ZrW2O7(OH,Cl)2·2H2O and its isomorphs were prepared by Acidic Steam Hydrothermal (ASH) method and the pure cubic ZrW2O8 was synthesized by dehydration of ZrW2O7(OH,Cl)2·2H2O. The control factors of ASH metho...ZrW2O7(OH,Cl)2·2H2O and its isomorphs were prepared by Acidic Steam Hydrothermal (ASH) method and the pure cubic ZrW2O8 was synthesized by dehydration of ZrW2O7(OH,Cl)2·2H2O. The control factors of ASH method, such as the type, concentration and volume of the acidic steam source, temperature and time of the reac- tion, were studied in detail. The results showed that HCl was a better volatile acidic steam source and the con- centration of HCl determined the product. At lower concentration of HCl, the main product was Na2W2O7·H2O rather than ZrW2O7(OH,Cl)2·2H2O. When the concentration was higher than 6 mol·L-1, the products in turn be- came sodium tungstates with the structure types of pyrochlore, hexagonal tungsten bronze and finally were trans- formed to ZrW2O7(OH,Cl)·22H2O precursors.展开更多
The compound C12H19Cl2N20·1/2H2O was obtained as the by-product of synthesizing silylene-bridged amino-oxazoline, and its structure was determined by X-ray diffraction. The crystal is of triclinic, space group P1...The compound C12H19Cl2N20·1/2H2O was obtained as the by-product of synthesizing silylene-bridged amino-oxazoline, and its structure was determined by X-ray diffraction. The crystal is of triclinic, space group P1, with a = 12.132（5）, b = 12.231（5）, c = 16.435（6） A^°, α = 97.485（8）, β = 106.106（7）,γ = 98.538（7）°, λ = 0.7103 A^°, V = 2279.0（15）A^°3, Z = 6, Dc = 1.251 g/cm^3, Mr = 286.19, F（000） = 906, R = 0.0846 and wR = 0.2295 for 6290 observed reflections with I 〉 2σ（I）. It is a Cl-salt. The compound was composed of phenyl, amino ion and amido derivatives. The aforementioned components were held together into a complicated three-dimensional network through three types of hydrogen bonding interactions.展开更多
The equilibrium solubility of one CsCl-YCl3-H2O ternary section of CsCl-YCl3-9.5%HCl-H2O quaternary sys-tem at T=298.15 K was investigated by the physico-chemical analysis method and the corresponding phase dia-gram w...The equilibrium solubility of one CsCl-YCl3-H2O ternary section of CsCl-YCl3-9.5%HCl-H2O quaternary sys-tem at T=298.15 K was investigated by the physico-chemical analysis method and the corresponding phase dia-gram was plotted. The crystallization of two new double salts Cs4YCl710H2O (4∶1 type) and Cs3Y2Cl914H2O (3∶2 type) was successful and they were obtained from the complicated system directly. Both were identified and characterized by X-ray, thermal analysis method of TG-DTG, DSC. The fluorescence experiments show that up-conversion phenomenon does not exist in compounds Cs4YCl7·0H2O and Cs3Y2Cl9·4H2O.展开更多
文摘ZrW2O7(OH,Cl)2·2H2O and its isomorphs were prepared by Acidic Steam Hydrothermal (ASH) method and the pure cubic ZrW2O8 was synthesized by dehydration of ZrW2O7(OH,Cl)2·2H2O. The control factors of ASH method, such as the type, concentration and volume of the acidic steam source, temperature and time of the reac- tion, were studied in detail. The results showed that HCl was a better volatile acidic steam source and the con- centration of HCl determined the product. At lower concentration of HCl, the main product was Na2W2O7·H2O rather than ZrW2O7(OH,Cl)2·2H2O. When the concentration was higher than 6 mol·L-1, the products in turn be- came sodium tungstates with the structure types of pyrochlore, hexagonal tungsten bronze and finally were trans- formed to ZrW2O7(OH,Cl)·22H2O precursors.
文摘The compound C12H19Cl2N20·1/2H2O was obtained as the by-product of synthesizing silylene-bridged amino-oxazoline, and its structure was determined by X-ray diffraction. The crystal is of triclinic, space group P1, with a = 12.132（5）, b = 12.231（5）, c = 16.435（6） A^°, α = 97.485（8）, β = 106.106（7）,γ = 98.538（7）°, λ = 0.7103 A^°, V = 2279.0（15）A^°3, Z = 6, Dc = 1.251 g/cm^3, Mr = 286.19, F（000） = 906, R = 0.0846 and wR = 0.2295 for 6290 observed reflections with I 〉 2σ（I）. It is a Cl-salt. The compound was composed of phenyl, amino ion and amido derivatives. The aforementioned components were held together into a complicated three-dimensional network through three types of hydrogen bonding interactions.
基金Project supported by the National Natural Science Foundation of China (No. 29371023).
文摘The equilibrium solubility of one CsCl-YCl3-H2O ternary section of CsCl-YCl3-9.5%HCl-H2O quaternary sys-tem at T=298.15 K was investigated by the physico-chemical analysis method and the corresponding phase dia-gram was plotted. The crystallization of two new double salts Cs4YCl710H2O (4∶1 type) and Cs3Y2Cl914H2O (3∶2 type) was successful and they were obtained from the complicated system directly. Both were identified and characterized by X-ray, thermal analysis method of TG-DTG, DSC. The fluorescence experiments show that up-conversion phenomenon does not exist in compounds Cs4YCl7·0H2O and Cs3Y2Cl9·4H2O.
