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2014 Volume 31 Issue 7
2014, 31(7): 749-756
doi: 10.3724/SP.J.1095.2014.30353
Abstract:
The nickel-iron batteries have been widely employed into electricity grid and backup power devices owing to their low cost,durable in use,eco-friendliness and safety.Additionally,the promising nickel-iron battery is widely discussed for applications in electric vehicles(EV).The principle and structural design of nickel-iron battery were introduced,and combined with the current research and development situation of nickel-iron battery at home and abroad.The comprehensive performance and application of nickel-iron battery were overviewed,focusing on the existing problems of iron anode,research status as well as development direction of nickel-iron battery.
The nickel-iron batteries have been widely employed into electricity grid and backup power devices owing to their low cost,durable in use,eco-friendliness and safety.Additionally,the promising nickel-iron battery is widely discussed for applications in electric vehicles(EV).The principle and structural design of nickel-iron battery were introduced,and combined with the current research and development situation of nickel-iron battery at home and abroad.The comprehensive performance and application of nickel-iron battery were overviewed,focusing on the existing problems of iron anode,research status as well as development direction of nickel-iron battery.
2014, 31(7): 757-762
doi: 10.3724/SP.J.1095.2014.30445
Abstract:
A polyolefin/ceramic composite membrane,ZrO2/SiO2/PP(PP:polypropylene),was prepared as the separator for Li-ion batteries in order to replace the traditional microporous polyolefin membrane.The polyolefin/ceramic composite membrane has high porosity,and can be well wetted by the liquid electrolyte.The ion conductivity of membrane is easily achieved by absorbing the liquid electrolyte due to the high capillary effect.The amphoteric character of ZrO2/SiO2 can scavenge acidic hydrogen fluoride,which is inevitably present in the LiPF6-based electrolytes used currently in the Li-ion batteries.With the polyolefin/ceramic composite membrane as a separator,the graphite/cathode cell exhibits good capacity retention.It is also found that the Li-ion cell fabricated in this manner not only has stable capacity retention,better high temperature performance,but also shows good high-rate performance.
A polyolefin/ceramic composite membrane,ZrO2/SiO2/PP(PP:polypropylene),was prepared as the separator for Li-ion batteries in order to replace the traditional microporous polyolefin membrane.The polyolefin/ceramic composite membrane has high porosity,and can be well wetted by the liquid electrolyte.The ion conductivity of membrane is easily achieved by absorbing the liquid electrolyte due to the high capillary effect.The amphoteric character of ZrO2/SiO2 can scavenge acidic hydrogen fluoride,which is inevitably present in the LiPF6-based electrolytes used currently in the Li-ion batteries.With the polyolefin/ceramic composite membrane as a separator,the graphite/cathode cell exhibits good capacity retention.It is also found that the Li-ion cell fabricated in this manner not only has stable capacity retention,better high temperature performance,but also shows good high-rate performance.
2014, 31(7): 763-769
doi: 10.3724/SP.J.1095.2014.30537
Abstract:
Solidum dichloroacetate(DCA) loaded electrospun mats was fabricated through the solution electrospun method.When applying this DCA-loaded electrospun mats on the therapy of the subcutaneous cervical cancer model,a 94% tumor suppression rate and an overall 38% recovery rate were achieved after 19 days' treatment.The trend of recurrence and metastasis was also significantly inhabited.Meanwhile,DCA-loaded electropsun mats improved the life quality of tumor-bearing mice fundamentally.Therefore,DCA administrated by electrospun mats is a safe approach for the treatment of anti-cervical cancer.
Solidum dichloroacetate(DCA) loaded electrospun mats was fabricated through the solution electrospun method.When applying this DCA-loaded electrospun mats on the therapy of the subcutaneous cervical cancer model,a 94% tumor suppression rate and an overall 38% recovery rate were achieved after 19 days' treatment.The trend of recurrence and metastasis was also significantly inhabited.Meanwhile,DCA-loaded electropsun mats improved the life quality of tumor-bearing mice fundamentally.Therefore,DCA administrated by electrospun mats is a safe approach for the treatment of anti-cervical cancer.
2014, 31(7): 770-777
doi: 10.3724/SP.J.1095.2014.40043
Abstract:
Using polypropylene containing pendant hydroxyl groups as initiator and stannous octoate as catalyst,a serial of well-defined polypropylene-graft-polycaprolactone polymers was synthesized via ring opening polymerization,and the structures of the polymers were characterized by NMR,IR,DSC and WAXD.In addition,the influence of temperature and time on the grafting reaction was studied.The results show that the optimal reaction temperature is 90℃ and the grafting lengths can be controlled by regulating reaction time.Furthermore,the functional polypropylene were used as compatibilizer for polypropylene/nylon-6 blends,and the influence of compatibilizer on the blends was investigated by SEM.The SEM reveals that the interfacial tension and dimensions of separated phases are markedly reduced while interfacial adhesion is greatly enhanced because of the addition of the compatibilizer.
Using polypropylene containing pendant hydroxyl groups as initiator and stannous octoate as catalyst,a serial of well-defined polypropylene-graft-polycaprolactone polymers was synthesized via ring opening polymerization,and the structures of the polymers were characterized by NMR,IR,DSC and WAXD.In addition,the influence of temperature and time on the grafting reaction was studied.The results show that the optimal reaction temperature is 90℃ and the grafting lengths can be controlled by regulating reaction time.Furthermore,the functional polypropylene were used as compatibilizer for polypropylene/nylon-6 blends,and the influence of compatibilizer on the blends was investigated by SEM.The SEM reveals that the interfacial tension and dimensions of separated phases are markedly reduced while interfacial adhesion is greatly enhanced because of the addition of the compatibilizer.
2014, 31(7): 778-781
doi: 10.3724/SP.J.1095.2014.30434
Abstract:
Without the addition of catalysts and solvents,15 known bis(indolyl) alkane compounds were synthesized under mild conditions from substituted indoles and substituted benzaldehydes in 65%~91% yields.The mechanism of this condensation reaction was discussed and the relationship between reaction speed and substituent groups was described.All the compounds synthesized were confirmed by 1H NMR,13C NMR and IR analysis.
Without the addition of catalysts and solvents,15 known bis(indolyl) alkane compounds were synthesized under mild conditions from substituted indoles and substituted benzaldehydes in 65%~91% yields.The mechanism of this condensation reaction was discussed and the relationship between reaction speed and substituent groups was described.All the compounds synthesized were confirmed by 1H NMR,13C NMR and IR analysis.
2014, 31(7): 782-787
doi: 10.3724/SP.J.1095.2014.30430
Abstract:
The twin drug(PHI) was synthesized by coupling ibuprofen(IPF) and paracetamol(PCM) using dicyclohexylcarbodiimide(DCC) as dehydrating agent,4-dimethylaminopyridine(DMAP) as catalyst,and anhydrous acetone and ethyl acetate as reaction solvents.PHI was purified by recrystallization and its structure was confirmed by IR and 1H NMR spectroscopy.The effect of catalyst,dehydrating agent,reaction time,feed ratio and reaction solvents on the yield of the product was investigated.The reaction conditions were optimized by the orthogonal test.The optimized reaction conditions are:the molar ratio of raw materials is n(PCM):n(IPF)=1:1.5,the optimal amount of DMAP is 10% mass fraction of ibuprofen;the volume of solvent is 70 mL(the volume ratio of ethyl acetate and acetone is 1:1) and the reaction time is 8 h.Under the optimized conditions,the yield of target is 66.5%.
The twin drug(PHI) was synthesized by coupling ibuprofen(IPF) and paracetamol(PCM) using dicyclohexylcarbodiimide(DCC) as dehydrating agent,4-dimethylaminopyridine(DMAP) as catalyst,and anhydrous acetone and ethyl acetate as reaction solvents.PHI was purified by recrystallization and its structure was confirmed by IR and 1H NMR spectroscopy.The effect of catalyst,dehydrating agent,reaction time,feed ratio and reaction solvents on the yield of the product was investigated.The reaction conditions were optimized by the orthogonal test.The optimized reaction conditions are:the molar ratio of raw materials is n(PCM):n(IPF)=1:1.5,the optimal amount of DMAP is 10% mass fraction of ibuprofen;the volume of solvent is 70 mL(the volume ratio of ethyl acetate and acetone is 1:1) and the reaction time is 8 h.Under the optimized conditions,the yield of target is 66.5%.
2014, 31(7): 788-792
doi: 10.3724/SP.J.1095.2014.30488
Abstract:
Nine Shiff bases 3-methyl-4-(X-substituted-benzylideneamino)-5-ethoxycarbonyl methylsulfanyl-1,2,4-triazole a~i were synthesized from 3-methyl-4-amino-5-ethoxycarbonylmethyl sulfanyl-1,2,4-triazole and substituted aromatic aldehydes.The structures of synthetic compounds were confirmed by 1H NMR,IR,MS analyses.The crystal structure of 3-methyl-4-(4-hydroxybenzylideneamino)-5-ethoxycarbonylmethylsulfanyl-1,2,4-triazole h(CCDC:910927) was determined by X-ray diffraction as:C14H16N4O3S,Mr=320.37,Orthorhombic,P2(1)2(1)2(1)/n,a=0.9220(10) nm,b=1.5823(17) nm,c=2.1667(2) nm,V=3.161(6) nm3,Z=8,F(000)=1344.The antifungal activities of the new Schiff bases against four vegetable pathogens have been tested.The EC95 values of compounds d,e and f against Gibberlla saubinetii and Fusarium oxysporium f.s.px.niveum indicate that their antifungal activities are better than that of triadimefon.
Nine Shiff bases 3-methyl-4-(X-substituted-benzylideneamino)-5-ethoxycarbonyl methylsulfanyl-1,2,4-triazole a~i were synthesized from 3-methyl-4-amino-5-ethoxycarbonylmethyl sulfanyl-1,2,4-triazole and substituted aromatic aldehydes.The structures of synthetic compounds were confirmed by 1H NMR,IR,MS analyses.The crystal structure of 3-methyl-4-(4-hydroxybenzylideneamino)-5-ethoxycarbonylmethylsulfanyl-1,2,4-triazole h(CCDC:910927) was determined by X-ray diffraction as:C14H16N4O3S,Mr=320.37,Orthorhombic,P2(1)2(1)2(1)/n,a=0.9220(10) nm,b=1.5823(17) nm,c=2.1667(2) nm,V=3.161(6) nm3,Z=8,F(000)=1344.The antifungal activities of the new Schiff bases against four vegetable pathogens have been tested.The EC95 values of compounds d,e and f against Gibberlla saubinetii and Fusarium oxysporium f.s.px.niveum indicate that their antifungal activities are better than that of triadimefon.
2014, 31(7): 793-798
doi: 10.3724/SP.J.1095.2014.30454
Abstract:
Four furan acylhydrazones derivatives(4a~4d) were synthesized from 2-furancarbaldehyde and benzohydrazide derivatives and characterized by using elemental analysis,1H NMR,FT-IR,UV and fluorescence spectroscopy methods.The results show that the 2D chain layered structure was assembled through intermolecular hydrogen bonds and face to face π…π stacking interactions of the furan rings.The single crystal of acylhydrazone 4a was obtained through the solvent evaporation method.Its crystal and molecular structures were determined through X-ray scattering.Fluorescence test shows that the acylhydrazone 4c has strong fluorescence.All furan acylhydrazones were screened for their antibacterial activities to Escherichia coli,Staphylococcus aureus and Pseudomonas aeruginosa by agar diffusion method.The result shows that acylhydrazone 4c has very significant antibacterial activity to Staphylococcus aureus.
Four furan acylhydrazones derivatives(4a~4d) were synthesized from 2-furancarbaldehyde and benzohydrazide derivatives and characterized by using elemental analysis,1H NMR,FT-IR,UV and fluorescence spectroscopy methods.The results show that the 2D chain layered structure was assembled through intermolecular hydrogen bonds and face to face π…π stacking interactions of the furan rings.The single crystal of acylhydrazone 4a was obtained through the solvent evaporation method.Its crystal and molecular structures were determined through X-ray scattering.Fluorescence test shows that the acylhydrazone 4c has strong fluorescence.All furan acylhydrazones were screened for their antibacterial activities to Escherichia coli,Staphylococcus aureus and Pseudomonas aeruginosa by agar diffusion method.The result shows that acylhydrazone 4c has very significant antibacterial activity to Staphylococcus aureus.
2014, 31(7): 799-805
doi: 10.3724/SP.J.1095.2014.30511
Abstract:
A newly Co2+ coordinated metal-organic framework had been successfully synthesized via one-step post-functionalization by hydrothermal method and characterized by Fourier transform infrared spectrometer,N2 adsorption and inductively coupled plasma.Using O2 as oxidant,mesoporous cobalt metal-organic framework was investigated as a heterogeneous catalytic material for the epoxidation of various olefins.Among them,the conversion of cyclooctene and the selectivity of epoxycyclooctane are 94% and 91%,respectively,and the turnover frequency is 509 h-1.PCN-100(Co) exhibits excellent stabilities in 5 recycles without any loss of catalytic performance.
A newly Co2+ coordinated metal-organic framework had been successfully synthesized via one-step post-functionalization by hydrothermal method and characterized by Fourier transform infrared spectrometer,N2 adsorption and inductively coupled plasma.Using O2 as oxidant,mesoporous cobalt metal-organic framework was investigated as a heterogeneous catalytic material for the epoxidation of various olefins.Among them,the conversion of cyclooctene and the selectivity of epoxycyclooctane are 94% and 91%,respectively,and the turnover frequency is 509 h-1.PCN-100(Co) exhibits excellent stabilities in 5 recycles without any loss of catalytic performance.
2014, 31(7): 806-811
doi: 10.3724/SP.J.1095.2014.30458
Abstract:
The modified mesoporous zeolites Al-FSM-16,Zr-FSM-16,and Al-Zr-ESM-16 were synthesized using cetyltrimethyl ammonium bromide(CTMAB) as the template,and characterized by XRD,IR,SEM,and BET.These catalysts were evaluated for synthesis of 3-(2-methyl-1H-indol-3-yl) cyclohexanone by catalytic Michael addition of 2-methylindole to cyclohex-2-enone under a solvent free condition.Al and Zr doping into the skeleton of the molecular sieve leads to larger pores molecular sieve,but the skeleton structure does not change significantly.Al or Zr doping increases the catalytic activity of FSM-16 molecular sieves and the Zr-FSM-16 molecular sieve has better activity.Under the following optimum reaction conditions:catalyst dosage 7.5%,molar ratio of cyclohex-2-enone to 2-methylindole being 1:1.1,reaction temperature 80℃ and reaction time 120 min,the yield of 3-(2-methyl-1H-indol-3-yl) cyclohexanone is up to 75.4%.
The modified mesoporous zeolites Al-FSM-16,Zr-FSM-16,and Al-Zr-ESM-16 were synthesized using cetyltrimethyl ammonium bromide(CTMAB) as the template,and characterized by XRD,IR,SEM,and BET.These catalysts were evaluated for synthesis of 3-(2-methyl-1H-indol-3-yl) cyclohexanone by catalytic Michael addition of 2-methylindole to cyclohex-2-enone under a solvent free condition.Al and Zr doping into the skeleton of the molecular sieve leads to larger pores molecular sieve,but the skeleton structure does not change significantly.Al or Zr doping increases the catalytic activity of FSM-16 molecular sieves and the Zr-FSM-16 molecular sieve has better activity.Under the following optimum reaction conditions:catalyst dosage 7.5%,molar ratio of cyclohex-2-enone to 2-methylindole being 1:1.1,reaction temperature 80℃ and reaction time 120 min,the yield of 3-(2-methyl-1H-indol-3-yl) cyclohexanone is up to 75.4%.
2014, 31(7): 812-816
doi: 10.3724/SP.J.1095.2014.30480
Abstract:
A functionalized ionic liquid-supported proline,1-methyl-3-{2-[(2s)-pyrrolidine-2-carbonyloxy]-ethyl}-1H-imidazol-3-iumtrifluoroacetate([Promim]CF3CO2),was used to catalyze the Henry condensation reaction of aldehydes with CH3CH2NO2 or CH3NO2.The desired products were obtained in 79%~95% yields,diastereomeric excess and enantiomeric excess was up to 3:1 and 85% under relatively mild conditions.[Promim]CF3CO2 could be efficiently recycled six times without the decrease of catalytic activity in the condensation reaction of 4-nitrobenzaldehyde and CH3CH2NO2.
A functionalized ionic liquid-supported proline,1-methyl-3-{2-[(2s)-pyrrolidine-2-carbonyloxy]-ethyl}-1H-imidazol-3-iumtrifluoroacetate([Promim]CF3CO2),was used to catalyze the Henry condensation reaction of aldehydes with CH3CH2NO2 or CH3NO2.The desired products were obtained in 79%~95% yields,diastereomeric excess and enantiomeric excess was up to 3:1 and 85% under relatively mild conditions.[Promim]CF3CO2 could be efficiently recycled six times without the decrease of catalytic activity in the condensation reaction of 4-nitrobenzaldehyde and CH3CH2NO2.
2014, 31(7): 817-822
doi: 10.3724/SP.J.1095.2014.30463
Abstract:
A series of silica supported cesium salts of molybdovanadophosphoric acid catalysts with different loadings was prepared by sol-gel technology.Their properties were verified by XRD,IR spectra,SEM and physical adsorption technology.The catalytic activity of these catalysts was evaluated for the liquid phase nitration of phenol with dilute nitric acid under mild conditions.The effects of various parameters on the nitration were tested,which included reaction time,catalyst loading and reactants ratio.The results indicate that the catalyst prepared has the Keggin type structure and these particles are well dispersed on the surface of silica.The catalysts exhibit strong activity and high selectivity toward the o-nitration of phenol with a yield of 88% under appropriate conditions.Moreover,the supported catalysts can be recovered simply and reused several times.After the nitration,the o-nitrophenol obtained can be extracted via steam distillation.
A series of silica supported cesium salts of molybdovanadophosphoric acid catalysts with different loadings was prepared by sol-gel technology.Their properties were verified by XRD,IR spectra,SEM and physical adsorption technology.The catalytic activity of these catalysts was evaluated for the liquid phase nitration of phenol with dilute nitric acid under mild conditions.The effects of various parameters on the nitration were tested,which included reaction time,catalyst loading and reactants ratio.The results indicate that the catalyst prepared has the Keggin type structure and these particles are well dispersed on the surface of silica.The catalysts exhibit strong activity and high selectivity toward the o-nitration of phenol with a yield of 88% under appropriate conditions.Moreover,the supported catalysts can be recovered simply and reused several times.After the nitration,the o-nitrophenol obtained can be extracted via steam distillation.
2014, 31(7): 823-827
doi: 10.3724/SP.J.1095.2014.30499
Abstract:
Complexes of oleanolic acid(OA) and alkanolamines(EAs)[Ethanolamine(MEA),diethanolamine(DEA) or triethanolamine(TEA)]were prepared by an ultrasonic method.The complexes were characterized by DSC,XRD,IR and Raman spectroscopy.It was found that the complexes is formed through the intermolecular force between OA and EAs rather than chemical bonding.The solubility of OA-EAs complexes is much higher than that of OA.The present study supplies a novel concept for the design of an efficient delivery system of OA.
Complexes of oleanolic acid(OA) and alkanolamines(EAs)[Ethanolamine(MEA),diethanolamine(DEA) or triethanolamine(TEA)]were prepared by an ultrasonic method.The complexes were characterized by DSC,XRD,IR and Raman spectroscopy.It was found that the complexes is formed through the intermolecular force between OA and EAs rather than chemical bonding.The solubility of OA-EAs complexes is much higher than that of OA.The present study supplies a novel concept for the design of an efficient delivery system of OA.
2014, 31(7): 828-834
doi: 10.3724/SP.J.1095.2014.30607
Abstract:
Firstly oleic acid and sodium undecylenate modified water-soluble magnetic fluid was prepared.Then in the presence of water-based magnetic fluid,fluorescent magnetic nanoparticles were successfully synthesized by soap-free and seeded emulsion polymerization of rare earth complex monomer Eu(AA)3Phen(AA=acrylic acid,phen=1,10-phenanthroline) polymerized with styrene(St) and glycidyl methacrylate(GMA) using potassium persulfate(KPS) as the initiator.The morphology and size of the products were characterized by transmission electron microscopy(TEM) and dynamic light scattering(DLS) granulometer.Experimental results show that the fluorescent magnetic nanoparticles have obvious core-shell structures.Their particle sizes are smaller than 100 nm and have narrow size distribution.The chemical and crystalline structures of the particles were analyzed by Fourier transform infrared spectroscopy(FTIR) and X-ray diffraction(XRD).The magnetic and fluorescent properties of the particles were characterized by vibrating sample magnetometer(VSM) and fluorescence spectrophotometer.These results show that the fluorescent nanoparticles exhibit the superparamagnetic property.Their fluorescence emission spectra show characteristic emission peaks of Eu3+ at 594 and 619 nm,respectively.
Firstly oleic acid and sodium undecylenate modified water-soluble magnetic fluid was prepared.Then in the presence of water-based magnetic fluid,fluorescent magnetic nanoparticles were successfully synthesized by soap-free and seeded emulsion polymerization of rare earth complex monomer Eu(AA)3Phen(AA=acrylic acid,phen=1,10-phenanthroline) polymerized with styrene(St) and glycidyl methacrylate(GMA) using potassium persulfate(KPS) as the initiator.The morphology and size of the products were characterized by transmission electron microscopy(TEM) and dynamic light scattering(DLS) granulometer.Experimental results show that the fluorescent magnetic nanoparticles have obvious core-shell structures.Their particle sizes are smaller than 100 nm and have narrow size distribution.The chemical and crystalline structures of the particles were analyzed by Fourier transform infrared spectroscopy(FTIR) and X-ray diffraction(XRD).The magnetic and fluorescent properties of the particles were characterized by vibrating sample magnetometer(VSM) and fluorescence spectrophotometer.These results show that the fluorescent nanoparticles exhibit the superparamagnetic property.Their fluorescence emission spectra show characteristic emission peaks of Eu3+ at 594 and 619 nm,respectively.
2014, 31(7): 835-840
doi: 10.3724/SP.J.1095.2014.30461
Abstract:
Dy3+ or Tm3+ doped zinc tetraborate(ZnB4O7) phosphors were prepared by the method of high temperature solid-state synthesis.The 3-dimensional thermoluminescent(TL) spectra of the phosphors after 60Co γ-ray radiation were measured at room temperature.The 3-dimensional TL spectra show that the main TL glow peaks of these phosphors appear at about 218℃.3-Dimensional emission spectra of main TL peaks for the ZnB4O7:Tm3+ phosphor are at 366,453,475,651 and 754 nm,while TL peaks for the ZnB4O7:Dy3+ phosphor are at 480,573,665 and 755 nm,respectively.The formation of all peaks is ascribed to the characteristic rare earth ion transitions of Tm3+ and Dy3+ .The ZnB4O7:Tm3+ phosphor exhibits a higher TL emission efficiency,indicating its latent applicability in the field of radiation dosimetry compared with the ZnB4O7:Dy3+ phosphor.The kinetics parameters of the main TL peak of the ZnB4O7:Tm3+ phosphor at 218℃ were investigated by using the peak shape method.This peak shows the second-order kinetics while the trap depth(E) and the frequency factor are evaluated as 1.64 eV and 3.42×1016 s-1,respectively.
Dy3+ or Tm3+ doped zinc tetraborate(ZnB4O7) phosphors were prepared by the method of high temperature solid-state synthesis.The 3-dimensional thermoluminescent(TL) spectra of the phosphors after 60Co γ-ray radiation were measured at room temperature.The 3-dimensional TL spectra show that the main TL glow peaks of these phosphors appear at about 218℃.3-Dimensional emission spectra of main TL peaks for the ZnB4O7:Tm3+ phosphor are at 366,453,475,651 and 754 nm,while TL peaks for the ZnB4O7:Dy3+ phosphor are at 480,573,665 and 755 nm,respectively.The formation of all peaks is ascribed to the characteristic rare earth ion transitions of Tm3+ and Dy3+ .The ZnB4O7:Tm3+ phosphor exhibits a higher TL emission efficiency,indicating its latent applicability in the field of radiation dosimetry compared with the ZnB4O7:Dy3+ phosphor.The kinetics parameters of the main TL peak of the ZnB4O7:Tm3+ phosphor at 218℃ were investigated by using the peak shape method.This peak shows the second-order kinetics while the trap depth(E) and the frequency factor are evaluated as 1.64 eV and 3.42×1016 s-1,respectively.
2014, 31(7): 841-846
doi: 10.3724/SP.J.1095.2014.30292
Abstract:
Gold nanoparticles were prepared by a bioreduction of chloroauric acid with vine tea powder extracts,and characterized by UV-Vis,TEM and size distribution.The process of biosynthesis was investigated by control variate method.The results show that pH of the reaction solution,temperature and the quantities of the chloroauric acid all have significant effects on the particle size,size distribution,morphology and stability of gold nanoparticles.At pH >6.47 or in the presence of excess vine tea powder extracts,gold nanoparticles tend to agglomerate and the size of gold nanoparticles increases with the temperature increasing.Therefore,an effective controllable green synthesis of gold nanoparticles can be realized by control variate method.
Gold nanoparticles were prepared by a bioreduction of chloroauric acid with vine tea powder extracts,and characterized by UV-Vis,TEM and size distribution.The process of biosynthesis was investigated by control variate method.The results show that pH of the reaction solution,temperature and the quantities of the chloroauric acid all have significant effects on the particle size,size distribution,morphology and stability of gold nanoparticles.At pH >6.47 or in the presence of excess vine tea powder extracts,gold nanoparticles tend to agglomerate and the size of gold nanoparticles increases with the temperature increasing.Therefore,an effective controllable green synthesis of gold nanoparticles can be realized by control variate method.
2014, 31(7): 847-851
doi: 10.3724/SP.J.1095.2014.30501
Abstract:
The intercalation reaction between aluminum dihydrogen tripolyphosphate(ATP) and organic amine such as methylamine,ethylamine,propylamine and butylamine were characterized by infrared,X-ray diffraction,scanning electron microscopy,energy disperses spectroscopy as well as gravitational thermal analysis and titration experiment.The results show that the organic amine is intercalated into the interlayer of ATP.The interlayer spacing of ATP is extended from 0.795 nm to 1.71 nm by intercalation of organic amine.The interlayer spacing of the intercalation compound is linear to the carbon number(Cn) of organic amine with d=0.229Cn+0.811 and R2=0.9986.Long molecule chains result in stripping tendency of the intercalation compounds.The acidity and thermal decomposition temperature of ATP are also changed after the intercalation of organic amine,but all layered particle morphologies are similar.
The intercalation reaction between aluminum dihydrogen tripolyphosphate(ATP) and organic amine such as methylamine,ethylamine,propylamine and butylamine were characterized by infrared,X-ray diffraction,scanning electron microscopy,energy disperses spectroscopy as well as gravitational thermal analysis and titration experiment.The results show that the organic amine is intercalated into the interlayer of ATP.The interlayer spacing of ATP is extended from 0.795 nm to 1.71 nm by intercalation of organic amine.The interlayer spacing of the intercalation compound is linear to the carbon number(Cn) of organic amine with d=0.229Cn+0.811 and R2=0.9986.Long molecule chains result in stripping tendency of the intercalation compounds.The acidity and thermal decomposition temperature of ATP are also changed after the intercalation of organic amine,but all layered particle morphologies are similar.
2014, 31(7): 852-859
doi: 10.3724/SP.J.1095.2014.30504
Abstract:
Two aryloxymethyl imidazolinium quaternary ammonium salts(phenoxymethyl imidazolinyl quaternary ammonium salt(POAI) and naphthoxymethyl imidazolinyl quaternary ammonium salt(NOAI)) were synthesized.Their corrosion inhibition and adsorption behaviors on A3 steel in 1 mol/L HCl solution were studied by mass loss and electrochemical techniques.The results show that the two compounds are good inhibitors for A3 steel in 1 mol/L HCl,and they are mixed-type corrosion inhibitors.NOAI was found to have a superior inhibition efficiency to POAI.The inhibition efficiency increases with the concentration of inhibitor and the temperature.The experimental results reveal that the adsorption processes are endothermic and belong to the chemical adsorption.The adsorption characteristics of inhibitors are followed by the Langemuir isotherm.
Two aryloxymethyl imidazolinium quaternary ammonium salts(phenoxymethyl imidazolinyl quaternary ammonium salt(POAI) and naphthoxymethyl imidazolinyl quaternary ammonium salt(NOAI)) were synthesized.Their corrosion inhibition and adsorption behaviors on A3 steel in 1 mol/L HCl solution were studied by mass loss and electrochemical techniques.The results show that the two compounds are good inhibitors for A3 steel in 1 mol/L HCl,and they are mixed-type corrosion inhibitors.NOAI was found to have a superior inhibition efficiency to POAI.The inhibition efficiency increases with the concentration of inhibitor and the temperature.The experimental results reveal that the adsorption processes are endothermic and belong to the chemical adsorption.The adsorption characteristics of inhibitors are followed by the Langemuir isotherm.
2014, 31(7): 860-864
doi: 10.3724/SP.J.1095.2014.30481
Abstract:
A graphene modified glassy carbon electrode(GN/GCE) was prepared.The electrochemical behavior of calcium dobesilate on the modified electrode was investigated in 0.05 mol/L H2SO4 by cyclic voltammetry.The GN/GCE shows an obvious electrocatalytic activity toward the redox reaction of calcium dobesilate and a new method for the determination of calcium dobesilate is established.On differential pulse voltammetry curves,a linear dependence of oxidation current versus calcium dobesilate concentration is obtained in the range of 2.0×10-9~1.2×10-6 mol/L,with a detection limit of 1.0×10-9 mol/L(S/N=3).The proposed method was applied to determine calcium dobesilate in capsule.The modified electrode shows excellent stability and reproducibility.
A graphene modified glassy carbon electrode(GN/GCE) was prepared.The electrochemical behavior of calcium dobesilate on the modified electrode was investigated in 0.05 mol/L H2SO4 by cyclic voltammetry.The GN/GCE shows an obvious electrocatalytic activity toward the redox reaction of calcium dobesilate and a new method for the determination of calcium dobesilate is established.On differential pulse voltammetry curves,a linear dependence of oxidation current versus calcium dobesilate concentration is obtained in the range of 2.0×10-9~1.2×10-6 mol/L,with a detection limit of 1.0×10-9 mol/L(S/N=3).The proposed method was applied to determine calcium dobesilate in capsule.The modified electrode shows excellent stability and reproducibility.
2014, 31(7): 865-870
doi: 10.3724/SP.J.1095.2014.30472
Abstract:
In pH 2.09~5.02 Britton-Robinson(BR) buffer medium,ceftriaxone(CTRX) reacts with acriflavine(AF) to form an 1:1 ion association complex,which results in quench of the fluorescence of acriflavine.The measurement wavelength of fluorescence quenching is located at λex/λem=266 nm/506 nm.The linear range for CTRX is from 0.056 mg/L to 5.0 mg/L,and its detection limit is 0.016 mg/L.The fluorescence spectra characteristics,the optimum reaction conditions and the effect of additive substances were investigated.The composition of ion-association complexes was discussed also.Based on the ion-association reaction,a high sensitive,simple and rapid method was proposed for the determination of CTRX.The method was applied for the determination of CTRX in human serum and urine samples with satisfactory results.
In pH 2.09~5.02 Britton-Robinson(BR) buffer medium,ceftriaxone(CTRX) reacts with acriflavine(AF) to form an 1:1 ion association complex,which results in quench of the fluorescence of acriflavine.The measurement wavelength of fluorescence quenching is located at λex/λem=266 nm/506 nm.The linear range for CTRX is from 0.056 mg/L to 5.0 mg/L,and its detection limit is 0.016 mg/L.The fluorescence spectra characteristics,the optimum reaction conditions and the effect of additive substances were investigated.The composition of ion-association complexes was discussed also.Based on the ion-association reaction,a high sensitive,simple and rapid method was proposed for the determination of CTRX.The method was applied for the determination of CTRX in human serum and urine samples with satisfactory results.
