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2012 Volume 29 Issue 11
2012, 29(11): 1221-1230
doi: 10.3724/SP.J.1095.2012.20133
Abstract:
Borate electrode materials for lithium ion batteries offer several appealing features,such as relatively light molar mass,abundant resources,environmental friendliness and relatively high theoretical specific capacities.In this article,we briefly reviewed the state-of-the art of borate cathode materials and borate anode materials,including LiFeBO3,LiMnBO3,LiCoBO3,Fe3BO6,FeBO3,Cr3BO6,Co2B2O5,Cu3B2O6 and VBO3.The recent research progress on their structures,preparation methods and electrochemical performances are presented.In addition,we proposed some possible solutions for the existed problems within these materials.
Borate electrode materials for lithium ion batteries offer several appealing features,such as relatively light molar mass,abundant resources,environmental friendliness and relatively high theoretical specific capacities.In this article,we briefly reviewed the state-of-the art of borate cathode materials and borate anode materials,including LiFeBO3,LiMnBO3,LiCoBO3,Fe3BO6,FeBO3,Cr3BO6,Co2B2O5,Cu3B2O6 and VBO3.The recent research progress on their structures,preparation methods and electrochemical performances are presented.In addition,we proposed some possible solutions for the existed problems within these materials.
2012, 29(11): 1231-1239
doi: 10.3724/SP.J.1095.2012.00549
Abstract:
A monomer has been designed,synthesized and polymerized with[Rh(nbd)Cl]2-Et3N(nbd:2,5-norbonadien) catalyst.The liquid crystalline polyacetylene bearing chiral terphenyl mesogen {-[(CHC(CH2)3OCO-terphenyl(OR*)2]n-,R*=(S)-2-methylbutyl,(PAM3OCO(TPh)(OR*)2)} was obtained in high molecular mass(mass-average relative molecular mass is 30300).The monomer shows enantiotropic smectic C(SmC*) phase by introducing chiral groups and terphenyl mesogen,while its corresponding polymer exhibits enantiotropic smectic A(SmA*) liquid crystalline behavior.The "jacket effect" induced by the terphenyl mesogen linked at mass center position endows the polymer with high thermal stability(356℃),high photoluminescence and aggregation-induced emission enhancement(AIEE).Upon UV irradiation,the light-emitting of the solid state of the polymer fabricated at room temperature is stronger than that of the dilute solution,and its internal quantum efficiency and external quantum efficiency are 0.214 and 0.023,respectively.Photoluminescence of the polymer quenched from the liquid crystalline state of is obviously stronger and red-shifted than those of the solution and thin film states under excitation at the ultraviolet wavelength.
A monomer has been designed,synthesized and polymerized with[Rh(nbd)Cl]2-Et3N(nbd:2,5-norbonadien) catalyst.The liquid crystalline polyacetylene bearing chiral terphenyl mesogen {-[(CHC(CH2)3OCO-terphenyl(OR*)2]n-,R*=(S)-2-methylbutyl,(PAM3OCO(TPh)(OR*)2)} was obtained in high molecular mass(mass-average relative molecular mass is 30300).The monomer shows enantiotropic smectic C(SmC*) phase by introducing chiral groups and terphenyl mesogen,while its corresponding polymer exhibits enantiotropic smectic A(SmA*) liquid crystalline behavior.The "jacket effect" induced by the terphenyl mesogen linked at mass center position endows the polymer with high thermal stability(356℃),high photoluminescence and aggregation-induced emission enhancement(AIEE).Upon UV irradiation,the light-emitting of the solid state of the polymer fabricated at room temperature is stronger than that of the dilute solution,and its internal quantum efficiency and external quantum efficiency are 0.214 and 0.023,respectively.Photoluminescence of the polymer quenched from the liquid crystalline state of is obviously stronger and red-shifted than those of the solution and thin film states under excitation at the ultraviolet wavelength.
2012, 29(11): 1240-1245
doi: 10.3724/SP.J.1095.2012.00576
Abstract:
Two polyamides(P1,P2) containing both azobenzene and 1,3,4-thiadiazole were synthesized.Their structures and properties are characterized by FT-IR,1H NMR,GPC and TGA.The intrinsic viscosity of P1 and P2 are 0.14 dL/g and 0.12 dL/g,the Mw and polydispersity index(PDI) of P1 and P2 are 28.8,24.8 kg/mol and 1.71,1.74,respectively.Temperatures at mass loss of 5% for P1 and P2 are 320℃ and 322℃,respectively.The introduction of long side chain of alkoxy significantly improved the solubility of the two polymers in common organic solvents such as chloroform,tetrahydrofuran and so on.Their optical properties were investigated by UV-Vis absorption spectroscopy and fluorescence emission spectroscopy.The results indicated that the azobenzene in the polymers involved a trans-cis photoisomerization under the radiation of 365 nm UV light;the contents of cis-isomer-photostationary in P1 and P2 are 86.8% and 77.4% with corresponding efficiency of 82.7% and 73.7% for the anti-cis isomerization.Fluorescence emission peaks of P1 and P2 appeared at 418 nm and 428 nm under excitation at 366 nm and 363 nm.
Two polyamides(P1,P2) containing both azobenzene and 1,3,4-thiadiazole were synthesized.Their structures and properties are characterized by FT-IR,1H NMR,GPC and TGA.The intrinsic viscosity of P1 and P2 are 0.14 dL/g and 0.12 dL/g,the Mw and polydispersity index(PDI) of P1 and P2 are 28.8,24.8 kg/mol and 1.71,1.74,respectively.Temperatures at mass loss of 5% for P1 and P2 are 320℃ and 322℃,respectively.The introduction of long side chain of alkoxy significantly improved the solubility of the two polymers in common organic solvents such as chloroform,tetrahydrofuran and so on.Their optical properties were investigated by UV-Vis absorption spectroscopy and fluorescence emission spectroscopy.The results indicated that the azobenzene in the polymers involved a trans-cis photoisomerization under the radiation of 365 nm UV light;the contents of cis-isomer-photostationary in P1 and P2 are 86.8% and 77.4% with corresponding efficiency of 82.7% and 73.7% for the anti-cis isomerization.Fluorescence emission peaks of P1 and P2 appeared at 418 nm and 428 nm under excitation at 366 nm and 363 nm.
2012, 29(11): 1246-1250
doi: 10.3724/SP.J.1095.2012.00537
Abstract:
To further study an efficient modified route for transforming an antibacterial fluoroquinolone to an antitumor compound,an oxadiazole heterocyclic ring,1,3,4-oxadiazole-thione,was used as an isostere of C-3 carboxylic group for pefloxacin 1,and a key intermediate,1-ethyl-6-fluoro-7-(4-methyl-piperazin-1-yl)-3-(3H-1,3,4-oxadiazole-2-thione-5-yl)-quinolin-4(1H)-one 4(5),was designed and synthesized.The intermediate was then subjected to an aminomethylation reaction with secondary amines or substituted anilines and formaldehyde to afford the corresponding oxadiazole thione Mannch bases 6a~6j as the title compounds,respectively.The structures for ten title compounds were characterized by elemental analysis,1H NMR and MS,and their anticancer activities in vitro against Hep-3B cancer cell lines were also evaluated.The results reveal that all the title compounds show more significant potent than that of parent compound 1,and those derived from aliphatic amines display higher activity than the aromatic amine compounds.
To further study an efficient modified route for transforming an antibacterial fluoroquinolone to an antitumor compound,an oxadiazole heterocyclic ring,1,3,4-oxadiazole-thione,was used as an isostere of C-3 carboxylic group for pefloxacin 1,and a key intermediate,1-ethyl-6-fluoro-7-(4-methyl-piperazin-1-yl)-3-(3H-1,3,4-oxadiazole-2-thione-5-yl)-quinolin-4(1H)-one 4(5),was designed and synthesized.The intermediate was then subjected to an aminomethylation reaction with secondary amines or substituted anilines and formaldehyde to afford the corresponding oxadiazole thione Mannch bases 6a~6j as the title compounds,respectively.The structures for ten title compounds were characterized by elemental analysis,1H NMR and MS,and their anticancer activities in vitro against Hep-3B cancer cell lines were also evaluated.The results reveal that all the title compounds show more significant potent than that of parent compound 1,and those derived from aliphatic amines display higher activity than the aromatic amine compounds.
2012, 29(11): 1251-1255
doi: 10.3724/SP.J.1095.2012.00547
Abstract:
Using 1,3-diphenylacetone as precursor,bibenzyldithiolmethane(1) was prepared through reacting 1,3-diphenylacetone with dry hydrogen sulfide and hydrogen chloride.Under microwave irradiation,compound 1 was subjected to esterification and hydrazinolysis to yield 1,1-bibenzyl-1,1-bimercaptoacetyl-hydrazine(3).The condensation reactions between compound 3 and aromatic aldehyde led to the production of a series of 1,1-bibenzyl-1,1-bimercaptoacetylhydrazone(4a~4n).Their structures were confirmed by IR,1H NMR,MS and elemental analysis.
Using 1,3-diphenylacetone as precursor,bibenzyldithiolmethane(1) was prepared through reacting 1,3-diphenylacetone with dry hydrogen sulfide and hydrogen chloride.Under microwave irradiation,compound 1 was subjected to esterification and hydrazinolysis to yield 1,1-bibenzyl-1,1-bimercaptoacetyl-hydrazine(3).The condensation reactions between compound 3 and aromatic aldehyde led to the production of a series of 1,1-bibenzyl-1,1-bimercaptoacetylhydrazone(4a~4n).Their structures were confirmed by IR,1H NMR,MS and elemental analysis.
2012, 29(11): 1256-1261
doi: 10.3724/SP.J.1095.2012.00554
Abstract:
β-Cyclodextrin(β-CD) copolymers and its metal complexes were synthesized via the polymerization between(6-O-butene diacid ester)-β-cyclodextrin and styrene.Their structures and properties were characterized by infrared spectrum(IR),ultraviolet spectrum(UV),elemental analysis(EA),differential scanning calorimeter(DSC) and thermogravimetry(TG).β-CD copolymers metal complexes used as urease inhibitors were investigated and showed prominent inhibition efficacy.The inhibition ratio of copolymer-Cu2+ complex was 96.67% with a loading of 4 g/L.
β-Cyclodextrin(β-CD) copolymers and its metal complexes were synthesized via the polymerization between(6-O-butene diacid ester)-β-cyclodextrin and styrene.Their structures and properties were characterized by infrared spectrum(IR),ultraviolet spectrum(UV),elemental analysis(EA),differential scanning calorimeter(DSC) and thermogravimetry(TG).β-CD copolymers metal complexes used as urease inhibitors were investigated and showed prominent inhibition efficacy.The inhibition ratio of copolymer-Cu2+ complex was 96.67% with a loading of 4 g/L.
2012, 29(11): 1262-1265
doi: 10.3724/SP.J.1095.2012.00578
Abstract:
4,6-Bis[(4'-diethylamino) styryl] pyrimidin-2-ol was synthesized and characterized.The UV-Vis and fluorescent properties were studied in phosphate buffer solutions at different pH value.The UV-Vis spectral results indicated that the peak located at ~500 nm reaches maximal intensity at pH=6.78.The fluorescent spectra data suggested that the intensity of emission peak decreased with increasing pH value.The fluorescence was quenched when the pH was 5.51.
4,6-Bis[(4'-diethylamino) styryl] pyrimidin-2-ol was synthesized and characterized.The UV-Vis and fluorescent properties were studied in phosphate buffer solutions at different pH value.The UV-Vis spectral results indicated that the peak located at ~500 nm reaches maximal intensity at pH=6.78.The fluorescent spectra data suggested that the intensity of emission peak decreased with increasing pH value.The fluorescence was quenched when the pH was 5.51.
2012, 29(11): 1266-1271
doi: 10.3724/SP.J.1095.2012.00558
Abstract:
[Cd2(HL)2(ox)]·1.5H2O was synthesized hydrothermally from Cd(NO3)2·4H2O,pyrazolyl derivative(H2L=2,6-di-(5-phenyl-1H-pyrazol-3-yl)pyridine) and oxalate(H2ox=oxalic acid).Structural analysis revealed that the complex crystallized in the triclinic system with P-1 space group.The Cd took a distorted octahedral geometry and was coordinated by two oxygen atoms from one ox ligand and four N atoms from two HL- ligands.Adjacent Cd atoms(Cd1/Cd2) were connected through bridging ox ligand and N atoms from HL- to generate two separate 1D chains structure.The complex was further characterized by elemental analysis,IR,UV-Vis spectroscopy and powder X-ray diffraction(PXRD).In addition,the complex displayed ideal thermal stability and photoluminescent properties,and exhibited some catalytic activity toward the oxidation of cyclohexane.
[Cd2(HL)2(ox)]·1.5H2O was synthesized hydrothermally from Cd(NO3)2·4H2O,pyrazolyl derivative(H2L=2,6-di-(5-phenyl-1H-pyrazol-3-yl)pyridine) and oxalate(H2ox=oxalic acid).Structural analysis revealed that the complex crystallized in the triclinic system with P-1 space group.The Cd took a distorted octahedral geometry and was coordinated by two oxygen atoms from one ox ligand and four N atoms from two HL- ligands.Adjacent Cd atoms(Cd1/Cd2) were connected through bridging ox ligand and N atoms from HL- to generate two separate 1D chains structure.The complex was further characterized by elemental analysis,IR,UV-Vis spectroscopy and powder X-ray diffraction(PXRD).In addition,the complex displayed ideal thermal stability and photoluminescent properties,and exhibited some catalytic activity toward the oxidation of cyclohexane.
2012, 29(11): 1272-1277
doi: 10.3724/SP.J.1095.2012.00559
Abstract:
The poorly-water soluble drug naproxen(NAP) was loaded on modified and unmodified mesoporous molecular sieves MCM-41.The drug-loaded samples were characterized by X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FT-IR),differential scanning caborimetry(DSC),scanning electron microscopy(SEM) analysis,transmission electron microscopy(TEM) analysis,nitrogen adsorption/desorption isotherms,respectively.The results showed that the hexagonal mesoporous structure was still remained after loading with drug molecules,which were entrapped inside the mesopores.The dissolution rate of NAP released from mesoporous molecular sieves MCM-41 was faster compared with the dissolution rate of pure NAP.In simulated intestinal fluid,the MCM-41-NAP and MCM-41-NH2-NAP exhibited 70% mass fraction burst release within 60 min.Remarkably,the dissolution rate of NAP released from all mesoporous materials is faster compared with the dissolution rate of pure NAP.At the same time,the release rate of NAP from the functionalized mesoporous materials was effectively controlled compared with that of the unmodified materials.
The poorly-water soluble drug naproxen(NAP) was loaded on modified and unmodified mesoporous molecular sieves MCM-41.The drug-loaded samples were characterized by X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FT-IR),differential scanning caborimetry(DSC),scanning electron microscopy(SEM) analysis,transmission electron microscopy(TEM) analysis,nitrogen adsorption/desorption isotherms,respectively.The results showed that the hexagonal mesoporous structure was still remained after loading with drug molecules,which were entrapped inside the mesopores.The dissolution rate of NAP released from mesoporous molecular sieves MCM-41 was faster compared with the dissolution rate of pure NAP.In simulated intestinal fluid,the MCM-41-NAP and MCM-41-NH2-NAP exhibited 70% mass fraction burst release within 60 min.Remarkably,the dissolution rate of NAP released from all mesoporous materials is faster compared with the dissolution rate of pure NAP.At the same time,the release rate of NAP from the functionalized mesoporous materials was effectively controlled compared with that of the unmodified materials.
2012, 29(11): 1278-1285
doi: 10.3724/SP.J.1095.2012.00555
Abstract:
Anatase titanium dioxide nanoparticles were employed for the adsorption of fluoride ions from aqueous solution.The process was studied in details by varying the pH value,adsorption time and temperature.The results showed that equilibrium was reached within 2.0 min at room temperature.The adsorption efficiency was over 97% at pH 2.0~10.0.Adsorbed fluoride ions were desorbed with 0.1 mol/L NaOH within 3.0 min,while the desorption efficiency could be up to 96%.The kinetic experimental data properly correlate with the second-order kinetic model.The apparent activation energy was calculated to be 6.85 kJ/mol.The overall rate process is mainly controlled by the intraparticle diffusion,while the boundary layer resistance cannot be ignored.The adsorption data could be well interpreted by the Langmuir and Dubinin-Radushkevich adsorption isotherms.The mean energy of adsorption was 4.26 kJ/mol at room temperature.The results show that ΔH0>0 and ΔG0<0 for the adsorption reaction,indicating that the adsorption process is a spontaneous and endothermic reaction.The co-existed ions such as HCO3- and PO43-,had greater effects on adsorption of fluoride ions.Removal efficiency of nano-TiO2 for fluoride ions obtained by dynamic adsorption is close to that obtained by the static adsorption.
Anatase titanium dioxide nanoparticles were employed for the adsorption of fluoride ions from aqueous solution.The process was studied in details by varying the pH value,adsorption time and temperature.The results showed that equilibrium was reached within 2.0 min at room temperature.The adsorption efficiency was over 97% at pH 2.0~10.0.Adsorbed fluoride ions were desorbed with 0.1 mol/L NaOH within 3.0 min,while the desorption efficiency could be up to 96%.The kinetic experimental data properly correlate with the second-order kinetic model.The apparent activation energy was calculated to be 6.85 kJ/mol.The overall rate process is mainly controlled by the intraparticle diffusion,while the boundary layer resistance cannot be ignored.The adsorption data could be well interpreted by the Langmuir and Dubinin-Radushkevich adsorption isotherms.The mean energy of adsorption was 4.26 kJ/mol at room temperature.The results show that ΔH0>0 and ΔG0<0 for the adsorption reaction,indicating that the adsorption process is a spontaneous and endothermic reaction.The co-existed ions such as HCO3- and PO43-,had greater effects on adsorption of fluoride ions.Removal efficiency of nano-TiO2 for fluoride ions obtained by dynamic adsorption is close to that obtained by the static adsorption.
2012, 29(11): 1286-1290
doi: 10.3724/SP.J.1095.2012.00551
Abstract:
The electrocatalytic activity of Ti/PbO2 anode for degradation of p-nitrophenol was studied with linear sweeping voltammetry and galvanostatic electrolysis.The electrocatalytic degradation pathway of p-nitrophenol was explored by HPLC analysis of the reaction mixture in the anodic oxidation and cathodic reduction processes.The results indicate that Ti/PbO2 electrode can electrocatalyze the degradation of p-nitrophenol effectively.The conversion of the 1.0 mmol/L p-nitrophenol achieved 98.6% when the electrolysis was carried out for 240 min with a constant current of 40&×10-3 A/cm2 at 35℃.The pathway of the electrocatalytic oxidation degradation of p-nitrophenol is p-nitrophenol→hydroquinone and pyocatechol→benzoquinone→maleic acid→oxalic acid→CO2 and H2O.The main product of the first step is hydroquinone.The conversions of benzoquinone to maleic acid and maleic acid to oxalic acid are the rate determining steps of anodic oxidation process.The p-nitrophenol can be reduced at the cathode.The reduction products include p-aminophenol.In an electrolytic cell without diaphragm,the cathodic reduction product,p-aminophenol,can be oxidated easily at the anode.The synergsic effect of the cathode and anode speeds up the degradation of p-nitrophenol in an undivided electrolytic cell compared to an electrolytic cell with diaphragm.
The electrocatalytic activity of Ti/PbO2 anode for degradation of p-nitrophenol was studied with linear sweeping voltammetry and galvanostatic electrolysis.The electrocatalytic degradation pathway of p-nitrophenol was explored by HPLC analysis of the reaction mixture in the anodic oxidation and cathodic reduction processes.The results indicate that Ti/PbO2 electrode can electrocatalyze the degradation of p-nitrophenol effectively.The conversion of the 1.0 mmol/L p-nitrophenol achieved 98.6% when the electrolysis was carried out for 240 min with a constant current of 40&×10-3 A/cm2 at 35℃.The pathway of the electrocatalytic oxidation degradation of p-nitrophenol is p-nitrophenol→hydroquinone and pyocatechol→benzoquinone→maleic acid→oxalic acid→CO2 and H2O.The main product of the first step is hydroquinone.The conversions of benzoquinone to maleic acid and maleic acid to oxalic acid are the rate determining steps of anodic oxidation process.The p-nitrophenol can be reduced at the cathode.The reduction products include p-aminophenol.In an electrolytic cell without diaphragm,the cathodic reduction product,p-aminophenol,can be oxidated easily at the anode.The synergsic effect of the cathode and anode speeds up the degradation of p-nitrophenol in an undivided electrolytic cell compared to an electrolytic cell with diaphragm.
2012, 29(11): 1291-1296
doi: 10.3724/SP.J.1095.2012.00580
Abstract:
The superhydrophobic film on copper surface was fabricated by immersing copper substrate in palmitic acid dissovled in ethanol.The optimal conditions for fabricating the superhydrophobic film on copper are:0.03 mol/L palmitic acid in ethanol solution,temperature of 20~22℃ and 144 h of immersion.The resultant superhydrophobic film was characterized and analyzed by means of scanning electron microscopy(SEM),contact angle goniometer,Fourier-transform infrared spectrometer(FTIR) and high precision electronic balance,respectively.The results showed that it was the grass-like Cu(CH3(CH2)14COO)2 microcluster with dimensional size in the range of 100~200 μm that was responsible for its hydrophobic property.The water contact angle of superhydrophobic surface is 150°.The superhydrophobic surface on copper showed superior anti-fouling performance.
The superhydrophobic film on copper surface was fabricated by immersing copper substrate in palmitic acid dissovled in ethanol.The optimal conditions for fabricating the superhydrophobic film on copper are:0.03 mol/L palmitic acid in ethanol solution,temperature of 20~22℃ and 144 h of immersion.The resultant superhydrophobic film was characterized and analyzed by means of scanning electron microscopy(SEM),contact angle goniometer,Fourier-transform infrared spectrometer(FTIR) and high precision electronic balance,respectively.The results showed that it was the grass-like Cu(CH3(CH2)14COO)2 microcluster with dimensional size in the range of 100~200 μm that was responsible for its hydrophobic property.The water contact angle of superhydrophobic surface is 150°.The superhydrophobic surface on copper showed superior anti-fouling performance.
2012, 29(11): 1297-1301
doi: 10.3724/SP.J.1095.2012.20001
Abstract:
CeO2-ZrO2 solid solution is an indispensable oxygen storage material for the three way catalyst to control the pollution gas emission from automobiles.In this paper,three series of Ce-Zr-Al nanocomposite(ACZ) was prepared by citrate acid sol-gel method,sol assistant co-precipitation and sol co-precipitation,respectively.The obtained samples were calcinated at 1000℃ for 4 h to test the thermal stability and oxygen storage capacity(OSC).The effect of synthetic methods on these properties was investigated by means of X-ray diffraction(XRD),Brunauer Emmett Teller(BET) specific surface area(SSA) and H2 temperature-programmed reduction(H2-TPR).The results revealed that the thermal stability and oxygen storage capacity of all the ACZ were improved compared to the pure CeO2-ZrO2 solid solution.The molar proportion of Al doped in ACZ is 5,10,5 for citrate acid sol-gel method,sol assistant co-precipitation and sol co-precipitation,respectively.ACZ prepared by citrate acid sol-gel method had the highest oxygen storage capacity(717.5 μmol/g-CeO2),account for 49.3% of the theoretical maximum.
CeO2-ZrO2 solid solution is an indispensable oxygen storage material for the three way catalyst to control the pollution gas emission from automobiles.In this paper,three series of Ce-Zr-Al nanocomposite(ACZ) was prepared by citrate acid sol-gel method,sol assistant co-precipitation and sol co-precipitation,respectively.The obtained samples were calcinated at 1000℃ for 4 h to test the thermal stability and oxygen storage capacity(OSC).The effect of synthetic methods on these properties was investigated by means of X-ray diffraction(XRD),Brunauer Emmett Teller(BET) specific surface area(SSA) and H2 temperature-programmed reduction(H2-TPR).The results revealed that the thermal stability and oxygen storage capacity of all the ACZ were improved compared to the pure CeO2-ZrO2 solid solution.The molar proportion of Al doped in ACZ is 5,10,5 for citrate acid sol-gel method,sol assistant co-precipitation and sol co-precipitation,respectively.ACZ prepared by citrate acid sol-gel method had the highest oxygen storage capacity(717.5 μmol/g-CeO2),account for 49.3% of the theoretical maximum.
2012, 29(11): 1302-1308
doi: 10.3724/SP.J.1095.2012.00460
Abstract:
Three kinds of novel sulfobetaine amphoteric surfactants with different hydrophobic groups were synthesiszed.Their structures were characterized by FT-IR spectroscopy.The surface tensions of the product in dilute aqueous solutions were measured at 25℃ by drop-volume method and then the critical micelle concentration(cmc) and surface tension at the critical micelle concentration(γcmc) were determined.The effects of the concentration and temperature on their foam properties were investigated by Ross-Miles method.Meanwhile the emulsifying properties of three kinds of sulfobetaines were investigated by a water diversion method.The experimental results showed that an increase of the aromatic ring size in the alkyl chain increased the critical micelle concentration and surface tension at the critical micelle concentration.However,with the increase of the aromatic ring size,the adsorption of arylalkyl surfactants began to weaken.As the mass concentration of three kinds of surfactants raised,the foaming power increased firstly,and then remained at a certain value.The foam stability was enhanced gradually with increasing the concentration.As the temperature increased,the foaming power was heightened significantly,while foam stability decreased.As the concentration increased,the emulsifying power of three kinds of surfactants increased firstly and then stayed to a certain value.
Three kinds of novel sulfobetaine amphoteric surfactants with different hydrophobic groups were synthesiszed.Their structures were characterized by FT-IR spectroscopy.The surface tensions of the product in dilute aqueous solutions were measured at 25℃ by drop-volume method and then the critical micelle concentration(cmc) and surface tension at the critical micelle concentration(γcmc) were determined.The effects of the concentration and temperature on their foam properties were investigated by Ross-Miles method.Meanwhile the emulsifying properties of three kinds of sulfobetaines were investigated by a water diversion method.The experimental results showed that an increase of the aromatic ring size in the alkyl chain increased the critical micelle concentration and surface tension at the critical micelle concentration.However,with the increase of the aromatic ring size,the adsorption of arylalkyl surfactants began to weaken.As the mass concentration of three kinds of surfactants raised,the foaming power increased firstly,and then remained at a certain value.The foam stability was enhanced gradually with increasing the concentration.As the temperature increased,the foaming power was heightened significantly,while foam stability decreased.As the concentration increased,the emulsifying power of three kinds of surfactants increased firstly and then stayed to a certain value.
2012, 29(11): 1309-1315
doi: 10.3724/SP.J.1095.2012.00488
Abstract:
The thermodynamic properties of microemulsion formed by six kinds of alkyl aryl sulfonates(AAS,synthesized in the laboratory) in the multi-component systems were investigated by dilution method.The influences of molecular structure,temperature,short chain alcohol,water content and salt concentration were respectively discussed.The results show that the increase of long alkyl carbon atom number(in alkyl aryl sulfonate molecule) causes the ΔGo→i0 of the AAS/n-butanol/n-decane/water microemulsion systems decrease,along with the increase of the ΔSo→i0,and facilitates the formation of the microemulsion.The ΔSo→i0 and carbon atom number of alkyl chain are in linear relationship,with ΔSo→i0=1.7975n+71.538.The ΔHo→i0 is a constant.As the aromatic rings shift from the edge to the middle of the long carbonic chains,the ΔGo→i0 of the microemulsion systems decreases,along with the decrease of ΔSo→i0 and ΔHo→i0,facilitating the formation of the microemulsion.With the increase of temperature,ΔGo→i0 of the microemulsion systems increase,hindering the formation of the microemulsion.The increase of carbon atom number of the alcohol causes ΔGo→i0 decrease,which enables the formation of the microemulsion.ΔGo→i0 and carbon atom number of the alcohol are in linear relationship,with ΔGo→i0=-2790.8n+7286.4(328 K).The increase of water content causes ΔGo→i0 increase and the formation ability of the microemulsion decreases.ΔGo→i0 and the volume of water are in linear relationship,with ΔGo→i0=6697.8V-7170.4(318 K).The increase of salt concentration causes ΔGo→i0 decrease,and the formation ability of the microemulsion increases.
The thermodynamic properties of microemulsion formed by six kinds of alkyl aryl sulfonates(AAS,synthesized in the laboratory) in the multi-component systems were investigated by dilution method.The influences of molecular structure,temperature,short chain alcohol,water content and salt concentration were respectively discussed.The results show that the increase of long alkyl carbon atom number(in alkyl aryl sulfonate molecule) causes the ΔGo→i0 of the AAS/n-butanol/n-decane/water microemulsion systems decrease,along with the increase of the ΔSo→i0,and facilitates the formation of the microemulsion.The ΔSo→i0 and carbon atom number of alkyl chain are in linear relationship,with ΔSo→i0=1.7975n+71.538.The ΔHo→i0 is a constant.As the aromatic rings shift from the edge to the middle of the long carbonic chains,the ΔGo→i0 of the microemulsion systems decreases,along with the decrease of ΔSo→i0 and ΔHo→i0,facilitating the formation of the microemulsion.With the increase of temperature,ΔGo→i0 of the microemulsion systems increase,hindering the formation of the microemulsion.The increase of carbon atom number of the alcohol causes ΔGo→i0 decrease,which enables the formation of the microemulsion.ΔGo→i0 and carbon atom number of the alcohol are in linear relationship,with ΔGo→i0=-2790.8n+7286.4(328 K).The increase of water content causes ΔGo→i0 increase and the formation ability of the microemulsion decreases.ΔGo→i0 and the volume of water are in linear relationship,with ΔGo→i0=6697.8V-7170.4(318 K).The increase of salt concentration causes ΔGo→i0 decrease,and the formation ability of the microemulsion increases.
2012, 29(11): 1316-1323
doi: 10.3724/SP.J.1095.2012.00545
Abstract:
Thirty-three,fifty-four,thirty-seven and twenty-nine volatile oil components from Fructus Amomi Rotundus,Fructus Galangae,Semen Alpiniae Katsumadai and Semen Myristicae,respectively,were identified and their relative contents were determined by gas chromatography-mass spectrometry(GC-MS).Total ion current chromatograms of them were divided into 4 fingerprint sections on the basis of peak retention time,and their volatile oil components were compared with each other.The results showed that the volatile oil components from Fructus Amomi Rotundus were distinctly different from those of Fructus Galangae,Semen Alpiniae Katsumadai or Semen Myristicae.Moreover,the major active ingredient of Fructus Amomi Rotundus was 1,8-cineole and its relative content was more than that of Fructus Galangae or Semen Alpiniae Katsumadai but it was not detected in the Semen Myristicae.Therefore,Fructus Amomi Rotundus couldn't be substituted with Fructus Galangae,Semen Alpiniae Katsumadai or Semen Myristicae.This study provides a new approach for the comparison and the quality assessment of Fructus Amomi Rotundus,Fructus Galangae,Semen Alpiniae Katsumadai and Semen Myristicae.
Thirty-three,fifty-four,thirty-seven and twenty-nine volatile oil components from Fructus Amomi Rotundus,Fructus Galangae,Semen Alpiniae Katsumadai and Semen Myristicae,respectively,were identified and their relative contents were determined by gas chromatography-mass spectrometry(GC-MS).Total ion current chromatograms of them were divided into 4 fingerprint sections on the basis of peak retention time,and their volatile oil components were compared with each other.The results showed that the volatile oil components from Fructus Amomi Rotundus were distinctly different from those of Fructus Galangae,Semen Alpiniae Katsumadai or Semen Myristicae.Moreover,the major active ingredient of Fructus Amomi Rotundus was 1,8-cineole and its relative content was more than that of Fructus Galangae or Semen Alpiniae Katsumadai but it was not detected in the Semen Myristicae.Therefore,Fructus Amomi Rotundus couldn't be substituted with Fructus Galangae,Semen Alpiniae Katsumadai or Semen Myristicae.This study provides a new approach for the comparison and the quality assessment of Fructus Amomi Rotundus,Fructus Galangae,Semen Alpiniae Katsumadai and Semen Myristicae.
2012, 29(11): 1324-1328
doi: 10.3724/SP.J.1095.2012.00569
Abstract:
The molecular docking techniques were used for predicting the interactions of two chromatographic stationary phase proteins with four pairs of chiral compounds,respectively.The results showed that the order of predicted binding free energies(ΔG) were consistent with the experimental order of chromatographic elution peaks(R-(+) and S-(-) type).Furthermore,the order of the absolute value of binding free energies difference(Δ(ΔG)) of the enantiomers(R-(+) and S-(-) type) were consistent with the experimental separation factor(α).These suggest that the capability protein to identify different chiral compounds and the elution order of compounds(R-(+) and S-(-) type) could be reflected by molecular docking.
The molecular docking techniques were used for predicting the interactions of two chromatographic stationary phase proteins with four pairs of chiral compounds,respectively.The results showed that the order of predicted binding free energies(ΔG) were consistent with the experimental order of chromatographic elution peaks(R-(+) and S-(-) type).Furthermore,the order of the absolute value of binding free energies difference(Δ(ΔG)) of the enantiomers(R-(+) and S-(-) type) were consistent with the experimental separation factor(α).These suggest that the capability protein to identify different chiral compounds and the elution order of compounds(R-(+) and S-(-) type) could be reflected by molecular docking.
2012, 29(11): 1329-1334
doi: 10.3724/SP.J.1095.2012.00577
Abstract:
In pH=1.89 Briton-Robinson(BR) buffer,HAuCl4 can be reduced by amoxicillin to form gold nanoparticles,resulting in characteristic plasmon resonance absorption signals at 537 nm and 720 nm.The intensity at 537 nm is proportional to the amoxicillin concentration in a certain range,and amoxicillin can be detected based on the plasmon resonance absorption intensities of the gold nanoparticles.Under the optimized conditions(pH=1.89,reaction temperature is 65℃,reaction time is 40 min),amoxicillin can be detected in the range of 2.0×10-6~3.6×10-5 mol/L with the detection limit of 1.3×10-7 mol/L.This method has been used in the synthesized samples determination of amoxicillin with the recovery of 90.4%~103.2% and a relative standard deviation of less than 4.6%,then it is applied to the determination of amoxicillin in two commercial capsules with satisfied results compared with HPLC method.
In pH=1.89 Briton-Robinson(BR) buffer,HAuCl4 can be reduced by amoxicillin to form gold nanoparticles,resulting in characteristic plasmon resonance absorption signals at 537 nm and 720 nm.The intensity at 537 nm is proportional to the amoxicillin concentration in a certain range,and amoxicillin can be detected based on the plasmon resonance absorption intensities of the gold nanoparticles.Under the optimized conditions(pH=1.89,reaction temperature is 65℃,reaction time is 40 min),amoxicillin can be detected in the range of 2.0×10-6~3.6×10-5 mol/L with the detection limit of 1.3×10-7 mol/L.This method has been used in the synthesized samples determination of amoxicillin with the recovery of 90.4%~103.2% and a relative standard deviation of less than 4.6%,then it is applied to the determination of amoxicillin in two commercial capsules with satisfied results compared with HPLC method.
2012, 29(11): 1335-1339
doi: 10.3724/SP.J.1095.2012.00540
Abstract:
Prominent fingermarks were obtained within 1~3 seconds after developed by the water-soluble mercaptosuccinic acid(MSA) modified CdTe quantum dots(QDs) with a wide-continuous excitation spectra and a narrow-symmetric emission spectra on various substrates.Latent fingermarks on water-immersed substrate and sticky adhesive tape were developed successfully.High sensitivity was also obtained on the development of latent fingermarks pressed continuously with the same finger.Compared with methyl violet,rhodamine 6G and mercaptoacetic acid(TGA) modified CdTe QDs,the MSA modified CdTe QDs showed the fastest developing speed and the best fingermarks quality.
Prominent fingermarks were obtained within 1~3 seconds after developed by the water-soluble mercaptosuccinic acid(MSA) modified CdTe quantum dots(QDs) with a wide-continuous excitation spectra and a narrow-symmetric emission spectra on various substrates.Latent fingermarks on water-immersed substrate and sticky adhesive tape were developed successfully.High sensitivity was also obtained on the development of latent fingermarks pressed continuously with the same finger.Compared with methyl violet,rhodamine 6G and mercaptoacetic acid(TGA) modified CdTe QDs,the MSA modified CdTe QDs showed the fastest developing speed and the best fingermarks quality.
2012, 29(11): 1340-1342
doi: 10.3724/SP.J.1095.2012.00552
Abstract:
A simple and efficient method has been developed for the oxybromination of six kinds of polycyclic aromatic hydrocarbons with the use of aqueous hydrobromic acid and hydrogen peroxide.The method requires no catalysts,and achieves bromination via the in situ generated active bromine.By controling the reaction temperature and the amount of bromination agent,the reaction can obtain the monobromination or dibromination of polycyclic aromatic hydrocarbons with a yield of 51.1%~94.2%.The oxybromination method is simple,safe,environmental friendly,and suitable for industrial production.The obtained products have been characterized by melting point measurement and 1H NMR.
A simple and efficient method has been developed for the oxybromination of six kinds of polycyclic aromatic hydrocarbons with the use of aqueous hydrobromic acid and hydrogen peroxide.The method requires no catalysts,and achieves bromination via the in situ generated active bromine.By controling the reaction temperature and the amount of bromination agent,the reaction can obtain the monobromination or dibromination of polycyclic aromatic hydrocarbons with a yield of 51.1%~94.2%.The oxybromination method is simple,safe,environmental friendly,and suitable for industrial production.The obtained products have been characterized by melting point measurement and 1H NMR.
