Aim To prepare and characterize solid dispersions of silymarin with the intention of improving their dissolution properties. Methods The solid dispersions were prepared by the fusion method with polyethylene glycol ...Aim To prepare and characterize solid dispersions of silymarin with the intention of improving their dissolution properties. Methods The solid dispersions were prepared by the fusion method with polyethylene glycol 6000(PEG 6000) as the carrier. Evaluation of the properties of the dispersions was performed using dissolution studies, X ray powder diffraction and Fourier transform infrared (FT IR) spectroscopy. Results The rate of dissolution of silymarin was considerably improved as compared with pure silymarin when formulated in solid dispersions with PEG 6000. The data of the X ray diffraction showed some changes in the parameters of lattice spacing [ d ], peak position and relative intensities. FT IR together with those from X ray diffraction showed the absence of well defined drug polymer interactions. Conclusion The dissolution improvement of poorly soluble silymarin could be illuminated by the changes of the lattice parameters of PEG 6000 and the drug.展开更多
Er-doped BiVO4 composite photocatalyst was hydrothermal synthesized and characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray Spectroscopy, X-ray photoelectron spectroscopy, ...Er-doped BiVO4 composite photocatalyst was hydrothermal synthesized and characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray Spectroscopy, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectra techniques. The activity of the catalyst was determined by oxidative decomposition of methyl orange in aqueous solution under visible-light irradiation. X-ray photoelectron spectroscopy and energy-dispersive X-ray Spectroscopy analysis revealed that the doped Er existed in the form of Er2O3. It also showed that the Er doping can enhance the visible-light absorption abilities of catalysts and their visible-light-driven photocatalytic activities in comparison with those of pure BiVO4.展开更多
A unique Rh/TiO2 solid acid catalyst modified with H2S04 was synthesized and evaluated in the esterification reaction of propylene glycol methyl ether and decomposition of methyl orange （MO） in aqueous phase under h...A unique Rh/TiO2 solid acid catalyst modified with H2S04 was synthesized and evaluated in the esterification reaction of propylene glycol methyl ether and decomposition of methyl orange （MO） in aqueous phase under halogen lamp irradiation. For this purpose, rhodium （Rh） nanoparticles were loaded on S02-/Ti02 via the photo-deposition method. It was found that S024-/Rh-Ti02 exhibited stronger catalytic activity than S02-/ Ti02. The new catalysts were characterized by X-ray powder diffraction （XRD）, Brunauer-Emmett-Teller （BET）, Transmission electron microscopy （TEM） and high-resolution （HRTEM）, X-ray photoelectron spec- troscopy （XPS） and Fourier Transform infrared spectroscopy （FrlR）. Results from XRD and BET show that S02-/Rh-Ti02 has higher specific surface area and smaller pore size than S02-fri02. The distribution of loaded Rh was found to be uniform with a particle size of 2-4 nm. Data from XPS reveal that Rh primarily exists as Rh~ and Rh3 ＋ in Rh-Ti02 and SO^-/Rh-TiO~. These valence forms of Rh likely contribute to the en- hanced catalytic activity. Furthermore, FT-IR spectra of the catalysts show an abundance of surface hydroxyl groups, which help the formation of hydroxyl radicals and the enhancement of surface acid density. The results show that more acid sites are formed on the sulfated Rh-Ti02, and these acidic sites are largely responsible for improving the catalytic performance. This superior SO]-/Rh-Ti02 catalyst has potential applications in reactions reouirinz efficient acid catalysts, includinz esterification reactions and waste water treatment.展开更多
A novel cerium(Ⅲ) salt of Dawson type tungstophosphoric acid(Ce2P2W18O62·16H2O) was prepared by doping cerous nitrate in H6P2W18O62·13H2O powder and characterized by thermogravimetry and differential therma...A novel cerium(Ⅲ) salt of Dawson type tungstophosphoric acid(Ce2P2W18O62·16H2O) was prepared by doping cerous nitrate in H6P2W18O62·13H2O powder and characterized by thermogravimetry and differential thermal analyses(TG/DTA),Fourier transform infrared spectroscopy(FT-IR),X-ray powder diffraction(XRD),pyridine infrared spectroscopy(Py-IR) and scanning electron microscopy(SEM).Its catalytic activity was evaluated by the probe reaction of synthesis of n-butyl acetate with acetic acid and n-butanol.The effects of various parameters such as molar ratio of n-butanol to acetic acid,reaction temperature,reaction time,and catalyst amount have been studied by single factor experiment.The results show that Ce2P2W18O62·16H2O behaved as an excellent heterogeneous catalyst in the synthesis of n-butyl acetate.The optimum synthetic conditions were determined as follows︰molar ratio of n-butanol to acetic acid at 2.0︰1.0,mass of the catalyst being 1.44% of the total reaction mixture,reaction temperature of 120 ℃ and reaction time of 150 min.Under above conditions,the conversion of acetic acid was above 97.8%.The selectivity of n-butyl acetate based on acetic acid was,in all cases,nearly 100%.The catalysts could be recycled and still exhibited high catalytic activity with 90.4% conversion after five cycles of reaction.It was found by means of TG-DTA and Py-IR that the catalyst deactivation was due to the adsorption of a complex of by-product on the active sites on catalysts surface or the catalyst loss in its separation from the products.Compared with using sulfuric acid as catalyst,the present procedure with Ce2P2W18O62·16H2O is a green productive technology due to simple process,higher yield,catalyst recycling and no corrosion for the production facilities.展开更多
Through improving the aging process during synthesis of the support, γ-Al2O3 with large pore volume and high surface area was synthesized by a facile secondary reforming method. The synthesis parameters, such as the ...Through improving the aging process during synthesis of the support, γ-Al2O3 with large pore volume and high surface area was synthesized by a facile secondary reforming method. The synthesis parameters, such as the reaction temperature, the first aging temperature and the second aging temperature, were investigated. The textural properties of γ-Al2O3 were characterized by means of N2 adsorption-desorption isotherms, X-ray powder diffractometry （XRD）, scanning electron microscopy （SEM）, Fourier transform infrared （FTIR） spectroscopy and thermogravimetry （TG）. The experimental results indicated that AACH and amorphous A1OOH were the precursors of alumina, which were formed via precipitation from solutions after reaction of aluminum sulphate with ammonium hydrogen carbonate. The precursor nanocrystallites grew and re-assembled during the secondary reforming process, which resulted in an increased pore size and pore volume and a decreased bulk density. The as-synthesized γ-Al2O3 materials featured meso/macroporosity, large pore volume （2.175 cm^3/g）, high surface area （237.8 m^2/g）, and low bulk density （0.284 g/mL）.展开更多
The dissolution mechanism of hemimorphite in NH3-（NH4）2SO4-H2O system at 298.15 K was investigated by X-ray powder diffraction （XRD）, scanning electron microscopy （SEM）, Fourier transform infrared spectroscopy ...The dissolution mechanism of hemimorphite in NH3-（NH4）2SO4-H2O system at 298.15 K was investigated by X-ray powder diffraction （XRD）, scanning electron microscopy （SEM）, Fourier transform infrared spectroscopy （FTIR） and X-ray photoelectron spectroscopy （XPS） analysis. The results show that hemimorphite is soluble in NH3-（NH4）2SO4-H2O system and its residue exists in the form of an amorphous SiO2 layer on the hemimorphite surface. The XPS data also indicate that the Si 2p3/2 and O ls spectra of the hemimorphite are broadened and shift to higher binding energies and their binding energies are closer to silica with an increase of total ammonia and time. Solubility of hemimorphite in NH3-（NH4）2SO4-H2O system was measured by means of isothermal solution method at 298.15 K based on the study of the dissolution mechanism of hemimorphite. The results show that the solubility of zinc in solution increases firstly and then decreases with the increase of cr（NH3） （total ammonia concentration） at different NH3/NH4^＋ ratios. The solubility of silicon in solution decreases from 0.0334 mol/kg in ct（NH3）-4.1245 mol/kg NH3-（NH4）2SO4-H2O solution to 0.0046 mol/kg in cT（NH3）=7.6035 mol/kg NH3-（NH4）2SO4-H2O solution.展开更多
Li Fe PO4/C was prepared via solid state reaction and characterized with X-ray powder diffraction and charge–discharge test. As-prepared Li Fe PO4/C has a triphylite structure and exhibits an excellent rate capabilit...Li Fe PO4/C was prepared via solid state reaction and characterized with X-ray powder diffraction and charge–discharge test. As-prepared Li Fe PO4/C has a triphylite structure and exhibits an excellent rate capability and capacity retention. Electrochemical impedance spectroscopy(EIS) was applied to investigate LixFe PO4/C(0<x<1) electrode on temperature variation. The valid equivalent circuit for EIS fitting was determined which contains an intercalation capacitance for Li+ ion accumulation and consumption in the electrode reaction. The surface layer impedance needs to be included in the equivalent circuit when Li Fe PO4/C is deeply delithiated at a relatively high temperature. EIS examination indicates that a temperature rise leads to a better reversibility, lower charge transfer resistance, higher exchange current density J0 and greater Li+ ion diffusion coefficient for the LixFe PO4/C electrode process. The Li+ ion concentration in LixFe PO4/C is potential to impact the Li+ ion diffusion coefficient, and a decrease in the former results in an increase in the latter.展开更多
The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quan...The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quantitative peaks are not well solved, and the accuracy and precision of the results are not satisfactory. This study employed the concept of mass absorption coefficient based on the internal standard method, and the full spectrum fitting and quantitative methods were used to solve the above technical problems. The sample was blended. the internal standard substance of zinc oxide was fully ground, and tablets were prepared by positive pressure method. Under certain instrumental conditions, the PXRD pattern was obtained by scanning. The percentage of gypsum fibrosum in Xiaokening tablet was obtained by quantitative analysis of full spectrum fitting internal standard by TOPAS software. The method was investigated by methodology. At the same time, the method was compared by ion chromatography, and SPSS software was used to make a significant t test on the results of the two methods. After the investigation, the average standard recovery rate of CaSO4-2H2O was 99.06%(RSD = 3.02%);and the recovery rate for simulated samples was 96.7%. The method had good specificity. After statistical analysis, there was no significant difference between the new PXRD method and the traditional method of ion chromatography.展开更多
Nanoscale europium（Ⅲ） metal-organic frameworks, Eu（BTC）（H20）.DMF, were synthesized by rapid microwave-assisted method. The components of the as-prepared products were confirmed by the elemental analysis, X-ray ...Nanoscale europium（Ⅲ） metal-organic frameworks, Eu（BTC）（H20）.DMF, were synthesized by rapid microwave-assisted method. The components of the as-prepared products were confirmed by the elemental analysis, X-ray powder diffraction （XRD）, thermal gravimetric analysis （TGA） and Fourier-transform infrared spectra （FTIR） analyses. Eu（BTC）（H20）.DMF with various morphologies, including particle-like, rod-like, straw-sheaf-like nanostructures, could be simply prepared by con- trolling the concentrations of the starting reactants. The optical measurements on the obtained Eu（BTC）（H20）- DMF indicated that all the nanomaterials show the characteristic emissions of the Eu3＋ ions at 578, 590, 612, 650, and 699 nm, which were at- tributed to 5Do→7FJ （J=0-4） transitions of the Eu3＋ ion, respectively. It was also noticed that the luminescent properties of the as-prepared products were heavily dependent on the morphologies and sizes of the nanomaterials. The assembled straw-sheaf-like architectures displayed the strongest emissions and the longest luminescence lifetime, which was mainly due to the fewest surface defects.展开更多
文摘Aim To prepare and characterize solid dispersions of silymarin with the intention of improving their dissolution properties. Methods The solid dispersions were prepared by the fusion method with polyethylene glycol 6000(PEG 6000) as the carrier. Evaluation of the properties of the dispersions was performed using dissolution studies, X ray powder diffraction and Fourier transform infrared (FT IR) spectroscopy. Results The rate of dissolution of silymarin was considerably improved as compared with pure silymarin when formulated in solid dispersions with PEG 6000. The data of the X ray diffraction showed some changes in the parameters of lattice spacing [ d ], peak position and relative intensities. FT IR together with those from X ray diffraction showed the absence of well defined drug polymer interactions. Conclusion The dissolution improvement of poorly soluble silymarin could be illuminated by the changes of the lattice parameters of PEG 6000 and the drug.
文摘Er-doped BiVO4 composite photocatalyst was hydrothermal synthesized and characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray Spectroscopy, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectra techniques. The activity of the catalyst was determined by oxidative decomposition of methyl orange in aqueous solution under visible-light irradiation. X-ray photoelectron spectroscopy and energy-dispersive X-ray Spectroscopy analysis revealed that the doped Er existed in the form of Er2O3. It also showed that the Er doping can enhance the visible-light absorption abilities of catalysts and their visible-light-driven photocatalytic activities in comparison with those of pure BiVO4.
基金Supported by the Youth Fund of Fujian Province(JA14290,JA15475)the Natural Fund of Fujian Province(2015J01601)the Collaborative Innovation Center of Clean Coal Gasification Technology(XK1403,XK1401)
文摘A unique Rh/TiO2 solid acid catalyst modified with H2S04 was synthesized and evaluated in the esterification reaction of propylene glycol methyl ether and decomposition of methyl orange （MO） in aqueous phase under halogen lamp irradiation. For this purpose, rhodium （Rh） nanoparticles were loaded on S02-/Ti02 via the photo-deposition method. It was found that S024-/Rh-Ti02 exhibited stronger catalytic activity than S02-/ Ti02. The new catalysts were characterized by X-ray powder diffraction （XRD）, Brunauer-Emmett-Teller （BET）, Transmission electron microscopy （TEM） and high-resolution （HRTEM）, X-ray photoelectron spec- troscopy （XPS） and Fourier Transform infrared spectroscopy （FrlR）. Results from XRD and BET show that S02-/Rh-Ti02 has higher specific surface area and smaller pore size than S02-fri02. The distribution of loaded Rh was found to be uniform with a particle size of 2-4 nm. Data from XPS reveal that Rh primarily exists as Rh~ and Rh3 ＋ in Rh-Ti02 and SO^-/Rh-TiO~. These valence forms of Rh likely contribute to the en- hanced catalytic activity. Furthermore, FT-IR spectra of the catalysts show an abundance of surface hydroxyl groups, which help the formation of hydroxyl radicals and the enhancement of surface acid density. The results show that more acid sites are formed on the sulfated Rh-Ti02, and these acidic sites are largely responsible for improving the catalytic performance. This superior SO]-/Rh-Ti02 catalyst has potential applications in reactions reouirinz efficient acid catalysts, includinz esterification reactions and waste water treatment.
基金Supported by the National Natural Science Foundation of China（21161009）the Natural Science Foundation of Jiangxi Province（20122BAB213001,20114BAB213002）the Science and Technology Foundation of Jiangxi Province（GJJ11613）
文摘A novel cerium(Ⅲ) salt of Dawson type tungstophosphoric acid(Ce2P2W18O62·16H2O) was prepared by doping cerous nitrate in H6P2W18O62·13H2O powder and characterized by thermogravimetry and differential thermal analyses(TG/DTA),Fourier transform infrared spectroscopy(FT-IR),X-ray powder diffraction(XRD),pyridine infrared spectroscopy(Py-IR) and scanning electron microscopy(SEM).Its catalytic activity was evaluated by the probe reaction of synthesis of n-butyl acetate with acetic acid and n-butanol.The effects of various parameters such as molar ratio of n-butanol to acetic acid,reaction temperature,reaction time,and catalyst amount have been studied by single factor experiment.The results show that Ce2P2W18O62·16H2O behaved as an excellent heterogeneous catalyst in the synthesis of n-butyl acetate.The optimum synthetic conditions were determined as follows︰molar ratio of n-butanol to acetic acid at 2.0︰1.0,mass of the catalyst being 1.44% of the total reaction mixture,reaction temperature of 120 ℃ and reaction time of 150 min.Under above conditions,the conversion of acetic acid was above 97.8%.The selectivity of n-butyl acetate based on acetic acid was,in all cases,nearly 100%.The catalysts could be recycled and still exhibited high catalytic activity with 90.4% conversion after five cycles of reaction.It was found by means of TG-DTA and Py-IR that the catalyst deactivation was due to the adsorption of a complex of by-product on the active sites on catalysts surface or the catalyst loss in its separation from the products.Compared with using sulfuric acid as catalyst,the present procedure with Ce2P2W18O62·16H2O is a green productive technology due to simple process,higher yield,catalyst recycling and no corrosion for the production facilities.
基金the financial support by the Natural Science Foundation of Liaoning Province of China (Grant No. 2013020122)the National Natural Science Foundationof China (Grant No. 21076100 and 51308045)the financial support by the PetroChina Company Limited (Grant No. 10-01A-01-01-01)
文摘Through improving the aging process during synthesis of the support, γ-Al2O3 with large pore volume and high surface area was synthesized by a facile secondary reforming method. The synthesis parameters, such as the reaction temperature, the first aging temperature and the second aging temperature, were investigated. The textural properties of γ-Al2O3 were characterized by means of N2 adsorption-desorption isotherms, X-ray powder diffractometry （XRD）, scanning electron microscopy （SEM）, Fourier transform infrared （FTIR） spectroscopy and thermogravimetry （TG）. The experimental results indicated that AACH and amorphous A1OOH were the precursors of alumina, which were formed via precipitation from solutions after reaction of aluminum sulphate with ammonium hydrogen carbonate. The precursor nanocrystallites grew and re-assembled during the secondary reforming process, which resulted in an increased pore size and pore volume and a decreased bulk density. The as-synthesized γ-Al2O3 materials featured meso/macroporosity, large pore volume （2.175 cm^3/g）, high surface area （237.8 m^2/g）, and low bulk density （0.284 g/mL）.
基金Projects(511340071) supported by the National Natural Science Foundation of China
文摘The dissolution mechanism of hemimorphite in NH3-（NH4）2SO4-H2O system at 298.15 K was investigated by X-ray powder diffraction （XRD）, scanning electron microscopy （SEM）, Fourier transform infrared spectroscopy （FTIR） and X-ray photoelectron spectroscopy （XPS） analysis. The results show that hemimorphite is soluble in NH3-（NH4）2SO4-H2O system and its residue exists in the form of an amorphous SiO2 layer on the hemimorphite surface. The XPS data also indicate that the Si 2p3/2 and O ls spectra of the hemimorphite are broadened and shift to higher binding energies and their binding energies are closer to silica with an increase of total ammonia and time. Solubility of hemimorphite in NH3-（NH4）2SO4-H2O system was measured by means of isothermal solution method at 298.15 K based on the study of the dissolution mechanism of hemimorphite. The results show that the solubility of zinc in solution increases firstly and then decreases with the increase of cr（NH3） （total ammonia concentration） at different NH3/NH4^＋ ratios. The solubility of silicon in solution decreases from 0.0334 mol/kg in ct（NH3）-4.1245 mol/kg NH3-（NH4）2SO4-H2O solution to 0.0046 mol/kg in cT（NH3）=7.6035 mol/kg NH3-（NH4）2SO4-H2O solution.
基金Project(2010ZC051)supported by the Natural Science Foundation of Yunnan Province,ChinaProject(20140439)supported by Analysis and Testing Foundation from Kunming University of Science and Technology,ChinaProject(14118245)supported by Starting Research Fund from Kunming University of Science and Technology,China
文摘Li Fe PO4/C was prepared via solid state reaction and characterized with X-ray powder diffraction and charge–discharge test. As-prepared Li Fe PO4/C has a triphylite structure and exhibits an excellent rate capability and capacity retention. Electrochemical impedance spectroscopy(EIS) was applied to investigate LixFe PO4/C(0<x<1) electrode on temperature variation. The valid equivalent circuit for EIS fitting was determined which contains an intercalation capacitance for Li+ ion accumulation and consumption in the electrode reaction. The surface layer impedance needs to be included in the equivalent circuit when Li Fe PO4/C is deeply delithiated at a relatively high temperature. EIS examination indicates that a temperature rise leads to a better reversibility, lower charge transfer resistance, higher exchange current density J0 and greater Li+ ion diffusion coefficient for the LixFe PO4/C electrode process. The Li+ ion concentration in LixFe PO4/C is potential to impact the Li+ ion diffusion coefficient, and a decrease in the former results in an increase in the latter.
文摘The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quantitative peaks are not well solved, and the accuracy and precision of the results are not satisfactory. This study employed the concept of mass absorption coefficient based on the internal standard method, and the full spectrum fitting and quantitative methods were used to solve the above technical problems. The sample was blended. the internal standard substance of zinc oxide was fully ground, and tablets were prepared by positive pressure method. Under certain instrumental conditions, the PXRD pattern was obtained by scanning. The percentage of gypsum fibrosum in Xiaokening tablet was obtained by quantitative analysis of full spectrum fitting internal standard by TOPAS software. The method was investigated by methodology. At the same time, the method was compared by ion chromatography, and SPSS software was used to make a significant t test on the results of the two methods. After the investigation, the average standard recovery rate of CaSO4-2H2O was 99.06%(RSD = 3.02%);and the recovery rate for simulated samples was 96.7%. The method had good specificity. After statistical analysis, there was no significant difference between the new PXRD method and the traditional method of ion chromatography.
基金supported by the National Natural Science Foundation of China(21101148,21371165,51372242,21210001,21471144)the National Natural Science Foundation for Creative Research Group(21221061)Jilin Province Youth Foundation(201201005,201201008)
文摘Nanoscale europium（Ⅲ） metal-organic frameworks, Eu（BTC）（H20）.DMF, were synthesized by rapid microwave-assisted method. The components of the as-prepared products were confirmed by the elemental analysis, X-ray powder diffraction （XRD）, thermal gravimetric analysis （TGA） and Fourier-transform infrared spectra （FTIR） analyses. Eu（BTC）（H20）.DMF with various morphologies, including particle-like, rod-like, straw-sheaf-like nanostructures, could be simply prepared by con- trolling the concentrations of the starting reactants. The optical measurements on the obtained Eu（BTC）（H20）- DMF indicated that all the nanomaterials show the characteristic emissions of the Eu3＋ ions at 578, 590, 612, 650, and 699 nm, which were at- tributed to 5Do→7FJ （J=0-4） transitions of the Eu3＋ ion, respectively. It was also noticed that the luminescent properties of the as-prepared products were heavily dependent on the morphologies and sizes of the nanomaterials. The assembled straw-sheaf-like architectures displayed the strongest emissions and the longest luminescence lifetime, which was mainly due to the fewest surface defects.
