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2008 Volume 25 Issue 6
2008, 25(6): 629-632
Abstract:
The effect of electrostatic field on the photodegradation of Methyl Orange (MO) with P25 TiO2 catalyst was investigated.The results showed that the effect of the electrostatic field is very different from the traditional electrically assisted photocatalysis (EAP).With the increase of the electrostatic field,the apparent photodegradation activity declined.The fastest degradation was obtained atc (TiO2)=0.5 g/L without electrostatic field.However,the degradation rate of the same system was lower under higher electrostatic fields.The apparent rate constant of the degradation reaction under 20 kV electrostatic field was only 56% of that in the same system without electrostatic field.Furthermore,under the 20 kV field,the photodegradation was independent of the dosage of TiO2.By comparing the particle size distribution and the sedimentation rate within and without electrostatic field,it was conduded that the effects of electrostatic field,such as the electrophoresis,the polarization and the destruction of surface charge layer,made the particles aggregate and deposit.The coagulation decreased the amount of the catalyst dispersed in the solutions,and finally,decreased the apparent rate constant of the degradation reaction.At the end,it was proposed that the coagulation effect could be used to recycle the TiO2 nanoparticles from the photodegraded wastewater.
The effect of electrostatic field on the photodegradation of Methyl Orange (MO) with P25 TiO2 catalyst was investigated.The results showed that the effect of the electrostatic field is very different from the traditional electrically assisted photocatalysis (EAP).With the increase of the electrostatic field,the apparent photodegradation activity declined.The fastest degradation was obtained atc (TiO2)=0.5 g/L without electrostatic field.However,the degradation rate of the same system was lower under higher electrostatic fields.The apparent rate constant of the degradation reaction under 20 kV electrostatic field was only 56% of that in the same system without electrostatic field.Furthermore,under the 20 kV field,the photodegradation was independent of the dosage of TiO2.By comparing the particle size distribution and the sedimentation rate within and without electrostatic field,it was conduded that the effects of electrostatic field,such as the electrophoresis,the polarization and the destruction of surface charge layer,made the particles aggregate and deposit.The coagulation decreased the amount of the catalyst dispersed in the solutions,and finally,decreased the apparent rate constant of the degradation reaction.At the end,it was proposed that the coagulation effect could be used to recycle the TiO2 nanoparticles from the photodegraded wastewater.
2008, 25(6): 633-636
Abstract:
The effects of pivotal experimental parameters,such as Te ion concentration and scan rate,on the mechanism of Te underpotential deposition (UPD) and its voltammetry characterization were studied with a system of Te underpotential deposition on Au substrate.The results show that the voltammetry characterization of Te underpotential deposition on Au surface was dependent on the Te ion concentration,and the variation in the metal ion concentration may affect the kinetics of the UPD process.Scan rate dependent cyclic voltammetry experiments reveal that the peak current of the Te UPD peak is not a linear function of the scan rate,v,but a linear function of a 2/3 power of the scan rate,v2/3.It was confirmed that Te UPD on Au obeyed a two-dimensional nucleation and growth mechanism.
The effects of pivotal experimental parameters,such as Te ion concentration and scan rate,on the mechanism of Te underpotential deposition (UPD) and its voltammetry characterization were studied with a system of Te underpotential deposition on Au substrate.The results show that the voltammetry characterization of Te underpotential deposition on Au surface was dependent on the Te ion concentration,and the variation in the metal ion concentration may affect the kinetics of the UPD process.Scan rate dependent cyclic voltammetry experiments reveal that the peak current of the Te UPD peak is not a linear function of the scan rate,v,but a linear function of a 2/3 power of the scan rate,v2/3.It was confirmed that Te UPD on Au obeyed a two-dimensional nucleation and growth mechanism.
2008, 25(6): 637-641
Abstract:
Continuous ZrO2 precursor fibers were prepared by the sol-gel method with zirconium oxychlorid as raw material,2-propyl as solvent,acetylacetone as complex,and then continuous ZrO2 fibers were obtained by sintering the precursor at 800℃.The chemistry structure and morphology of the fibers were studied by FT-IR,TGA,elemental analysis and SEM.The process and related influencing factors of the preparation of spinnable zirconium sol were studied.The results show that the zirconium sol has a good spinnability when n(zirconium oxychlorid):n(dioxogen)=1:3,reaction time is 6 h and aging temperature is 15℃.The main component of the ZrO2 precursor fibers is hydrous zirconia chelated by acetyl acetone.The mean diameter of the sintered ZrO2 fibers is about 15 μm;there are lots of nanometer pores in ZrO2 fibers,and cracks are found.
Continuous ZrO2 precursor fibers were prepared by the sol-gel method with zirconium oxychlorid as raw material,2-propyl as solvent,acetylacetone as complex,and then continuous ZrO2 fibers were obtained by sintering the precursor at 800℃.The chemistry structure and morphology of the fibers were studied by FT-IR,TGA,elemental analysis and SEM.The process and related influencing factors of the preparation of spinnable zirconium sol were studied.The results show that the zirconium sol has a good spinnability when n(zirconium oxychlorid):n(dioxogen)=1:3,reaction time is 6 h and aging temperature is 15℃.The main component of the ZrO2 precursor fibers is hydrous zirconia chelated by acetyl acetone.The mean diameter of the sintered ZrO2 fibers is about 15 μm;there are lots of nanometer pores in ZrO2 fibers,and cracks are found.
2008, 25(6): 642-646
Abstract:
In a 0.1 mol/L NaAc-HAc buffer solution (pH=5.0),the electrochemical behavior of 2,4-and 2,5-dinitrophenol was investigated at the glassy carbon electrode modified with multi walled carbon nanotube.Each of them exhibited sensitive reduction responses of nitryls.It was found that the reduction peak of nitryl of the position 4-nitrate group of 2,4-dinitrophenol showed great difference from that of the position 5-nitrate group of 2,5-dinitrophenol.The difference between the two reduction potentials was as large as 180 mV.By measuring the reduction signals of a mixed sample with linear sweep voltammetry,and improving the resolution by taking semi-derivatives,dinitrophenol isomers were determined simultaneously and quantitatively.The linear calibration ranges were 1.0×10-6~5.0×10-4 mol/L for both 2,4-and 2,5-dinitrophenol,with detection limits of 2.1×10-7 mol/L for 2,4- and 1.1×10-7 mol/L for 2,5-dinitrophenol,respectively.This method was applied to the detection of dinitrophenols in artificial wastewater,and the recovery was from 97.6% to 103.3%.
In a 0.1 mol/L NaAc-HAc buffer solution (pH=5.0),the electrochemical behavior of 2,4-and 2,5-dinitrophenol was investigated at the glassy carbon electrode modified with multi walled carbon nanotube.Each of them exhibited sensitive reduction responses of nitryls.It was found that the reduction peak of nitryl of the position 4-nitrate group of 2,4-dinitrophenol showed great difference from that of the position 5-nitrate group of 2,5-dinitrophenol.The difference between the two reduction potentials was as large as 180 mV.By measuring the reduction signals of a mixed sample with linear sweep voltammetry,and improving the resolution by taking semi-derivatives,dinitrophenol isomers were determined simultaneously and quantitatively.The linear calibration ranges were 1.0×10-6~5.0×10-4 mol/L for both 2,4-and 2,5-dinitrophenol,with detection limits of 2.1×10-7 mol/L for 2,4- and 1.1×10-7 mol/L for 2,5-dinitrophenol,respectively.This method was applied to the detection of dinitrophenols in artificial wastewater,and the recovery was from 97.6% to 103.3%.
2008, 25(6): 647-650
Abstract:
A mixture of glycine,sodium hydroxide and 5-(2-chlorophenyl) furan-2-carbonyl chloride in a water-petroleum ether solution containing phase transfer catalyst N(CH3)4 Br was refluxed,and sodium N-(5-(2-chlorophenyl) furan-2-formyl) glycine was prepared.After acidification of the sodium salt,N-(5-(2-chloro-phenyl) furan-2-formyl) glycine was obtained.With N,N'-dicyclohexylcarbodiimide (DCC) as dehydration agent,amine or hydrazide derivatives of N-(5-(2-chlorophenyl) furan-2-formyl)-glycine were prepared from the reaction of the sodium salt with substituted anilines or substituted benzohydrazides respectively in DMF.The structures of all the target compounds were confirmed by IR,1H NMR,MS,and elemental analysis.MTT assay showed that most of the target compounds possessed certain inhibition activity against K562 Cells at 1×10-4 g/mL in vitro.
A mixture of glycine,sodium hydroxide and 5-(2-chlorophenyl) furan-2-carbonyl chloride in a water-petroleum ether solution containing phase transfer catalyst N(CH3)4 Br was refluxed,and sodium N-(5-(2-chlorophenyl) furan-2-formyl) glycine was prepared.After acidification of the sodium salt,N-(5-(2-chloro-phenyl) furan-2-formyl) glycine was obtained.With N,N'-dicyclohexylcarbodiimide (DCC) as dehydration agent,amine or hydrazide derivatives of N-(5-(2-chlorophenyl) furan-2-formyl)-glycine were prepared from the reaction of the sodium salt with substituted anilines or substituted benzohydrazides respectively in DMF.The structures of all the target compounds were confirmed by IR,1H NMR,MS,and elemental analysis.MTT assay showed that most of the target compounds possessed certain inhibition activity against K562 Cells at 1×10-4 g/mL in vitro.
2008, 25(6): 651-655
Abstract:
Ten novel derivatives of 2-Aryloxymethylbenzimidazole-1-acetylhydrazines were synthesized efficiently and quickly by N-alkylation and hydrazinolysis of 2-aryloxy-methylbenzimidazoles and methyl 2-chloroacetate under MWI and PTC conditions in the presence of PEG-400 as the phase transfer catalyst.All the products were characterized by elemental analysis,FT-IR,1H NMR and 13C NMR.The preliminary biological activity tests show that all the compounds have the more regulating activities for the growth of wheat than that of heteroauxing.
Ten novel derivatives of 2-Aryloxymethylbenzimidazole-1-acetylhydrazines were synthesized efficiently and quickly by N-alkylation and hydrazinolysis of 2-aryloxy-methylbenzimidazoles and methyl 2-chloroacetate under MWI and PTC conditions in the presence of PEG-400 as the phase transfer catalyst.All the products were characterized by elemental analysis,FT-IR,1H NMR and 13C NMR.The preliminary biological activity tests show that all the compounds have the more regulating activities for the growth of wheat than that of heteroauxing.
2008, 25(6): 656-660
Abstract:
In a BR buffer medium of pH 4.5~5.5,sodium aescinate can be bound to Night blue dye to form a binding product of 1:1,which results in great enhancement of RRS and a new RRS spectrum appears.The maximum RRS peak was located at 416 nm and the intensity of RRS was directly proportional to the concentration of SA in a range of 0.025~20.0×10-6 g/mL for an NB-SA system.The method had high sensitivity and the detecting limit of SA (3σ) was 7.5×10-9 g/mL for an NB-SA system.The influences of some coexisiting substances were investigated.The RRS method was applied to the determination of trace amounts of sodium aescinate in injection samples,tablet samples and urine samples with satisfactory results.
In a BR buffer medium of pH 4.5~5.5,sodium aescinate can be bound to Night blue dye to form a binding product of 1:1,which results in great enhancement of RRS and a new RRS spectrum appears.The maximum RRS peak was located at 416 nm and the intensity of RRS was directly proportional to the concentration of SA in a range of 0.025~20.0×10-6 g/mL for an NB-SA system.The method had high sensitivity and the detecting limit of SA (3σ) was 7.5×10-9 g/mL for an NB-SA system.The influences of some coexisiting substances were investigated.The RRS method was applied to the determination of trace amounts of sodium aescinate in injection samples,tablet samples and urine samples with satisfactory results.
2008, 25(6): 661-664
Abstract:
The title complex[Cu4Cl4(bipy)2] was hydrothermally synthesized and its crystal structure was determined by X-ray diffraction.It belongs to triclinic system with space group P-1.The cell parameters are:a=0.743 7(2) nm,b=0.942 99(4) nm,c=0.950 88(4) nm,α=64.164(3)°,β=74.170(3)°,γ=88.757(3)°,V=0.573 77(16) nm3,Z=1,Dx=2.050 g/cm3,μ(MoKα)=4.139 mm-1,F(000)=348,R1=0.055 9,wR2=0.162 5.The title compound consists of molecular units constructed around a Cu4 parallelogram with obvious Cu…Cu bonds.The solid at room temperature exhibits intense red photoluminescence at 539 and 649 nm.Quantum chemistry calculations of the compound were performed with Guassian 03 program at HF/6-31G level to study the electronic structure and bonding characteristics.
The title complex[Cu4Cl4(bipy)2] was hydrothermally synthesized and its crystal structure was determined by X-ray diffraction.It belongs to triclinic system with space group P-1.The cell parameters are:a=0.743 7(2) nm,b=0.942 99(4) nm,c=0.950 88(4) nm,α=64.164(3)°,β=74.170(3)°,γ=88.757(3)°,V=0.573 77(16) nm3,Z=1,Dx=2.050 g/cm3,μ(MoKα)=4.139 mm-1,F(000)=348,R1=0.055 9,wR2=0.162 5.The title compound consists of molecular units constructed around a Cu4 parallelogram with obvious Cu…Cu bonds.The solid at room temperature exhibits intense red photoluminescence at 539 and 649 nm.Quantum chemistry calculations of the compound were performed with Guassian 03 program at HF/6-31G level to study the electronic structure and bonding characteristics.
2008, 25(6): 665-668
Abstract:
High density,well ordered,vertically aligned and uniform titanium oxide nanotube arrays were fabricated on the surface of pure titanium sheet by direct electrochemical anodic oxidation with 0.5% HF and 0.5% HF+1 mol/L (NH4)H2PO4 as the supporting electrolyte at 20 V.XRD and SEM techniques were used to characterize titanium oxide nanotube arrays.The XRD result shows that TiO2 showed the anatase phase after having been annealed for 1 hour under 400℃.SEM shows the length of nanotubes did not increase after reaction for 20 mins in an electrolyte solution of 0.5% HF.But in an electrolyte solution of 0.5% HF+1 mol/L (NH4)H2PO4,at 20 V after reaction for 15 h,the average diameter of nanotubes is about 70~90 nm,and the length of nanotubes is about 2.2 μm.Photo-electrochemical character curves were tested in an electrolyte solution of 1 mol/L KOH under the irradiation of a high-voltage mercury lamp,photocurrent is about 3.5 mA/cm2 for nanotubes with a length of 2.2 μm.With TiO2 nanotubes of 2.2 μm in length as anode,under illuminating of a high-voltage mercury lamp at 0.45 V bias potential,after 4 h,the COD degradation degree of Methylene Blue electrolyte (10 mg/L) is about 93%.
High density,well ordered,vertically aligned and uniform titanium oxide nanotube arrays were fabricated on the surface of pure titanium sheet by direct electrochemical anodic oxidation with 0.5% HF and 0.5% HF+1 mol/L (NH4)H2PO4 as the supporting electrolyte at 20 V.XRD and SEM techniques were used to characterize titanium oxide nanotube arrays.The XRD result shows that TiO2 showed the anatase phase after having been annealed for 1 hour under 400℃.SEM shows the length of nanotubes did not increase after reaction for 20 mins in an electrolyte solution of 0.5% HF.But in an electrolyte solution of 0.5% HF+1 mol/L (NH4)H2PO4,at 20 V after reaction for 15 h,the average diameter of nanotubes is about 70~90 nm,and the length of nanotubes is about 2.2 μm.Photo-electrochemical character curves were tested in an electrolyte solution of 1 mol/L KOH under the irradiation of a high-voltage mercury lamp,photocurrent is about 3.5 mA/cm2 for nanotubes with a length of 2.2 μm.With TiO2 nanotubes of 2.2 μm in length as anode,under illuminating of a high-voltage mercury lamp at 0.45 V bias potential,after 4 h,the COD degradation degree of Methylene Blue electrolyte (10 mg/L) is about 93%.
2008, 25(6): 669-672
Abstract:
Complexes PVA-Fe(Ⅲ),PVA-Zn(Ⅱ),PVA-Cd(Ⅱ) and PVA-Hg(Ⅱ) were synthesized by the coordination reaction of corresponding metal ions with polyvinyl alcohol (PVA) in solution.The complexes were characterized by IR,Raman and XPS.The IR spectra showed that νC-O shifted to lower wavenumbers by 8~11 cm-1 from 1 094 cm-1(PVA),and νC-C shifted to lower wavenumbers by 3~8 cm-1 from 1 430 cm-1(PVA).The Raman spectra of the complexes indicated that there was a new metal-oxygen absorption peak in the 200~400 cm-1 region.The XPS spectrum of PVA-Fe(Ⅲ) indicated that the binding energies of O1s(533.0 eV),C1s(285.0 eV) and Fe2p(712.0 eV) were different for PVA[O1s(532.5 eV),C1s(284.6 eV)]and FeCl3[Fe2p(711.2 eV)].The above results showed that a coordination bond was formed between the hydroxide oxygen in PVA and the empty orbital in the metal ions.The anti-bacterial experiment results showed that the anti-bacterial activity of PVA-Hg(Ⅱ) complex to escherichia coli,bacillus subtilis and staphylococcus aureus were very good,the anti-bacterial activity of PVA-Zn(Ⅱ) was weak,and PVA-Zn(Ⅱ) and PVA-Cd(Ⅱ) had no anti-bacterial activity.
Complexes PVA-Fe(Ⅲ),PVA-Zn(Ⅱ),PVA-Cd(Ⅱ) and PVA-Hg(Ⅱ) were synthesized by the coordination reaction of corresponding metal ions with polyvinyl alcohol (PVA) in solution.The complexes were characterized by IR,Raman and XPS.The IR spectra showed that νC-O shifted to lower wavenumbers by 8~11 cm-1 from 1 094 cm-1(PVA),and νC-C shifted to lower wavenumbers by 3~8 cm-1 from 1 430 cm-1(PVA).The Raman spectra of the complexes indicated that there was a new metal-oxygen absorption peak in the 200~400 cm-1 region.The XPS spectrum of PVA-Fe(Ⅲ) indicated that the binding energies of O1s(533.0 eV),C1s(285.0 eV) and Fe2p(712.0 eV) were different for PVA[O1s(532.5 eV),C1s(284.6 eV)]and FeCl3[Fe2p(711.2 eV)].The above results showed that a coordination bond was formed between the hydroxide oxygen in PVA and the empty orbital in the metal ions.The anti-bacterial experiment results showed that the anti-bacterial activity of PVA-Hg(Ⅱ) complex to escherichia coli,bacillus subtilis and staphylococcus aureus were very good,the anti-bacterial activity of PVA-Zn(Ⅱ) was weak,and PVA-Zn(Ⅱ) and PVA-Cd(Ⅱ) had no anti-bacterial activity.
2008, 25(6): 673-676
Abstract:
Dithiocarbamate-modified chitosan (chitosan xanthogenate,DTC-CTS) was characterized respectively by infrared,UV-Vis and Thermogravimetry.The different adsorbing capacities of DTC-CTS and CTS for Cu2+ in aqueous solution were compared.The effects of pH,temperature,time and degree of substitution on the adsorbing capacity were investigated.The results demonstrate that the higher the degree of substitution,the better the adsorbing capacity.The optimum pH range of adsorption of DTC-CTS for Cu2+ is 6.0~7.0,the optimum adsorption temperature is 40℃,the optimum adsorption time is 0.5 h.Under such conditions,the adsorbing content of DTC-CTS for Cu2+ is 349.5 mg/g,which is 7% more than that of CTS.Adsorbed Cu2+ can be quantitatively eluted from DTC-CTS with 10% ammonia at a washing off rate of 96%.DTC-CTS can be used for repeatedly three times.
Dithiocarbamate-modified chitosan (chitosan xanthogenate,DTC-CTS) was characterized respectively by infrared,UV-Vis and Thermogravimetry.The different adsorbing capacities of DTC-CTS and CTS for Cu2+ in aqueous solution were compared.The effects of pH,temperature,time and degree of substitution on the adsorbing capacity were investigated.The results demonstrate that the higher the degree of substitution,the better the adsorbing capacity.The optimum pH range of adsorption of DTC-CTS for Cu2+ is 6.0~7.0,the optimum adsorption temperature is 40℃,the optimum adsorption time is 0.5 h.Under such conditions,the adsorbing content of DTC-CTS for Cu2+ is 349.5 mg/g,which is 7% more than that of CTS.Adsorbed Cu2+ can be quantitatively eluted from DTC-CTS with 10% ammonia at a washing off rate of 96%.DTC-CTS can be used for repeatedly three times.
2008, 25(6): 677-680
Abstract:
An efficient and high-yield synthesis of 3-methoxy-4-formylphenonyl p-methylbensulphonate (5) was accomplished with vanillin as the starting material in three steps.It involved the converstion of vanillin into hydrazine (4) and the metalic reduction of hydrazine 4 into the intermediate vanillic amine.The phosphonium 6 was synthesized in solid phase by the reaction of 6-bromohexyoic acid with triphenylphosphine,and then the Wittig condensation of phosphonium 6 with iso-butanol afforded 8-methoxynon-cis-6-enoic acid (7).Finally,compound 7 was connected with the amine 5,and then was hydrolyzed to the target compound under ultrasonic condition.IR,NMR and HRMS were used to confirm the structure of the title compound.
An efficient and high-yield synthesis of 3-methoxy-4-formylphenonyl p-methylbensulphonate (5) was accomplished with vanillin as the starting material in three steps.It involved the converstion of vanillin into hydrazine (4) and the metalic reduction of hydrazine 4 into the intermediate vanillic amine.The phosphonium 6 was synthesized in solid phase by the reaction of 6-bromohexyoic acid with triphenylphosphine,and then the Wittig condensation of phosphonium 6 with iso-butanol afforded 8-methoxynon-cis-6-enoic acid (7).Finally,compound 7 was connected with the amine 5,and then was hydrolyzed to the target compound under ultrasonic condition.IR,NMR and HRMS were used to confirm the structure of the title compound.
2008, 25(6): 681-684
Abstract:
Carboxymethyl-β-cyclodextrin (CM-β-CD) was separately prepared by dry process and wet process.CM-β-CD was characterized by Fourier transform infrared spectrometry (FTIR),and then its solubi-lity,degree of substitution,reaction energy and yield were determined.The results show that reaction effect of dry process is from 37% to 46%,while yield of about 83%.The dry process has a higher reaction energy and a higher yield than the wet process.The optimum conditions of the dry preparation are the mole ratio of chloroacetic acid to β-cyclodextrin is 6,reaction temperature is 40℃,reaction time is 4 h.
Carboxymethyl-β-cyclodextrin (CM-β-CD) was separately prepared by dry process and wet process.CM-β-CD was characterized by Fourier transform infrared spectrometry (FTIR),and then its solubi-lity,degree of substitution,reaction energy and yield were determined.The results show that reaction effect of dry process is from 37% to 46%,while yield of about 83%.The dry process has a higher reaction energy and a higher yield than the wet process.The optimum conditions of the dry preparation are the mole ratio of chloroacetic acid to β-cyclodextrin is 6,reaction temperature is 40℃,reaction time is 4 h.
2008, 25(6): 685-688
Abstract:
Gel polymer electrolytes comprising 1-butyl-3-methylimidazolium-chloride-ZnCl2[BMM](Cl-ZnCl2) Lewis acid room temperature ionic liquid in PMMA matrix were prepared by means of in situ radical polymerization of vinyl monomers.The polymer matrix was formed by free radical polymerization of methyl methacrylate (MMA) monomers.Structure and properities of the product were studied by FTIR,AC,TG,GPC.The interactions and structure changes of [BMM]Cl-ZnCl2/PMMA were investigated by FTIR,which showed composites structure.When n([BMM]Cl-ZnCl2):n(MMA) is 7:3,the gel polymer electrolyte showed the maximum ionic conductivity of about 0.36×10-3 S/cm at room temperature.The gel polymer electrolytes had greater thermal stability than the traditional non-aqueous electrolyte systems including organic solvent.They exhibited high decomposition temperatures above 286℃.Mw/Mn ratios of the gel polymer electrolytes were decresed as [BMM]Cl-ZnCl2 mol content increased,which showed narrower molecular mass distribution.Ionic conductivities of the gel polymer electrolytes were increased as [BMM]Cl-ZnCl2 mol content increased.
Gel polymer electrolytes comprising 1-butyl-3-methylimidazolium-chloride-ZnCl2[BMM](Cl-ZnCl2) Lewis acid room temperature ionic liquid in PMMA matrix were prepared by means of in situ radical polymerization of vinyl monomers.The polymer matrix was formed by free radical polymerization of methyl methacrylate (MMA) monomers.Structure and properities of the product were studied by FTIR,AC,TG,GPC.The interactions and structure changes of [BMM]Cl-ZnCl2/PMMA were investigated by FTIR,which showed composites structure.When n([BMM]Cl-ZnCl2):n(MMA) is 7:3,the gel polymer electrolyte showed the maximum ionic conductivity of about 0.36×10-3 S/cm at room temperature.The gel polymer electrolytes had greater thermal stability than the traditional non-aqueous electrolyte systems including organic solvent.They exhibited high decomposition temperatures above 286℃.Mw/Mn ratios of the gel polymer electrolytes were decresed as [BMM]Cl-ZnCl2 mol content increased,which showed narrower molecular mass distribution.Ionic conductivities of the gel polymer electrolytes were increased as [BMM]Cl-ZnCl2 mol content increased.
2008, 25(6): 689-692
Abstract:
Different organic reagents were selected to modify the pyrophyllite with wet activation technics,and the adsorption behavior of the modified pyrophyllite for polar hydroquinone in water was tested.The result states that the adsorption capacity of modified pyrophyllite powder is greatly increased in comparison with that of natural pyrophyllite.The modified pyrophyllite can adsorb 83.1% of hydroquinone molecules,while natural pyrophyllite did only 26.8% of them.The optimized conditions of nature pyrophyllite adsorbing hydroquinone in water are particle size less than 7.9 μm,ratio of pyrophyllite to hydroquinone solution 1:8,pH value of solutions 6.05~6.25 and reacting time 25 min.The optimized conditions of activation are reagents quantity 1%,temperature 75℃ and reacting time 2 h.The optimized conditions of modified pyrophyllite adsorbing hydroquinone in water are ratio of pyrophyllite to hydroquinone solution 1:8,pH value of solution 6~7 and reacting time 30 min.Meanwhile,XRD,IR and SEM methods were used to characterise the structure of the sample,and the mechanisms of modification were discussed.
Different organic reagents were selected to modify the pyrophyllite with wet activation technics,and the adsorption behavior of the modified pyrophyllite for polar hydroquinone in water was tested.The result states that the adsorption capacity of modified pyrophyllite powder is greatly increased in comparison with that of natural pyrophyllite.The modified pyrophyllite can adsorb 83.1% of hydroquinone molecules,while natural pyrophyllite did only 26.8% of them.The optimized conditions of nature pyrophyllite adsorbing hydroquinone in water are particle size less than 7.9 μm,ratio of pyrophyllite to hydroquinone solution 1:8,pH value of solutions 6.05~6.25 and reacting time 25 min.The optimized conditions of activation are reagents quantity 1%,temperature 75℃ and reacting time 2 h.The optimized conditions of modified pyrophyllite adsorbing hydroquinone in water are ratio of pyrophyllite to hydroquinone solution 1:8,pH value of solution 6~7 and reacting time 30 min.Meanwhile,XRD,IR and SEM methods were used to characterise the structure of the sample,and the mechanisms of modification were discussed.
2008, 25(6): 693-696
Abstract:
In pH=1.98 buffer solution,dipyridamole associates with eosine Y and produces a greatly enhanced resonance light scattering (RLS) signals at 315 nm.It was found that the enhanced RLS intensity (ΔIRLS) at 315 nm is proportional to the concentration of dipyridamole,and thus a new method for determining trace dipyridamole has been established accordingly.This method has an advantage of simplicity in experi-mental operation and conditon.The determination limit of dipyridamole is 16.1 nmol/L when the concentrations of eosine Y is 3.0×10-5 mol/L.Simultaneously this method has been successfully applied to the actual samples,and the relatively standard deviation between 1.3% 2.5%,the recovery rate of actual sample is about (99.2±3.3)%~(102.0±1.7)%,indicating that this analysis method has the good determination accuracy and the reliability.
In pH=1.98 buffer solution,dipyridamole associates with eosine Y and produces a greatly enhanced resonance light scattering (RLS) signals at 315 nm.It was found that the enhanced RLS intensity (ΔIRLS) at 315 nm is proportional to the concentration of dipyridamole,and thus a new method for determining trace dipyridamole has been established accordingly.This method has an advantage of simplicity in experi-mental operation and conditon.The determination limit of dipyridamole is 16.1 nmol/L when the concentrations of eosine Y is 3.0×10-5 mol/L.Simultaneously this method has been successfully applied to the actual samples,and the relatively standard deviation between 1.3% 2.5%,the recovery rate of actual sample is about (99.2±3.3)%~(102.0±1.7)%,indicating that this analysis method has the good determination accuracy and the reliability.
2008, 25(6): 697-701
Abstract:
CePO4 fluorescence nanomaterials with different crystal structures and morphology was hydrothermally synthesized and characterized with the techniques of X-ray diffraction (XRD),transmission electron microscopy (TEM),scanning electron microscopy (SEM) and fluorescence spectroscopy,etc.The effects of pH and temperature on the crystal structure,morphology and fluorescent intensity of CePO4 were investigated.The SEM results indicated that CePO4 prepared in acidic solution (pH=1,120℃) were nanorods,while CePO4 prepared in alkaline solution (pH=12,120℃) were nanoparticles.The XRD results showed that CePO4 prepared in acidic (pH=1,120℃) solution had a hexagonal crystal structure.However,the crystallinity of CePO4 obtained in the acidic solution was better than that of CePO4 obtained in the alkaline solution.The crystal structure of CePO4 depended on the preparation temperature.The CePO4 had a hexagonal crystal structure when it was prepared at 120℃ and pH=1.CePO4 with monoclinic and hexagonal crystal structures can be simultaneously formed with increasing the preparation temperature.Only CePO4 with the monoclinic structure was obtained when the temperature was 200℃.Fluorescence spectra indicated that both hexagonal and monoclinic CePO4 showed a broad emission band at between 300~400 nm due to the 5d-4f emission of cerium.However,the fluorescence intensity of the monoclinic CePO4 was stronger than that of hexagonal one.
CePO4 fluorescence nanomaterials with different crystal structures and morphology was hydrothermally synthesized and characterized with the techniques of X-ray diffraction (XRD),transmission electron microscopy (TEM),scanning electron microscopy (SEM) and fluorescence spectroscopy,etc.The effects of pH and temperature on the crystal structure,morphology and fluorescent intensity of CePO4 were investigated.The SEM results indicated that CePO4 prepared in acidic solution (pH=1,120℃) were nanorods,while CePO4 prepared in alkaline solution (pH=12,120℃) were nanoparticles.The XRD results showed that CePO4 prepared in acidic (pH=1,120℃) solution had a hexagonal crystal structure.However,the crystallinity of CePO4 obtained in the acidic solution was better than that of CePO4 obtained in the alkaline solution.The crystal structure of CePO4 depended on the preparation temperature.The CePO4 had a hexagonal crystal structure when it was prepared at 120℃ and pH=1.CePO4 with monoclinic and hexagonal crystal structures can be simultaneously formed with increasing the preparation temperature.Only CePO4 with the monoclinic structure was obtained when the temperature was 200℃.Fluorescence spectra indicated that both hexagonal and monoclinic CePO4 showed a broad emission band at between 300~400 nm due to the 5d-4f emission of cerium.However,the fluorescence intensity of the monoclinic CePO4 was stronger than that of hexagonal one.
2008, 25(6): 702-705
Abstract:
The electrocatalytic oxidation of N-Acetyl-L-Cysteine (NAC) at a 10-methylphenothiazine (MPT) modified carbon paste electrode (MPT/CPE) was investigated by cyclic voltammetry (CV).Although NAC itself showed a very poor electrochemical response at a carbon paste electrode (CPE),the response could be greatly enhanced at MPT/CPE,which enables a sensitive electrochemical determination of substrate NAC.The reaction rate constant for the catalytic oxidation was evaluated to be (1.59±0.03)×103(mol·L-1)-1·s-1 by chronoamperometry (CA).The catalytic oxidation peak current of NAC vs its concentration had a good linear relationship in concentration range of 1.0×10-6~1.3×10-3 mol/L with a correlation coefficient of 0.999 3,and a detection limit of 8.0×10-7 mol/L by linear sweep voltammetry (LSV).This method can be applied to the determination of real samples.
The electrocatalytic oxidation of N-Acetyl-L-Cysteine (NAC) at a 10-methylphenothiazine (MPT) modified carbon paste electrode (MPT/CPE) was investigated by cyclic voltammetry (CV).Although NAC itself showed a very poor electrochemical response at a carbon paste electrode (CPE),the response could be greatly enhanced at MPT/CPE,which enables a sensitive electrochemical determination of substrate NAC.The reaction rate constant for the catalytic oxidation was evaluated to be (1.59±0.03)×103(mol·L-1)-1·s-1 by chronoamperometry (CA).The catalytic oxidation peak current of NAC vs its concentration had a good linear relationship in concentration range of 1.0×10-6~1.3×10-3 mol/L with a correlation coefficient of 0.999 3,and a detection limit of 8.0×10-7 mol/L by linear sweep voltammetry (LSV).This method can be applied to the determination of real samples.
2008, 25(6): 706-709
Abstract:
Particulate sorbent with substantially reduced valence promoter metal nickel supported on Zinc Titanate or Zinc Ferrite provides a system for the desulfurization of a feed stream of FCC gasoline.The optimum preparation conditions for this sorbent were that the concentration of nickel nitrate was 10 mol/L,dipping time 1 h,baking temperature 600℃,and baking time 1 h.The sorbent exhibited an excellent desulfurization capacity in a fixed-bed absorber at 350℃ and 0.75 MPa.Sulfur content in FCC gasoline was reduced to 50 μg/g;the lifetime of the regenerated sorbent was 150 h;the octane number was about 89 when the ratio of H2/gasoline was optimum;the yield of gasoline was about 98%;the amount of end hydrogen (400 mL/min) can influence the effect of desulfurization.
Particulate sorbent with substantially reduced valence promoter metal nickel supported on Zinc Titanate or Zinc Ferrite provides a system for the desulfurization of a feed stream of FCC gasoline.The optimum preparation conditions for this sorbent were that the concentration of nickel nitrate was 10 mol/L,dipping time 1 h,baking temperature 600℃,and baking time 1 h.The sorbent exhibited an excellent desulfurization capacity in a fixed-bed absorber at 350℃ and 0.75 MPa.Sulfur content in FCC gasoline was reduced to 50 μg/g;the lifetime of the regenerated sorbent was 150 h;the octane number was about 89 when the ratio of H2/gasoline was optimum;the yield of gasoline was about 98%;the amount of end hydrogen (400 mL/min) can influence the effect of desulfurization.
2008, 25(6): 710-713
Abstract:
The indirect determination of boron and phosphorus in steel was invesgitated by flame atom absorption spectrometry (FAAS) method with extraction.1,2-Dichloroethane was used to extract the associate consisting of borax,phenylhydroxyacetic acid and[Fe(phen)3]2+ in a weak acid,then Fe of the associate was stripped with water.Methyl isobutyl ketone was used for extracting phosphomolybdate complex in the acid.The content of boron and phosphorus was investigated in steel samples by determining the amount of iron in the water phase and molybdenum in organic phase by flame atom absorption spectrometry.The dynamic calibration curves of boron and phosphorus were obtained within 0.04~1.00 mg/L and 0.12~3.24 mg/L respectively.The limits of detections are 0.036 mg/L for boron and 0.015 mg/L for phosphorus.This method has the advantages of simple operation,good selectivity and low detection limit,showing a good potential to determine trace boron in steel.
The indirect determination of boron and phosphorus in steel was invesgitated by flame atom absorption spectrometry (FAAS) method with extraction.1,2-Dichloroethane was used to extract the associate consisting of borax,phenylhydroxyacetic acid and[Fe(phen)3]2+ in a weak acid,then Fe of the associate was stripped with water.Methyl isobutyl ketone was used for extracting phosphomolybdate complex in the acid.The content of boron and phosphorus was investigated in steel samples by determining the amount of iron in the water phase and molybdenum in organic phase by flame atom absorption spectrometry.The dynamic calibration curves of boron and phosphorus were obtained within 0.04~1.00 mg/L and 0.12~3.24 mg/L respectively.The limits of detections are 0.036 mg/L for boron and 0.015 mg/L for phosphorus.This method has the advantages of simple operation,good selectivity and low detection limit,showing a good potential to determine trace boron in steel.
2008, 25(6): 714-717
Abstract:
Poly(N-methyl-N-p-vinylbenzylacetamide) resin was prepared from macroporous crosslinked chloro-methylated polystyrene by methylamination and acetylation,and in the process the chlorine content of the resin decreased from 3.95 mmol/g to 0.63 mmol/g.Adsorption isotherm of phenol onto the resin from aqua was measured,and the equilibrium data can be characterized by Freundlich isotherms.The enthalpy,free energy,and entropy for the adsorption were calculated according to thermodynamic function relationships.The adsorption enthalpy was -24.65~-71.20 kJ/mol,the adsorption free energy -4.64~-6.07 kJ/mol,and the adsorption entropy -62.35~-218.56 J/(mol·K),when the adsorption capacity was in the range of 10~40 mg/g.In addition,the adsorption mechanism of hydrogen bonding and hydrophobic interaction was discussed.This functionalized resin may be applied in the removal of phenol in the wastewater with phenolic compounds and the extraction of active components with hydrogen bonding donator of Chinese traditional and herbal drugs.
Poly(N-methyl-N-p-vinylbenzylacetamide) resin was prepared from macroporous crosslinked chloro-methylated polystyrene by methylamination and acetylation,and in the process the chlorine content of the resin decreased from 3.95 mmol/g to 0.63 mmol/g.Adsorption isotherm of phenol onto the resin from aqua was measured,and the equilibrium data can be characterized by Freundlich isotherms.The enthalpy,free energy,and entropy for the adsorption were calculated according to thermodynamic function relationships.The adsorption enthalpy was -24.65~-71.20 kJ/mol,the adsorption free energy -4.64~-6.07 kJ/mol,and the adsorption entropy -62.35~-218.56 J/(mol·K),when the adsorption capacity was in the range of 10~40 mg/g.In addition,the adsorption mechanism of hydrogen bonding and hydrophobic interaction was discussed.This functionalized resin may be applied in the removal of phenol in the wastewater with phenolic compounds and the extraction of active components with hydrogen bonding donator of Chinese traditional and herbal drugs.
2008, 25(6): 718-721
Abstract:
Nano-TiO2 powder prepared by sol-gel method was used to modify carbon paste electrode successfully.Optimum conditions for detection of trace indium at the modified electrode and the electrochemistry stability of the modified electrode were investigated by simultaneous cyclic voltammetry.There was a sensitive oxidation peak in the voltammogram at -0.832 V characteristic of trace indium in HAc-NaAc buffer whose pH was 5.4 when the accumulation time was 200 s and the potential scan rate was 200 mV/s.There was a good liner relationship between the peak current and In3+ concentration in a range of 1.0×10-11~1.0×10-9 mol/L with a correlation coefficient of 0.995,and the detection limit was 0.125×10-11 mol/L.This proposed method was applied to the analysis of actual water samples and the average recovery was 96.16%.The oxidation process of indium was controlled by both charge transfer and diffusion at the modified electrode.This oxidation process of indium was irreversible,and its average activation energy was 72.36 kJ/mol.
Nano-TiO2 powder prepared by sol-gel method was used to modify carbon paste electrode successfully.Optimum conditions for detection of trace indium at the modified electrode and the electrochemistry stability of the modified electrode were investigated by simultaneous cyclic voltammetry.There was a sensitive oxidation peak in the voltammogram at -0.832 V characteristic of trace indium in HAc-NaAc buffer whose pH was 5.4 when the accumulation time was 200 s and the potential scan rate was 200 mV/s.There was a good liner relationship between the peak current and In3+ concentration in a range of 1.0×10-11~1.0×10-9 mol/L with a correlation coefficient of 0.995,and the detection limit was 0.125×10-11 mol/L.This proposed method was applied to the analysis of actual water samples and the average recovery was 96.16%.The oxidation process of indium was controlled by both charge transfer and diffusion at the modified electrode.This oxidation process of indium was irreversible,and its average activation energy was 72.36 kJ/mol.
2008, 25(6): 722-725
Abstract:
A new method for the determination of trace amounts of zirconium was described.A multi-walled carbon nanotube modified carbon black microelectrode was prepared and the cathodic adsorptive voltammetric behavior of the zirconium-calcium-alizarin red S(ARS) mix-polynuclear complex at the modified electrode was investigated.Via the second derivative linear sweep technique,it was found that in a buffer solution of 0.096 mol/L acetic acid and 0.048 mol/L potassium biphthalate (pH=3.8),the complex adsorbed to the modified electrode,yielding one sensitive peak at -502 mV (vsSCE).The peak current of the complex was linearly correlated with Zr(Ⅳ) concentration in a range of 6.0×10-12~8.0×10-7 mol/L,and the detection limit was 4.0×10-12 mol/L (S/N=3) for 180 s accumulation.The method was applied to the determination of trace zirconium in ore samples and the results were satisfactory.
A new method for the determination of trace amounts of zirconium was described.A multi-walled carbon nanotube modified carbon black microelectrode was prepared and the cathodic adsorptive voltammetric behavior of the zirconium-calcium-alizarin red S(ARS) mix-polynuclear complex at the modified electrode was investigated.Via the second derivative linear sweep technique,it was found that in a buffer solution of 0.096 mol/L acetic acid and 0.048 mol/L potassium biphthalate (pH=3.8),the complex adsorbed to the modified electrode,yielding one sensitive peak at -502 mV (vsSCE).The peak current of the complex was linearly correlated with Zr(Ⅳ) concentration in a range of 6.0×10-12~8.0×10-7 mol/L,and the detection limit was 4.0×10-12 mol/L (S/N=3) for 180 s accumulation.The method was applied to the determination of trace zirconium in ore samples and the results were satisfactory.
2008, 25(6): 726-729
Abstract:
4-(ω-Arcyloybutoxy) benzoic acid was synthesized from ethyl p-hydroxy benzoate,4-chlorbutylacetat and acrylic acid as major raw materials.With dicyclihexylcarbodiimide (DCC) as reagent and 4-dimethylaminopyridine (DMAP) as catalyst,a series of the objective products were obtained with a yield more than 60%.The mass fractions of the products by LC were over 99%.The effect of synthesis technique and extraction procedure on the yield has been discussed.At last,a reasonable synthesis condition is found.FT-IR,1H NMR,MS,POM with hot stage and DSC were used to study the structure,phase behavior and mesophase texture of the compounds.The results showed that the texture of the liquid crystal compounds were the type of nematic liquid crystalline,and the liquid crystal compounds had good crystal performance in a wide temperature range.
4-(ω-Arcyloybutoxy) benzoic acid was synthesized from ethyl p-hydroxy benzoate,4-chlorbutylacetat and acrylic acid as major raw materials.With dicyclihexylcarbodiimide (DCC) as reagent and 4-dimethylaminopyridine (DMAP) as catalyst,a series of the objective products were obtained with a yield more than 60%.The mass fractions of the products by LC were over 99%.The effect of synthesis technique and extraction procedure on the yield has been discussed.At last,a reasonable synthesis condition is found.FT-IR,1H NMR,MS,POM with hot stage and DSC were used to study the structure,phase behavior and mesophase texture of the compounds.The results showed that the texture of the liquid crystal compounds were the type of nematic liquid crystalline,and the liquid crystal compounds had good crystal performance in a wide temperature range.
2008, 25(6): 730-733
Abstract:
A method for the determination of furazolidone residue in shrimp by high performance capillary electrophoresis with amperometric detection system was established.Several parameters affecting the determination were studied,including running buffer concentration,acidity,sampling time and separation voltage and organic additive.Under the following conditions:Na2B4O7-NaOH(Na2B4O7 30 mmol/L,pH=9.0 as buffer solution,CH3OH as organic additive,25 kV as running voltage,a linearity exists between peak height (Y) and mass concentration (c) in a range of 0.5~100 mg/L,the linear coefficient is 0.999 2,determination limit is 0.01 mg/L.
A method for the determination of furazolidone residue in shrimp by high performance capillary electrophoresis with amperometric detection system was established.Several parameters affecting the determination were studied,including running buffer concentration,acidity,sampling time and separation voltage and organic additive.Under the following conditions:Na2B4O7-NaOH(Na2B4O7 30 mmol/L,pH=9.0 as buffer solution,CH3OH as organic additive,25 kV as running voltage,a linearity exists between peak height (Y) and mass concentration (c) in a range of 0.5~100 mg/L,the linear coefficient is 0.999 2,determination limit is 0.01 mg/L.
2008, 25(6): 734-737
Abstract:
A new approach to preparation of chemically modified carboxymethyl chitosan (CM) derivatives was reported,where CM was prepared from chitosan with chloroactic acid as the carboxymethyl reagent first,and then N-quaternary ammonium group was introduced by the reaction of CM with 2,3-epoxypropyl trimethylammonium.The degree of substitution (DS) of carboxymethyl group was 0.73 and the DS of the quaternization group was 0.59.The mass-averaged molecular weight of CMQ was 1.1×104.The structures of the derivatives were characterized by FT-IR,XRD and 13C NMR.The effect of the CMQ on the human cervical carcinoma HeLa cells showed that CMQ can inhibit the proliferation and induce the apoptosis of HeLa cells.
A new approach to preparation of chemically modified carboxymethyl chitosan (CM) derivatives was reported,where CM was prepared from chitosan with chloroactic acid as the carboxymethyl reagent first,and then N-quaternary ammonium group was introduced by the reaction of CM with 2,3-epoxypropyl trimethylammonium.The degree of substitution (DS) of carboxymethyl group was 0.73 and the DS of the quaternization group was 0.59.The mass-averaged molecular weight of CMQ was 1.1×104.The structures of the derivatives were characterized by FT-IR,XRD and 13C NMR.The effect of the CMQ on the human cervical carcinoma HeLa cells showed that CMQ can inhibit the proliferation and induce the apoptosis of HeLa cells.
2008, 25(6): 738-740
Abstract:
Poly(chloromethylstyrene) nanoparticles with diameters of 65.0 nm were prepared from chloromethystyrene in a mixture emulsion of LAS and polyether.The chemical composition was identified by IR and the particle size and size distribution were measured by Zetaplus and TEM.Results showed that the polymer content in the mixture emulsion system can be improved greatly,and the diameter of the product can be controlled in nanometer scale.The system was very stable.TEM result showed synechia occured among resulting nano-spheres,which was attributed to the chloromethyl on the benzene ring.
Poly(chloromethylstyrene) nanoparticles with diameters of 65.0 nm were prepared from chloromethystyrene in a mixture emulsion of LAS and polyether.The chemical composition was identified by IR and the particle size and size distribution were measured by Zetaplus and TEM.Results showed that the polymer content in the mixture emulsion system can be improved greatly,and the diameter of the product can be controlled in nanometer scale.The system was very stable.TEM result showed synechia occured among resulting nano-spheres,which was attributed to the chloromethyl on the benzene ring.
2008, 25(6): 741-743
Abstract:
The epoxy resin/1,8-diaminonaphthalene curing system was studied by DSC and Fourier transform infrared spectrometry (FT-IR).The results show the gel temperature Ti(360.33 K),curing temperature Tp(391.79 K) and completeness curing temperature Tf(413.05 K) was determined by DSC.Via the Kissinger and Ozawa methods,the apparent energy of activation (ΔE) was 67.166 kJ/mol and 70.379 kJ/mol respectively,the reaction order (n=1) was calculated according to Crane theory.
The epoxy resin/1,8-diaminonaphthalene curing system was studied by DSC and Fourier transform infrared spectrometry (FT-IR).The results show the gel temperature Ti(360.33 K),curing temperature Tp(391.79 K) and completeness curing temperature Tf(413.05 K) was determined by DSC.Via the Kissinger and Ozawa methods,the apparent energy of activation (ΔE) was 67.166 kJ/mol and 70.379 kJ/mol respectively,the reaction order (n=1) was calculated according to Crane theory.
2008, 25(6): 744-746
Abstract:
A series of 2-amino-7-methyl-5-oxo-4-aryl-4H,5H-pyrano[4,3-b]pyran-3-carbonitriles were first synthesized by the reaction of each of the aromatic aldehydes with malononitrile and 4-hydroxyl-6-methyl-2-pyranone in acetic anhydride under ultrasonic irradiation.The yields were in the range of 72%~83%.The structures of the products were confirmed by IR,1H NMR and elemental analysis.The structure of 4e was determined by X-ray analysis.The crystal was monoclinic with space group C2/c,a=2.149 17(7) nm,b=0.824 98(2) nm,c=1.791 37(6) nm,α=90°,β=112.104(2)°,γ=90°,Mr=314.72,V=2.942 54(16) nm3,Z=8,Dc=1.421 kg/m3,F(000)=1 296,R=0.049 5,wR=0.087 8.
A series of 2-amino-7-methyl-5-oxo-4-aryl-4H,5H-pyrano[4,3-b]pyran-3-carbonitriles were first synthesized by the reaction of each of the aromatic aldehydes with malononitrile and 4-hydroxyl-6-methyl-2-pyranone in acetic anhydride under ultrasonic irradiation.The yields were in the range of 72%~83%.The structures of the products were confirmed by IR,1H NMR and elemental analysis.The structure of 4e was determined by X-ray analysis.The crystal was monoclinic with space group C2/c,a=2.149 17(7) nm,b=0.824 98(2) nm,c=1.791 37(6) nm,α=90°,β=112.104(2)°,γ=90°,Mr=314.72,V=2.942 54(16) nm3,Z=8,Dc=1.421 kg/m3,F(000)=1 296,R=0.049 5,wR=0.087 8.
2008, 25(6): 747-749
Abstract:
A series of N,N'-diary adipyl bis-azo compounds was synthesized from home-made N,N'-diaryl adipyl dihydrazide via oxidation system Fe(NO3)3·9H2O.The products were confirmed by elemental analysis,IR and 1H NMR.Two N-H absorption peaks of N,N'-diaryl adipyl dihydrazide in the infrared spectrum were approximately at 3 200~3 400 cm-1,while the two N-H absorption peaks were disappeared for oxidized products;two N-H chemical shifts of N,N'-diaryl adipyl dihydrazide in 1H NMR were about from 7.3 to 10.5,however,the same N-H chemical shifts were missing oxidized products;the results of elemental analyses for the products are in accord with their theoretical values.The yields were about from 80% to 94%.
A series of N,N'-diary adipyl bis-azo compounds was synthesized from home-made N,N'-diaryl adipyl dihydrazide via oxidation system Fe(NO3)3·9H2O.The products were confirmed by elemental analysis,IR and 1H NMR.Two N-H absorption peaks of N,N'-diaryl adipyl dihydrazide in the infrared spectrum were approximately at 3 200~3 400 cm-1,while the two N-H absorption peaks were disappeared for oxidized products;two N-H chemical shifts of N,N'-diaryl adipyl dihydrazide in 1H NMR were about from 7.3 to 10.5,however,the same N-H chemical shifts were missing oxidized products;the results of elemental analyses for the products are in accord with their theoretical values.The yields were about from 80% to 94%.
2008, 25(6): 750-752
Abstract:
Take gas diffusion electrode of zinc-air battery for example and add catalyst by layers,we studied the effect of changing catalyst layer location on the performance of gas diffusion electrode.Based on the current collection,the cathode can be divided into two sides as A side and B side.Based on the catalyst location difference,four kinds of cathode have been made,where the catalyst was added to both sides,neither side,only A side and only B side.The discharge results of the four kinds of the cathodes were compared and analyzed under the same condition.Experiment shows that the performance of the gas diffusion electrode in which the catalyst layer was added to the electrolyte side (B side) is better.The concentration polarization and Ohm polarization of the zinc-battery can be increased when the catalyst was added to the air side (A side).
Take gas diffusion electrode of zinc-air battery for example and add catalyst by layers,we studied the effect of changing catalyst layer location on the performance of gas diffusion electrode.Based on the current collection,the cathode can be divided into two sides as A side and B side.Based on the catalyst location difference,four kinds of cathode have been made,where the catalyst was added to both sides,neither side,only A side and only B side.The discharge results of the four kinds of the cathodes were compared and analyzed under the same condition.Experiment shows that the performance of the gas diffusion electrode in which the catalyst layer was added to the electrolyte side (B side) is better.The concentration polarization and Ohm polarization of the zinc-battery can be increased when the catalyst was added to the air side (A side).
