Two 3D 4-fold interpenetrated metal-organic frameworks, [Mn（L）（bpy）]n （1） and [Cu（HL）（bpy）]n （2）（H3L = 4,4＇,4＇＇-（benzene-1,3,5-triyl-tri（methyleneoxy）） tribenzoic acid, bpy = 4,4′-bipyridine）, we...Two 3D 4-fold interpenetrated metal-organic frameworks, [Mn（L）（bpy）]n （1） and [Cu（HL）（bpy）]n （2）（H3L = 4,4＇,4＇＇-（benzene-1,3,5-triyl-tri（methyleneoxy）） tribenzoic acid, bpy = 4,4′-bipyridine）, were synthesized under hydrothermal conditions, and characterized by element analyses, IR spectra, thermogravimetric analyses, X-ray powder diffraction and magnetic property studies. The single-crystal X-ray analyses revealed that 1 and 2 are homogeneous. 1 crystallizes in monoclinic, space group Cc with a = 26.794（2）, b = 11.6346（10）, c = 21.4614（18） ？, β = 91.570（2）°, V = 6687.9（10） A^3, Z = 8, Mr = 736.59, D = 1.463 g·cm^（-3）, μ = 0.458 mm^-1c, R（int） = 0.0524, F（000） = 3040, the final R = 0.0844 and wR = 0.2266 for 8092 observed reflections（I 〉 2σ（I））. 2 crystallizes in monoclinic, space group Cc with a = 27.609（12）, b = 11.126（10）, c = 21.490（9） ？, β = 92.131（2）°, V = 6597（5） A^3, Z = 8, Mr = 746.21, Dc = 1503 g·cm^（-3）, μ = 0.726 mm^-1, R（int） = 0.0542, F（000） = 3080, the final R =0.0681 and wR = 0.1831 for 6777 observed reflections（I 〉 2σ（I））. Two compounds are 3D [2＋2]-type 4-fold interpenetrated frameworks with（6^3）（6^9.8） hms topology. The magnetic study of compound 2 shows the presence of weak antiferromagnetic interaction between the Cu^Ⅱ ions in 2.展开更多
Ti-HMS materials were prepared by grafting titanocene onto the inner wails of hexagonal mesoporous silica （HMS）. The materials were characterized via powder X-ray diffraction, N2 adsorption-desorption isotherms, dif...Ti-HMS materials were prepared by grafting titanocene onto the inner wails of hexagonal mesoporous silica （HMS）. The materials were characterized via powder X-ray diffraction, N2 adsorption-desorption isotherms, diffuse reflectance UV-Vis spectroscopy, and thermo-gravimetric analysis. The template of HMS was removed by calcination, ethanol-extraction, and ethanol-extraction followed by hydrolysis. The available grafting sites of OH groups depend on the different template removal methods of HMS. Ethanol-extraction followed by hydrolysis favors site-isolated Ti atoms in HMS. The catalytic performances of Ti-HMS materials were tested in the oxidation of 4-tert-butyholuene with aqueous hydrogen peroxide. Ti-HMS prepared from HMS via the processing of ethanol-extraction followed by hydrolysis as support gave a maximum conversion of 7. 5% and a complete selectivity to 4-tert-butyl-benzaldehyde, and showed a higher activity compared with those prepared by calcination and ethanol-extraction.展开更多
基金Supported by the Education Committee of Sichuan Province(12ZA090,13CZ0019 and 14ZB0220)Key Laboratory of Green Catalysis of Sichuan Institutes of High Education(LZJ14201)Sichuan University of Science and Engineering(Y2014018)
文摘Two 3D 4-fold interpenetrated metal-organic frameworks, [Mn（L）（bpy）]n （1） and [Cu（HL）（bpy）]n （2）（H3L = 4,4＇,4＇＇-（benzene-1,3,5-triyl-tri（methyleneoxy）） tribenzoic acid, bpy = 4,4′-bipyridine）, were synthesized under hydrothermal conditions, and characterized by element analyses, IR spectra, thermogravimetric analyses, X-ray powder diffraction and magnetic property studies. The single-crystal X-ray analyses revealed that 1 and 2 are homogeneous. 1 crystallizes in monoclinic, space group Cc with a = 26.794（2）, b = 11.6346（10）, c = 21.4614（18） ？, β = 91.570（2）°, V = 6687.9（10） A^3, Z = 8, Mr = 736.59, D = 1.463 g·cm^（-3）, μ = 0.458 mm^-1c, R（int） = 0.0524, F（000） = 3040, the final R = 0.0844 and wR = 0.2266 for 8092 observed reflections（I 〉 2σ（I））. 2 crystallizes in monoclinic, space group Cc with a = 27.609（12）, b = 11.126（10）, c = 21.490（9） ？, β = 92.131（2）°, V = 6597（5） A^3, Z = 8, Mr = 746.21, Dc = 1503 g·cm^（-3）, μ = 0.726 mm^-1, R（int） = 0.0542, F（000） = 3080, the final R =0.0681 and wR = 0.1831 for 6777 observed reflections（I 〉 2σ（I））. Two compounds are 3D [2＋2]-type 4-fold interpenetrated frameworks with（6^3）（6^9.8） hms topology. The magnetic study of compound 2 shows the presence of weak antiferromagnetic interaction between the Cu^Ⅱ ions in 2.
基金the National Natural Science Foundation of China(No 20541002)the Natural Science Foundation of Zhejiang Province(No 405025)
文摘Ti-HMS materials were prepared by grafting titanocene onto the inner wails of hexagonal mesoporous silica （HMS）. The materials were characterized via powder X-ray diffraction, N2 adsorption-desorption isotherms, diffuse reflectance UV-Vis spectroscopy, and thermo-gravimetric analysis. The template of HMS was removed by calcination, ethanol-extraction, and ethanol-extraction followed by hydrolysis. The available grafting sites of OH groups depend on the different template removal methods of HMS. Ethanol-extraction followed by hydrolysis favors site-isolated Ti atoms in HMS. The catalytic performances of Ti-HMS materials were tested in the oxidation of 4-tert-butyholuene with aqueous hydrogen peroxide. Ti-HMS prepared from HMS via the processing of ethanol-extraction followed by hydrolysis as support gave a maximum conversion of 7. 5% and a complete selectivity to 4-tert-butyl-benzaldehyde, and showed a higher activity compared with those prepared by calcination and ethanol-extraction.
