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2016 Volume 79 Issue 6
2016, 79(6): 483-489
Abstract:
In recent years, increasing attention have been focused on the silafluorene-containing compounds due to their unique electronic structures and photoelectric properties, which are widely used in the field of OLED, PSC, OFET etc. Herein the recent progress made in the syntheses, structure modifications, properties and applications of silafluorene-containing compounds are reviewed.
In recent years, increasing attention have been focused on the silafluorene-containing compounds due to their unique electronic structures and photoelectric properties, which are widely used in the field of OLED, PSC, OFET etc. Herein the recent progress made in the syntheses, structure modifications, properties and applications of silafluorene-containing compounds are reviewed.
2016, 79(6): 490-495
Abstract:
The synthesis of nanomaterials by template method is a very important technique and has been widely studied on industry fields due to its remarkable controllability. The pore size, shape and structure of synthetic mesoporous nanomaterials are precisely controlled by structure-oriented, skeleton filling, the balance and matching charge functionalization of template. In this paper developments and characteristics of hard and soft templates in the process of nanomaterials synthesis are emphasized. The recent research progresses of syntheses of the nanomaterials using template techniques in biological materials, electrochemistry, chemical synthesis and catalysis are reviewed. The advantages and disadvantages of the template method during the preparing processes are discussed. The syntheses of the mesoporous nanomaterials by template method will be potentially developed on supramolecular functional materials, photochemical reactions and catalysis industries.
The synthesis of nanomaterials by template method is a very important technique and has been widely studied on industry fields due to its remarkable controllability. The pore size, shape and structure of synthetic mesoporous nanomaterials are precisely controlled by structure-oriented, skeleton filling, the balance and matching charge functionalization of template. In this paper developments and characteristics of hard and soft templates in the process of nanomaterials synthesis are emphasized. The recent research progresses of syntheses of the nanomaterials using template techniques in biological materials, electrochemistry, chemical synthesis and catalysis are reviewed. The advantages and disadvantages of the template method during the preparing processes are discussed. The syntheses of the mesoporous nanomaterials by template method will be potentially developed on supramolecular functional materials, photochemical reactions and catalysis industries.
2016, 79(6): 496-502
Abstract:
Ag nanoparticles (Ag NPs)/polymer composite materials have made rapid progress in recent years. They also have attracted tremendous attention due to their outstanding physical and chemical properties, especially in the aspect of high antibacterial activity. In this paper, the progress in synthetic methods and antibacterial effect of Ag NPs/polymer composites in recent years was reviewed, and the prospects of development and application of them were also discussed.
Ag nanoparticles (Ag NPs)/polymer composite materials have made rapid progress in recent years. They also have attracted tremendous attention due to their outstanding physical and chemical properties, especially in the aspect of high antibacterial activity. In this paper, the progress in synthetic methods and antibacterial effect of Ag NPs/polymer composites in recent years was reviewed, and the prospects of development and application of them were also discussed.
2016, 79(6): 503-508
Abstract:
Due to the unique two-dimensional structure of single atomic layer and excellent performance, graphene (Gr) attracted numerous attentions of many scientists. It will broaden prospective applications in many fields, such as materials, electronics, chemistry, energy, and bio-medicine and so on. For the future developments and applications of Gr, it is crucial to know how to obtain Gr with high quality and high yield. Microwave reduction, a green, efficient and handy method, is an important approach for producing Gr. The progress in preparation of Gr, doped Gr and Gr nanocomposites by microwave method and the applications of Gr nanocomposites as anode materials for the lithium-ion batteries were reviewed, and the prospect of them were presented, too.
Due to the unique two-dimensional structure of single atomic layer and excellent performance, graphene (Gr) attracted numerous attentions of many scientists. It will broaden prospective applications in many fields, such as materials, electronics, chemistry, energy, and bio-medicine and so on. For the future developments and applications of Gr, it is crucial to know how to obtain Gr with high quality and high yield. Microwave reduction, a green, efficient and handy method, is an important approach for producing Gr. The progress in preparation of Gr, doped Gr and Gr nanocomposites by microwave method and the applications of Gr nanocomposites as anode materials for the lithium-ion batteries were reviewed, and the prospect of them were presented, too.
2016, 79(6): 509-515
Abstract:
β-secretase (BACE1) is responsible for the initial cleavage of transmembrane amyloid precursor protein that leads to the production of β-amyloid (Aβ) peptides in the brain, and is a prime target for Alzheimer's disease (AD). In this paper, 34 kinds of dihydroisoquinoline derivatives as BACE1 inhibitors were studied by three-dimensional quantitative structure-activity relationship and molecular docking methods. The resultant optimal comparative molecular similarity indices analysis (CoMSIA) model, constructed based on the steric, hydrophobic and hydrogen-bond donor fields, displays a strong predictability (Q2=0.47, Rncv2=0.93, Rpre2=0.95). This model and the derived information may help to provide better understanding of the structure features and binding mode of BACE1 inhibitors and to facilitate corresponding novel inhibitors' design.
β-secretase (BACE1) is responsible for the initial cleavage of transmembrane amyloid precursor protein that leads to the production of β-amyloid (Aβ) peptides in the brain, and is a prime target for Alzheimer's disease (AD). In this paper, 34 kinds of dihydroisoquinoline derivatives as BACE1 inhibitors were studied by three-dimensional quantitative structure-activity relationship and molecular docking methods. The resultant optimal comparative molecular similarity indices analysis (CoMSIA) model, constructed based on the steric, hydrophobic and hydrogen-bond donor fields, displays a strong predictability (Q2=0.47, Rncv2=0.93, Rpre2=0.95). This model and the derived information may help to provide better understanding of the structure features and binding mode of BACE1 inhibitors and to facilitate corresponding novel inhibitors' design.
2016, 79(6): 516-522
Abstract:
The secondary structure, nanostructure and macro-feature of peptide GFS-15 were characterized by circular dichroism spectroscopy (CD), AFM and Congo red dye. The influence of concentration, self-assembly time and ions on the self-assembly process of the peptide were studied by cyclic voltammetry (CV) and CD. The results showed that this peptide can form nano-fiber which can bind to gold electrode to form the hydrogel support 3D cell culture matrix. 3D cell culture test and 3D cell culture real-time tests confirmed the cell strain not only growth in the nano 3D microenvironment, but also self-assembling to gold electrode sensor (nano-gold particles) surface. This study may inspire cell real-time monitor and nano-biomedical developing.
The secondary structure, nanostructure and macro-feature of peptide GFS-15 were characterized by circular dichroism spectroscopy (CD), AFM and Congo red dye. The influence of concentration, self-assembly time and ions on the self-assembly process of the peptide were studied by cyclic voltammetry (CV) and CD. The results showed that this peptide can form nano-fiber which can bind to gold electrode to form the hydrogel support 3D cell culture matrix. 3D cell culture test and 3D cell culture real-time tests confirmed the cell strain not only growth in the nano 3D microenvironment, but also self-assembling to gold electrode sensor (nano-gold particles) surface. This study may inspire cell real-time monitor and nano-biomedical developing.
2016, 79(6): 523-527
Abstract:
Mechanical ball grinding as a rapid and environmentally friendly synthetic method emerges great potential in the solvent-free synthesis of double metal cyanide (DMC) catalysts. Zn-Ni DMCs with small amounts of co-complexing agents (co-CAs) were successfully synthesized through the grinding process. Elemental analysis and FT-IR results indicated that the DMC catalysts were successfully mixed with various co-CAs. The SEM images showed that the resulting DMC catalysts were nanoscale. The DMC complex was proven to be an effective catalyst for the ring-open copolymerization of propylene oxide (PO) with phthalic anhydride (PA) without solvent under controlled reaction condition (6 h, 110℃). For copolymerization, the DMCs showed relatively high activity, and the obtained polyester poly (PO-co-PA) exhibited high molecular weight and narrow polydispersity index.
Mechanical ball grinding as a rapid and environmentally friendly synthetic method emerges great potential in the solvent-free synthesis of double metal cyanide (DMC) catalysts. Zn-Ni DMCs with small amounts of co-complexing agents (co-CAs) were successfully synthesized through the grinding process. Elemental analysis and FT-IR results indicated that the DMC catalysts were successfully mixed with various co-CAs. The SEM images showed that the resulting DMC catalysts were nanoscale. The DMC complex was proven to be an effective catalyst for the ring-open copolymerization of propylene oxide (PO) with phthalic anhydride (PA) without solvent under controlled reaction condition (6 h, 110℃). For copolymerization, the DMCs showed relatively high activity, and the obtained polyester poly (PO-co-PA) exhibited high molecular weight and narrow polydispersity index.
2016, 79(6): 528-533
Abstract:
The Dawson type yttriumphosphotungstates supported on 4A zeolite(Y2P2W18O62·nH2O/4A zeolite)with different loading level were prepared by immersion process and characterized by FT IR, SEM, EDS, NH3-TPD and N2 adsorption-desorption. They were applied to the synthesis of acetylsalicylic acid. The influences of catalyst dosage, the mole ratio of reactants, reaction temperature, reaction time and reusability of catalyst on the synthesis were investigated. The results showed that as-prepared yttriumphosphotungstates kept Dawson structure before or after loading on 4A zeolite. Both Y2P2W18O62·nH2O and 40%Y2P2W18O62·nH2O/4A zeolite took the form of spheres. The specific surface area, acid strength and acid amount were enhanced by loading Y2P2W18O62·nH2O on 4A zeolite. The optimal conditions of synthesis reaction were as follows:w (Y2P2W18O62·nH2O/4A zeolite) was 2.3%, the molar ratio of salicylic acid to acetic anhydride was 1:3,reaction temperature of 80℃, reaction time of 30 min. The yield of acetylsalicylic acid could reach 95.2% under the optimum conditions and kept 77.9% after the catalyst being used six times.
The Dawson type yttriumphosphotungstates supported on 4A zeolite(Y2P2W18O62·nH2O/4A zeolite)with different loading level were prepared by immersion process and characterized by FT IR, SEM, EDS, NH3-TPD and N2 adsorption-desorption. They were applied to the synthesis of acetylsalicylic acid. The influences of catalyst dosage, the mole ratio of reactants, reaction temperature, reaction time and reusability of catalyst on the synthesis were investigated. The results showed that as-prepared yttriumphosphotungstates kept Dawson structure before or after loading on 4A zeolite. Both Y2P2W18O62·nH2O and 40%Y2P2W18O62·nH2O/4A zeolite took the form of spheres. The specific surface area, acid strength and acid amount were enhanced by loading Y2P2W18O62·nH2O on 4A zeolite. The optimal conditions of synthesis reaction were as follows:w (Y2P2W18O62·nH2O/4A zeolite) was 2.3%, the molar ratio of salicylic acid to acetic anhydride was 1:3,reaction temperature of 80℃, reaction time of 30 min. The yield of acetylsalicylic acid could reach 95.2% under the optimum conditions and kept 77.9% after the catalyst being used six times.
2016, 79(6): 534-538
Abstract:
Graphene oxide (GO) is prepared by the modified Hummers method and reduced by a new low-temperature chemical reduction. The structure and morphology of GO and reduced graphene oxide (rGO) was characterized by FT IR, XRD, Raman, XPS, SEM and AFM. Results showed GO can be reduced by using chitosan as the reductant even at low temperature environment. This means the reduction of GO and application of graphene can be realized concurrently at same one low temperature environment.
Graphene oxide (GO) is prepared by the modified Hummers method and reduced by a new low-temperature chemical reduction. The structure and morphology of GO and reduced graphene oxide (rGO) was characterized by FT IR, XRD, Raman, XPS, SEM and AFM. Results showed GO can be reduced by using chitosan as the reductant even at low temperature environment. This means the reduction of GO and application of graphene can be realized concurrently at same one low temperature environment.
2016, 79(6): 539-543
Abstract:
A novel mannitol-based oil gelator was synthesized from cyclohexanone and mannitol through ketal reaction. Factors including reaction time, weight of catalyst, weight of molecular sieve, the ratio of the reactants that influenced on the reaction yield were studied. Under the optimal conditions, that is, 12 g molecular sieve, 0.8 g catalyst, the mole ratio of cyclohexanone to mannitol 6.2:1, and the reaction time 1 h, 52% yield of oil gelator can be achieved. The test of the gelation ability of as-synthesized sugar-based gelator indicated that it can gel several solvents like petrol and silicone oil. The critical gelation concentrations for diesel, petrol and silicone oil were 0.74(wt)%, 2.70(wt)% and 0.39(wt)%, respectively.
A novel mannitol-based oil gelator was synthesized from cyclohexanone and mannitol through ketal reaction. Factors including reaction time, weight of catalyst, weight of molecular sieve, the ratio of the reactants that influenced on the reaction yield were studied. Under the optimal conditions, that is, 12 g molecular sieve, 0.8 g catalyst, the mole ratio of cyclohexanone to mannitol 6.2:1, and the reaction time 1 h, 52% yield of oil gelator can be achieved. The test of the gelation ability of as-synthesized sugar-based gelator indicated that it can gel several solvents like petrol and silicone oil. The critical gelation concentrations for diesel, petrol and silicone oil were 0.74(wt)%, 2.70(wt)% and 0.39(wt)%, respectively.
2016, 79(6): 544-549
Abstract:
The salinity of the feed, especially at the high salinity, had an obviously effect on the membrane fouling. The sludge filterability would be deteriorated at the salt concentration of 5 g/L in the feed to lead to the increase of the rate of membrane fouling. The concentrations of soluble microbial product (SMP) and extracellular polymeric substances (EPS) in the activated sludge, especially the content of protein in SMP, were closely related to the concentration of the sodium ions, which had a more significant effect on the tightly bound EPS (TB) than that of the loosely bound EPS (LB). The salinity had a little impact on the removal of COD and NH4+-N, and their removal rate was maintained above 92% and 94%, respectively. However, a significantly decrease in the TP removal was observed under high salinity condition.
The salinity of the feed, especially at the high salinity, had an obviously effect on the membrane fouling. The sludge filterability would be deteriorated at the salt concentration of 5 g/L in the feed to lead to the increase of the rate of membrane fouling. The concentrations of soluble microbial product (SMP) and extracellular polymeric substances (EPS) in the activated sludge, especially the content of protein in SMP, were closely related to the concentration of the sodium ions, which had a more significant effect on the tightly bound EPS (TB) than that of the loosely bound EPS (LB). The salinity had a little impact on the removal of COD and NH4+-N, and their removal rate was maintained above 92% and 94%, respectively. However, a significantly decrease in the TP removal was observed under high salinity condition.
2016, 79(6): 550-553
Abstract:
In this work, a novel method for rapid detection of thiol compounds was established using fluorescein isothiocyanate (FITC) as fluorescence probe. The method was based on the quenching of the fluorescence of FITC by thiol compounds. Thiol compounds could be detected in 5 minutes at the optimized conditions including pH and reaction time. The method was used to detect glutathione (GSH) in real samples and showed good selectivity and recovery. The limits of detection (LOD) were 3.08 μmol/L for glutathione (GSH), 2.66 μmol/L for homocysteine (Hcy), 1.28 μmol/L for cysteine (Cys), and 1.92 μmol/L for dithiothreitol (DTT).
In this work, a novel method for rapid detection of thiol compounds was established using fluorescein isothiocyanate (FITC) as fluorescence probe. The method was based on the quenching of the fluorescence of FITC by thiol compounds. Thiol compounds could be detected in 5 minutes at the optimized conditions including pH and reaction time. The method was used to detect glutathione (GSH) in real samples and showed good selectivity and recovery. The limits of detection (LOD) were 3.08 μmol/L for glutathione (GSH), 2.66 μmol/L for homocysteine (Hcy), 1.28 μmol/L for cysteine (Cys), and 1.92 μmol/L for dithiothreitol (DTT).
2016, 79(6): 554-557
Abstract:
Nucleic acids and proteins are two kinds of most important molecules in cells. Study on their interaction is one of the key issues in molecular biology. Here, we investigated the interaction between thrombin and its corresponding aptamer (T15) based on a new ultra-low-field biological force spectroscopy. The result showed that the binding force of thrombin/aptamer complex is about 80 pN. In addition, the dissociation kinetic information of thrombin/apatamer had been obtained on the molecular level.
Nucleic acids and proteins are two kinds of most important molecules in cells. Study on their interaction is one of the key issues in molecular biology. Here, we investigated the interaction between thrombin and its corresponding aptamer (T15) based on a new ultra-low-field biological force spectroscopy. The result showed that the binding force of thrombin/aptamer complex is about 80 pN. In addition, the dissociation kinetic information of thrombin/apatamer had been obtained on the molecular level.
2016, 79(6): 558-561
Abstract:
The supermolecular compound[PyBImH2]·[SnCl6] (PyBIm=2-(pyrid-4-yl)benzimidazole) had been synthesized and characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The compound crystallizes in orthorhombic Pbcn space group with the crystal cell parameters:a=7.1468(3) Å, b=15.0493(6) Å, c=16.1195(8) Å, V=1733.72(13) Å3, Z=4, Dc=2.025 g/cm3, Mr=528.63, μ(MoKα)=2.395mm-1, F(000)=1024. The final R1=0.0264 and wR2=0.0665. Sn4+ is coordinated by six chloride ions in an octahedron geometry.[SnCl6]2- anions and[PyBImH2]2+ cations are linked together via hydrogen bonds and π-π stacking interactions, forming a three-dimensional supermolecular framework.
The supermolecular compound[PyBImH2]·[SnCl6] (PyBIm=2-(pyrid-4-yl)benzimidazole) had been synthesized and characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The compound crystallizes in orthorhombic Pbcn space group with the crystal cell parameters:a=7.1468(3) Å, b=15.0493(6) Å, c=16.1195(8) Å, V=1733.72(13) Å3, Z=4, Dc=2.025 g/cm3, Mr=528.63, μ(MoKα)=2.395mm-1, F(000)=1024. The final R1=0.0264 and wR2=0.0665. Sn4+ is coordinated by six chloride ions in an octahedron geometry.[SnCl6]2- anions and[PyBImH2]2+ cations are linked together via hydrogen bonds and π-π stacking interactions, forming a three-dimensional supermolecular framework.
2016, 79(6): 562-565
Abstract:
Micro-nano titanium dioxide conductive powder coated by antimony doped tin dioxide was prepared by the chemical co-precipitation method and characterized by XRD and SEM. The effect of the different antimony mass on the conductive properties of powder was examined. The results of cyclic voltammetry (CV) and alternating-current impedance diagrams curves analyzing on the composite electrode prepared by electrochemical workstation showed that with the increase of scanning speed, oxidation and reduction peaks moved to the cathode and anode, respectively, and the shape of the peaks didn't change obviously; when the mass ratio of SnCl4·5H2O and SbCl3 was 10, capacitive reactance arc radius of the sample was the smallest and the slope was the largest, the resistance of the sample was minimum. The conductive performance of the powder sample prepared under the optimized condition was the best, which was in accordance with the results obtained by resistivity measurement using electrical resistivity device. So using AC impedance method and CV to investigate the conductivity of conductive powder was feasible.
Micro-nano titanium dioxide conductive powder coated by antimony doped tin dioxide was prepared by the chemical co-precipitation method and characterized by XRD and SEM. The effect of the different antimony mass on the conductive properties of powder was examined. The results of cyclic voltammetry (CV) and alternating-current impedance diagrams curves analyzing on the composite electrode prepared by electrochemical workstation showed that with the increase of scanning speed, oxidation and reduction peaks moved to the cathode and anode, respectively, and the shape of the peaks didn't change obviously; when the mass ratio of SnCl4·5H2O and SbCl3 was 10, capacitive reactance arc radius of the sample was the smallest and the slope was the largest, the resistance of the sample was minimum. The conductive performance of the powder sample prepared under the optimized condition was the best, which was in accordance with the results obtained by resistivity measurement using electrical resistivity device. So using AC impedance method and CV to investigate the conductivity of conductive powder was feasible.
2016, 79(6): 566-569
Abstract:
For all reactions with certain reaction order, no matter how the reaction order is, the nonlinear fitting method is applicable. This method can be divided into two steps. In the first step, the reaction order is obtained by nonlinear fitting of the experimental data; in the second step, by the help of reaction order obtained in the first step, the reaction rate constant can be obtained by once more nonlinear fitting of experimental data. Compared with the traditional method of establishing the reaction rate equation, the nonlinear fitting method is easy to operate, and the processing results are concise and accurate.
For all reactions with certain reaction order, no matter how the reaction order is, the nonlinear fitting method is applicable. This method can be divided into two steps. In the first step, the reaction order is obtained by nonlinear fitting of the experimental data; in the second step, by the help of reaction order obtained in the first step, the reaction rate constant can be obtained by once more nonlinear fitting of experimental data. Compared with the traditional method of establishing the reaction rate equation, the nonlinear fitting method is easy to operate, and the processing results are concise and accurate.
2016, 79(6): 570-575
Abstract:
The great demand of novel ecological agriculture applicable functional materials and development of optical agriculture have put forward higher requirements for the chemistry related disciplines. This paper presents a comprehensive research style experiment ‘Preparation and characterization of agricultural light-conversion composite material based on Sr2Si5N8:Eu2+ and cellulose’. The purpose is that, through the experimental principle explanations, research ideas and methods discussion, material preparations, characterizations and data processing, the students can fully grasp the key knowledge of optical materials, cellulose hydrolysis, preparation of composite material, spectroscopic characterization, mechanical performance analysis, and so on. Practice shows that this experiment can be helpful to promote students' innovative spirit, enhance their engineering practice ability and basic scientific research ability, which can finally improve the quality of education and teaching.
The great demand of novel ecological agriculture applicable functional materials and development of optical agriculture have put forward higher requirements for the chemistry related disciplines. This paper presents a comprehensive research style experiment ‘Preparation and characterization of agricultural light-conversion composite material based on Sr2Si5N8:Eu2+ and cellulose’. The purpose is that, through the experimental principle explanations, research ideas and methods discussion, material preparations, characterizations and data processing, the students can fully grasp the key knowledge of optical materials, cellulose hydrolysis, preparation of composite material, spectroscopic characterization, mechanical performance analysis, and so on. Practice shows that this experiment can be helpful to promote students' innovative spirit, enhance their engineering practice ability and basic scientific research ability, which can finally improve the quality of education and teaching.
2016, 79(6): 575-575
Abstract:
1,2-Diethoxybenzene was synthesized by using 1,2-benzenediol and bromoethane as starting materials and polyethylene glycol as phase transfer catalyst. Then 1,2-diethoxy-4-nitrophathalic was synthesized through nitration of 1,2-diethoxybenzene with acetic acid and nitric acid. The effects of the reaction temperature, reaction time, molar ratio of raw materials and amount of the catalyst on the yield of product were investigated. The optimal reaction condition of 1,2-diethoxybenzene was n(C6H4(OH)2):n(NaOH):n(C2H5Br)=1:2.6:2.4, reaction temperature 80℃, reaction time 4 hours, catalyst 2g. The average yield of 1,2-diethoxybenzene was 88%. The optimal reaction condition of 4-nitrophathalic was n(C10H14O2):n(HNO3)=1:1.2, acetic acid 25 mL, reaction time 30 minutes, reaction temperature 20℃. Its average yield was 99%.
1,2-Diethoxybenzene was synthesized by using 1,2-benzenediol and bromoethane as starting materials and polyethylene glycol as phase transfer catalyst. Then 1,2-diethoxy-4-nitrophathalic was synthesized through nitration of 1,2-diethoxybenzene with acetic acid and nitric acid. The effects of the reaction temperature, reaction time, molar ratio of raw materials and amount of the catalyst on the yield of product were investigated. The optimal reaction condition of 1,2-diethoxybenzene was n(C6H4(OH)2):n(NaOH):n(C2H5Br)=1:2.6:2.4, reaction temperature 80℃, reaction time 4 hours, catalyst 2g. The average yield of 1,2-diethoxybenzene was 88%. The optimal reaction condition of 4-nitrophathalic was n(C10H14O2):n(HNO3)=1:1.2, acetic acid 25 mL, reaction time 30 minutes, reaction temperature 20℃. Its average yield was 99%.
