inhibition of complexes 1 and 2 at the concentration of 100 μmol·L-1 on Helicobacter pylori urease are 37.2% and 81.5%, respectively. Complex 2 has IC50 value of 21.5 μmol·L-1. Molecular docking study indicates that there form effective interactions between complex 2 and the active site of the urease. CCDC: 961635, 1; 961636, 2.
2014, 30(3): 649-653
doi: 10.11862/CJIC.2014.054
Abstract:
The effect of Bi2O3 doping on the structure and dielectric properties of Ag(Nb0.8Ta0.2)O3 ceramics was investigated in this paper. The results of X-ray diffraction (XRD) showed that the doping of Bi2O3 could tend to accelerate the reduction of Ag, which may originate from the substitution of Bi3+ for Ag+. A certain doping amount of Bi2O3 would result in the increase of dielectric constant, and the decrease of dielectric loss of Ag(Nb0.8Ta0.2)O3 ceramics at room temperature, and making temperature coefficient shift for negative direction. The reason for the improvement of dielectric properties was also discussed. When the amount of Bi2O3 was about 3.5wt%, the sample had the best dielectric properties, larger permittivity (ε=672) and smaller dielectric loss (tanδ=7.3×10-4).
The effect of Bi2O3 doping on the structure and dielectric properties of Ag(Nb0.8Ta0.2)O3 ceramics was investigated in this paper. The results of X-ray diffraction (XRD) showed that the doping of Bi2O3 could tend to accelerate the reduction of Ag, which may originate from the substitution of Bi3+ for Ag+. A certain doping amount of Bi2O3 would result in the increase of dielectric constant, and the decrease of dielectric loss of Ag(Nb0.8Ta0.2)O3 ceramics at room temperature, and making temperature coefficient shift for negative direction. The reason for the improvement of dielectric properties was also discussed. When the amount of Bi2O3 was about 3.5wt%, the sample had the best dielectric properties, larger permittivity (ε=672) and smaller dielectric loss (tanδ=7.3×10-4).
2014, 30(3): 654-658
doi: 10.11862/CJIC.2014.014
Abstract:
A new interlocked 2Dachiral coordination polymers {[Zn(BIDPE)(pim)]·(H2O)}n (1) was prepared under hydrothermal conditions based on V-shaped ligand 4,4'-bis(imidazol-1-yl)diphenyl ether (BIDPE) with aliphatic pimelic acid (H2pim). The complex was characterized by IR spectroscopy, TGA, X-ray powder and single-crystal diffraction. It crystallizes in the monoclinic system, space group P21/c. The neighboring Zn(Ⅱ) ions are linked by BIDPE and pim2-anions to form infinitely 2Dchiral layer, two identical 2Dchiral layers interlocked each other to give 2Dchiral+2Dchiral→2Dchiral sheet. The helical directions of adjacent interlocked 2Dchiral sheets are reverse, which stacked in ABAB mode to form 2Dachiral network. In addition, the solid-state photoluminescent property of 1 was also studied. CCDC: 933583.
A new interlocked 2Dachiral coordination polymers {[Zn(BIDPE)(pim)]·(H2O)}n (1) was prepared under hydrothermal conditions based on V-shaped ligand 4,4'-bis(imidazol-1-yl)diphenyl ether (BIDPE) with aliphatic pimelic acid (H2pim). The complex was characterized by IR spectroscopy, TGA, X-ray powder and single-crystal diffraction. It crystallizes in the monoclinic system, space group P21/c. The neighboring Zn(Ⅱ) ions are linked by BIDPE and pim2-anions to form infinitely 2Dchiral layer, two identical 2Dchiral layers interlocked each other to give 2Dchiral+2Dchiral→2Dchiral sheet. The helical directions of adjacent interlocked 2Dchiral sheets are reverse, which stacked in ABAB mode to form 2Dachiral network. In addition, the solid-state photoluminescent property of 1 was also studied. CCDC: 933583.
2014, 30(3): 659-663
doi: 10.11862/CJIC.2014.055
Abstract:
A new complex Mn(L)2(2,2'-bipy)2 (1) with 2-(4-methylbenzoyl)benzoic acid (HL) as a ligand has been synthesized. Crystal data for 1 are as follows: monoclinic, space group P21/c, a=1.719 8(2) nm, b=1.039 80(14) nm, c=2.346 3(3) nm, β=95.732(3)°, V=4.174 8(9) nm3, Dc=1.346 g·cm-3, Z=4, μ(Mo Kα)=0.373 mm-1, F(000)=1 756, final discrepancy factors R1=0.042 3, wR2=0.094 9. In 1, Mn(Ⅱ) ion is coordinated by six atoms to give a distorted octahedral coordination geometry. The electrochemical, luminescence and magnetic properties of 1 are studied. The results show that the electron transfer of 1 is quasi reversible in the electrode reaction corresponding to Mn(Ⅲ)/Mn(Ⅱ), and 1 exhibits one relatively strong fluorescent emission band at around 536~556 nm. In addition, 1 displays antiferromagnetic property in temperatures range of 300~2 K. CCDC: 924900.
A new complex Mn(L)2(2,2'-bipy)2 (1) with 2-(4-methylbenzoyl)benzoic acid (HL) as a ligand has been synthesized. Crystal data for 1 are as follows: monoclinic, space group P21/c, a=1.719 8(2) nm, b=1.039 80(14) nm, c=2.346 3(3) nm, β=95.732(3)°, V=4.174 8(9) nm3, Dc=1.346 g·cm-3, Z=4, μ(Mo Kα)=0.373 mm-1, F(000)=1 756, final discrepancy factors R1=0.042 3, wR2=0.094 9. In 1, Mn(Ⅱ) ion is coordinated by six atoms to give a distorted octahedral coordination geometry. The electrochemical, luminescence and magnetic properties of 1 are studied. The results show that the electron transfer of 1 is quasi reversible in the electrode reaction corresponding to Mn(Ⅲ)/Mn(Ⅱ), and 1 exhibits one relatively strong fluorescent emission band at around 536~556 nm. In addition, 1 displays antiferromagnetic property in temperatures range of 300~2 K. CCDC: 924900.
Syntheses and Structural Characterization of Triorganotin(Ⅳ) Complexes Containing Pamoic Acid Ligand
2014, 30(3): 664-670
doi: 10.11862/CJIC.2014.109
Abstract:
Three organotin(Ⅳ) complexes {[(Ph3Sn)(pa)]·Et3N}n(1)、 (Bu3Sn)2(pa) (2) and [(Me3Sn)2(pa)]·CH2Cl2(3) were synthesized by the reaction of pamoic acid (H2pa, 2, 3-diphenyl-propionic acid) and the corresponding triorganotin chloride R3SnCl (R=Ph, Bu, Me). All the complexes were characterized by elemental analysis, FTIR, NMR (1H, 13C, 119Sn) spectroscopy and single crystal X-ray diffraction. Structural analyses have revealed that the complex 1 is an infinite polymeric chain, in which each tin atom is linked by the bidentate bridging pamoic acid ligand, the center tin atom adopts a five-coordinated distorted trigonal bipyramidal geometry. However, the complexes 2 and 3 show dinuclear tin structure, the center tin atoms adopt four-coordinated distorted tetrahedral geometry. CCDC: 727157, 1; 892440, 2; 732076, 3.
Three organotin(Ⅳ) complexes {[(Ph3Sn)(pa)]·Et3N}n(1)、 (Bu3Sn)2(pa) (2) and [(Me3Sn)2(pa)]·CH2Cl2(3) were synthesized by the reaction of pamoic acid (H2pa, 2, 3-diphenyl-propionic acid) and the corresponding triorganotin chloride R3SnCl (R=Ph, Bu, Me). All the complexes were characterized by elemental analysis, FTIR, NMR (1H, 13C, 119Sn) spectroscopy and single crystal X-ray diffraction. Structural analyses have revealed that the complex 1 is an infinite polymeric chain, in which each tin atom is linked by the bidentate bridging pamoic acid ligand, the center tin atom adopts a five-coordinated distorted trigonal bipyramidal geometry. However, the complexes 2 and 3 show dinuclear tin structure, the center tin atoms adopt four-coordinated distorted tetrahedral geometry. CCDC: 727157, 1; 892440, 2; 732076, 3.
2014, 30(3): 671-676
doi: 10.11862/CJIC.2014.006
Abstract:
[Mn2(O2CC6H11)2(bipy)4](ClO4)2(C6H11CO2H=cyclohexanecarboxylic acid; bipy=2,2'-bipyridine) was synthesized under hydrothermal condition by reactions of Mn(ClO4)2·6H2O, C6H11CO2Na and bipy. In the dinuclear cation [Mn2(O2CC6H11)2(bipy)4]2+, adjacent Mn atoms are linked together through two cyclohexanecarboxylate ligands in syn-anti bridging mode. The molecules are packed together through π-π stacking of the pyridyl groups and weak hydrogen bonding interactions of C-H…O into three-dimensional supramolecular network. Magnetic study indicates there exists weak antiferromagnetic interactions between the adjacent Mn(Ⅱ) ions. CCDC: 748489.
[Mn2(O2CC6H11)2(bipy)4](ClO4)2(C6H11CO2H=cyclohexanecarboxylic acid; bipy=2,2'-bipyridine) was synthesized under hydrothermal condition by reactions of Mn(ClO4)2·6H2O, C6H11CO2Na and bipy. In the dinuclear cation [Mn2(O2CC6H11)2(bipy)4]2+, adjacent Mn atoms are linked together through two cyclohexanecarboxylate ligands in syn-anti bridging mode. The molecules are packed together through π-π stacking of the pyridyl groups and weak hydrogen bonding interactions of C-H…O into three-dimensional supramolecular network. Magnetic study indicates there exists weak antiferromagnetic interactions between the adjacent Mn(Ⅱ) ions. CCDC: 748489.
2014, 30(3): 677-682
doi: 10.11862/CJIC.2014.105
Abstract:
In this study, Eu(Ⅲ) complex nanocrystals had grown on graphene oxide (GO) by π-π stacking. Fourier transform infrared spectroscopy (FTIR), transmission electron morphology (TEM) and X-ray diffraction (XRD) were used to demonstrate the successful growth of Eu(Ⅲ) complex nanocrystals on GO surface. Investigations using fluorescence spectroscopy proved the fluorescence property of the composite and the fluorescence quenching concentration of Eu3+ was 18wt%. Thermogravimetric analysis(TGA) showed that the thermal stability of the composite had been remarkably improved comparing with pure complex.
In this study, Eu(Ⅲ) complex nanocrystals had grown on graphene oxide (GO) by π-π stacking. Fourier transform infrared spectroscopy (FTIR), transmission electron morphology (TEM) and X-ray diffraction (XRD) were used to demonstrate the successful growth of Eu(Ⅲ) complex nanocrystals on GO surface. Investigations using fluorescence spectroscopy proved the fluorescence property of the composite and the fluorescence quenching concentration of Eu3+ was 18wt%. Thermogravimetric analysis(TGA) showed that the thermal stability of the composite had been remarkably improved comparing with pure complex.
2014, 30(3): 683-688
doi: 10.11862/CJIC.2014.119
Abstract:
A new coordination polymer, [Co(oba)(3,4'-Hbpt)]·H2O (H2oba=4,4' -oxybis (benzoic acid) and 3,4'-Hbpt=3-(3-pyridyl)-5-(4'-pyridyl)-1-H-1,2,4-triazole), was prepared in the presence of V-shaped ligand H2oba, rigid ligand 3,4'-Hbpt and cobalt acetate by hydrothermal reactions. The title complex was characterized by single-crystal X-ray diffraction, thermogravimetric analyses, elemental analysis and IR spectroscopy. It belongs to monoclinic system, space group P21/c. In the complex, the Co(Ⅱ) ions are linked by two carboxylate groups from protonated V-shaped oba2- to form an 8-membered ring. Then, oba2-, 3,4'-Hbpt connect adjacent Co(Ⅱ) ions to form a 25-membered ring. Furthermore, the adjacent eight-membered and 25-membered rings are connected by oba2- pillars to form a 2D layer-hole in the structure. In addition, theoretical calculation based on density functional theory (DFT) at B3LYP/6-31G*(d) and 6-31G**(d,p) level is also employed to explicate the most optimized conformation, and investigate stability, frontier orbitals and the optimal configuration of H2oba, which is corresponded with experimental conformation. CCDC: 930887.
A new coordination polymer, [Co(oba)(3,4'-Hbpt)]·H2O (H2oba=4,4' -oxybis (benzoic acid) and 3,4'-Hbpt=3-(3-pyridyl)-5-(4'-pyridyl)-1-H-1,2,4-triazole), was prepared in the presence of V-shaped ligand H2oba, rigid ligand 3,4'-Hbpt and cobalt acetate by hydrothermal reactions. The title complex was characterized by single-crystal X-ray diffraction, thermogravimetric analyses, elemental analysis and IR spectroscopy. It belongs to monoclinic system, space group P21/c. In the complex, the Co(Ⅱ) ions are linked by two carboxylate groups from protonated V-shaped oba2- to form an 8-membered ring. Then, oba2-, 3,4'-Hbpt connect adjacent Co(Ⅱ) ions to form a 25-membered ring. Furthermore, the adjacent eight-membered and 25-membered rings are connected by oba2- pillars to form a 2D layer-hole in the structure. In addition, theoretical calculation based on density functional theory (DFT) at B3LYP/6-31G*(d) and 6-31G**(d,p) level is also employed to explicate the most optimized conformation, and investigate stability, frontier orbitals and the optimal configuration of H2oba, which is corresponded with experimental conformation. CCDC: 930887.
2014, 30(3): 689-695
doi: 10.11862/CJIC.2014.062
Abstract:
The nanocrystallite cuprous oxide (Cu2O) thin films with tunable crystallite size were prepared by a one-step chemical bath deposition (CBD) method, where copper sulfate was used as the copper precursor. The influence of deposition temperature on structure, crystallite size, nucleation site density, film thickness and opto-electronic properties of the thin films was investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and UV-Vis spectroscopy. The results reveal that the crystallite size, film thickness and band gap of Cu2O thin films vary in the range of 33~51 nm, 392~556 nm and 2.47~2.61 eV, respectively, with the deposition temperature change in the range of 60~90 ℃. In addition, the absorption edges of UV-Vis transmittance spectra are blue-shifted apparently with the decrease in crystallite size. Meanwhile, the growth process and the mechanism for the varied nucleation site density and particle size of Cu2O thin films were also discussed.
The nanocrystallite cuprous oxide (Cu2O) thin films with tunable crystallite size were prepared by a one-step chemical bath deposition (CBD) method, where copper sulfate was used as the copper precursor. The influence of deposition temperature on structure, crystallite size, nucleation site density, film thickness and opto-electronic properties of the thin films was investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and UV-Vis spectroscopy. The results reveal that the crystallite size, film thickness and band gap of Cu2O thin films vary in the range of 33~51 nm, 392~556 nm and 2.47~2.61 eV, respectively, with the deposition temperature change in the range of 60~90 ℃. In addition, the absorption edges of UV-Vis transmittance spectra are blue-shifted apparently with the decrease in crystallite size. Meanwhile, the growth process and the mechanism for the varied nucleation site density and particle size of Cu2O thin films were also discussed.
2014, 30(3): 696-704
doi: 10.11862/CJIC.2014.064
Abstract:
Two energetic complexes with 2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105) [Cu4O2 (C4N6O5H2)2(CH3COO)2(DMF)2]·DMF(1)((C4N6O5H2)2-is obtained by losing two protons from LLM-105) and [Co(C4N6O5H3)3]·7H2O(2) ((C4N6O5H3)- is obtained by losing a proton from LLM-105) have been synthesized and structurally characterized using X-ray diffraction. The results reveal that complex 1 belongs to the orthorhombic system (space group Pbca) and complex 2 belongs to the trigonal system (space group R3). Thermal decomposition of LLM-105 and two complexes was examined by DSC and TG-DTG analyses. The kinetic parameters of the exothermic processes of two complexes were studied by the Kissingers and Ozawa-Doyles methods. DSC measurements show that two complexes have decreased the higher thermal decomposition temperature of AP by 117.42 and 71.85 ℃, increased the exothermic quantity of decomposition by 1 916.97 and 1 433.76 J·g-1 respectively, showing good catalytic effects on the thermal decomposition of AP. CCDC: 938305, LLM-105; 911164, 1; 911163, 2.
Two energetic complexes with 2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105) [Cu4O2 (C4N6O5H2)2(CH3COO)2(DMF)2]·DMF(1)((C4N6O5H2)2-is obtained by losing two protons from LLM-105) and [Co(C4N6O5H3)3]·7H2O(2) ((C4N6O5H3)- is obtained by losing a proton from LLM-105) have been synthesized and structurally characterized using X-ray diffraction. The results reveal that complex 1 belongs to the orthorhombic system (space group Pbca) and complex 2 belongs to the trigonal system (space group R3). Thermal decomposition of LLM-105 and two complexes was examined by DSC and TG-DTG analyses. The kinetic parameters of the exothermic processes of two complexes were studied by the Kissingers and Ozawa-Doyles methods. DSC measurements show that two complexes have decreased the higher thermal decomposition temperature of AP by 117.42 and 71.85 ℃, increased the exothermic quantity of decomposition by 1 916.97 and 1 433.76 J·g-1 respectively, showing good catalytic effects on the thermal decomposition of AP. CCDC: 938305, LLM-105; 911164, 1; 911163, 2.
2014, 30(3): 705-709
doi: 10.11862/CJIC.2014.100
Abstract:
A regularly shaped spherical magnesium hydroxide was synthesized through gas-liquid contact method. The structure, morphology, size distribution, and other characteristics of the spherical magnesium hydroxide were characterized by X-ray diffraction, thermogravimetry-derivative thermogravimetry, scanning electron microscopy, and laser particle analysis. Results reveal that the synthesized spherical magnesium hydroxide has good particle dispersion, a particle diameter of D50=7.41 μm and a thermal decomposition temperature above 363.6 ℃. The formation mechanism of the spherical magnesium hydroxide was discussed according to the principle of gas-liquid contact reaction, and the high volatility and easy absorbability characteristics of ammonia.
A regularly shaped spherical magnesium hydroxide was synthesized through gas-liquid contact method. The structure, morphology, size distribution, and other characteristics of the spherical magnesium hydroxide were characterized by X-ray diffraction, thermogravimetry-derivative thermogravimetry, scanning electron microscopy, and laser particle analysis. Results reveal that the synthesized spherical magnesium hydroxide has good particle dispersion, a particle diameter of D50=7.41 μm and a thermal decomposition temperature above 363.6 ℃. The formation mechanism of the spherical magnesium hydroxide was discussed according to the principle of gas-liquid contact reaction, and the high volatility and easy absorbability characteristics of ammonia.
2014, 30(3): 710-716
doi: 10.11862/CJIC.2014.120
Abstract:
An asymmetrical Salamo-type ligand, 5-methoxy-6'-hydroxy-2,2'-[ethylenedioxybis(nitrilomethylidyne)]diphenol (H3L), and its Zn(Ⅱ) complex, [Zn4L2(CH3OH)2(OAc)2], have been synthesized and structurally characterized by X-ray diffraction methods. X-ray crystallographic analyses reveal that the ligand adopts a V-shaped configuration, in which the two benzene rings are approximately perpendicular, making a dihedral angle of 85.71(3)°; the Zn(Ⅱ) complex adopts two different kinds of coordination geometries: trigonal bipyramidal and square pyramidal geometries. Meanwhile, each Zn(Ⅱ) complex molecule links four other molecules to form an infinite 2D layer structure through intermolecular hydrogen bond interactions. CCDC: 954985, H3L; 954984, Zn(Ⅱ) complex.
An asymmetrical Salamo-type ligand, 5-methoxy-6'-hydroxy-2,2'-[ethylenedioxybis(nitrilomethylidyne)]diphenol (H3L), and its Zn(Ⅱ) complex, [Zn4L2(CH3OH)2(OAc)2], have been synthesized and structurally characterized by X-ray diffraction methods. X-ray crystallographic analyses reveal that the ligand adopts a V-shaped configuration, in which the two benzene rings are approximately perpendicular, making a dihedral angle of 85.71(3)°; the Zn(Ⅱ) complex adopts two different kinds of coordination geometries: trigonal bipyramidal and square pyramidal geometries. Meanwhile, each Zn(Ⅱ) complex molecule links four other molecules to form an infinite 2D layer structure through intermolecular hydrogen bond interactions. CCDC: 954985, H3L; 954984, Zn(Ⅱ) complex.
