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2012 Volume 29 Issue 7
2012, 29(7): 733-739
doi: 10.3724/SP.J.1095.2012.00500
Abstract:
Both particle size and morphology of cerium-doped yttrium aluminium garnet(YAG: Ce) yellow phosphors could exert significant influence on their phtoluminescence as well as further applications.It has been demonstrated that the desired morphology is spherical with a controlled size.In this paper,progresses of morphologic and size control of YAG: Ce phosphors by the synthesis methods,technology parameters and post-treatment techniques were summarized,the advantages and disadvantages of morphologic control measures were discussed,and the main features of regulation and control for powder morphology were concluded.
Both particle size and morphology of cerium-doped yttrium aluminium garnet(YAG: Ce) yellow phosphors could exert significant influence on their phtoluminescence as well as further applications.It has been demonstrated that the desired morphology is spherical with a controlled size.In this paper,progresses of morphologic and size control of YAG: Ce phosphors by the synthesis methods,technology parameters and post-treatment techniques were summarized,the advantages and disadvantages of morphologic control measures were discussed,and the main features of regulation and control for powder morphology were concluded.
Synthesis of a Novel UV Absorbent and Its Application in Polylactic Acid Superfine Fibrous Membranes
2012, 29(7): 740-744
doi: 10.3724/SP.J.1095.2012.00347
Abstract:
A novel UV absorbent,(3-hydroxy-4-benzoyl)phenyl 2,3;4,6-di-O-cyclohexylidene-D-β-mannopyranoside(UV-O-DHM),was synthesized using 2,4-dihydroxy-benzophenone(UV-O) and D-mannose as raw materials.The compound exhibited high decomposition temperature(Td) at 372.6℃ and possessed good thermal stability.The biodegradable anti-UV polylactic acid(PLA) superfine fibrous membranes were prepared via electro-spinning through mixing UV-O-DHM into dichloromethane solution of PLA,and the features of the fiber were clearly characterized by scanning electron microscope.The fiber has uniform diameter of 3~4 μm and is evenly covered by the nano-porous.The UV-O-DHM/PLA superfine fiber has good ultraviolet absorption performance.With increasing concentration of UV-O-DHM,UV transmittance(T%) decreased,and when the mass fraction of UV-O-DHM was 1.1%,T% was almost 0 in 230~350 nm,and the UV protection level was better than that of UV-O/PLA superfine fiber in 365~380 nm.
A novel UV absorbent,(3-hydroxy-4-benzoyl)phenyl 2,3;4,6-di-O-cyclohexylidene-D-β-mannopyranoside(UV-O-DHM),was synthesized using 2,4-dihydroxy-benzophenone(UV-O) and D-mannose as raw materials.The compound exhibited high decomposition temperature(Td) at 372.6℃ and possessed good thermal stability.The biodegradable anti-UV polylactic acid(PLA) superfine fibrous membranes were prepared via electro-spinning through mixing UV-O-DHM into dichloromethane solution of PLA,and the features of the fiber were clearly characterized by scanning electron microscope.The fiber has uniform diameter of 3~4 μm and is evenly covered by the nano-porous.The UV-O-DHM/PLA superfine fiber has good ultraviolet absorption performance.With increasing concentration of UV-O-DHM,UV transmittance(T%) decreased,and when the mass fraction of UV-O-DHM was 1.1%,T% was almost 0 in 230~350 nm,and the UV protection level was better than that of UV-O/PLA superfine fiber in 365~380 nm.
2012, 29(7): 745-750
doi: 10.3724/SP.J.1095.2012.00284
Abstract:
The micro structures of epoxy toughened by polyester hot melt adhesive PE30 was studied by SEM.The influence of addition polyester hot melt adhesive PE30 on heat stability of epoxy was studied by DSC,DMC,and TGA.The mechanical properties,including impact strength,bending strength,fracture strength were measured.The results showed that a suitable usage of PE30 is 15%.In the process of curing,the epoxy resin matrix containing polyester hot melt adhesive came out and induced a phase separation,from the single-phase to continuous phase and then to reverse phase.Comparing with the pure epoxy resin,the impact strength and fracture strength were increased by 250% and 127%,respectively.The bending strength and modulus were reduced by 27% and 44%,respectively.The glass transition temperature and starting thermo-gravimetric temperature were reduced by 1.5%,and mechanical loss peak temperature was reduced by 2.5%.It is show that the polyester hot melt adhesive PE30 can significantly toughen the epoxy resin while maintain its thermal performance.
The micro structures of epoxy toughened by polyester hot melt adhesive PE30 was studied by SEM.The influence of addition polyester hot melt adhesive PE30 on heat stability of epoxy was studied by DSC,DMC,and TGA.The mechanical properties,including impact strength,bending strength,fracture strength were measured.The results showed that a suitable usage of PE30 is 15%.In the process of curing,the epoxy resin matrix containing polyester hot melt adhesive came out and induced a phase separation,from the single-phase to continuous phase and then to reverse phase.Comparing with the pure epoxy resin,the impact strength and fracture strength were increased by 250% and 127%,respectively.The bending strength and modulus were reduced by 27% and 44%,respectively.The glass transition temperature and starting thermo-gravimetric temperature were reduced by 1.5%,and mechanical loss peak temperature was reduced by 2.5%.It is show that the polyester hot melt adhesive PE30 can significantly toughen the epoxy resin while maintain its thermal performance.
2012, 29(7): 751-756
doi: 10.3724/SP.J.1095.2012.00348
Abstract:
Poly(ethylene 2,5-furandicarboxylate)(PEF) was directly and successfully synthesized via the direct esterification method(PTA method) starting from 2,5-furandicarboxylic acid(FDCA) and ethylene glycol(EG),in which stannous oxalate was chosen as catalyst.Effect of the molar ratio of FDCA to EG(1: 1.2~1: 2.0),dosage of stannous octanoate(0.3×10-3~5×10-3 mol/mol FDCA),esterification temperature(180~220℃),polycondensation temperature(220~250℃) and dosage of trimethyl phosphate(1×10-4~3×10-3 mol/mol FDCA) on the esterification and polycondensation processes were studied in details.The optimized process conditions were found to be:n(FDCA): n((EG)=1: 1.6,stannous oxalate dosage is 1×10-3 mol/mol FDCA,polycondensation temperature is 240℃,polycondensation time is 480 min and trimethyl phosphate dosage is 3×10-4 mol/mol FDCA.The results of Fourier transform infrared spectroscopy(FTIR) and nuclear magnetic resonance spectroscopy(1H NMR) confirmed the expected PEF structure.
Poly(ethylene 2,5-furandicarboxylate)(PEF) was directly and successfully synthesized via the direct esterification method(PTA method) starting from 2,5-furandicarboxylic acid(FDCA) and ethylene glycol(EG),in which stannous oxalate was chosen as catalyst.Effect of the molar ratio of FDCA to EG(1: 1.2~1: 2.0),dosage of stannous octanoate(0.3×10-3~5×10-3 mol/mol FDCA),esterification temperature(180~220℃),polycondensation temperature(220~250℃) and dosage of trimethyl phosphate(1×10-4~3×10-3 mol/mol FDCA) on the esterification and polycondensation processes were studied in details.The optimized process conditions were found to be:n(FDCA): n((EG)=1: 1.6,stannous oxalate dosage is 1×10-3 mol/mol FDCA,polycondensation temperature is 240℃,polycondensation time is 480 min and trimethyl phosphate dosage is 3×10-4 mol/mol FDCA.The results of Fourier transform infrared spectroscopy(FTIR) and nuclear magnetic resonance spectroscopy(1H NMR) confirmed the expected PEF structure.
2012, 29(7): 757-761
doi: 10.3724/SP.J.1095.2012.00333
Abstract:
A new ligand N-[2-cyclohexylmethoxy-4(1-(2,2'-bipyridinemethyl)amino)acetylamino] phenylmethanesulfonamide(NSC-PA),for potential labeling [99mTc(CO)3(H2O)3]+ was synthesized by hydroxyl-alkylation,amino-methylsulfonylation,nitro-reduction,amino-bromideacetylation and N-alkylation from 2-amino-5-nitrophenol.Simple experimental operation,short period and purified products could be obtained under optimized conditions.The structures of all the compounds were confirmed by 1H NMR,IR and MS.The purity of the target compound was over 98% as given by HPLC result.The target product could be used for future labeling studies.This synthesis is promising in the exploration of new imaging reagent for breast cancer.
A new ligand N-[2-cyclohexylmethoxy-4(1-(2,2'-bipyridinemethyl)amino)acetylamino] phenylmethanesulfonamide(NSC-PA),for potential labeling [99mTc(CO)3(H2O)3]+ was synthesized by hydroxyl-alkylation,amino-methylsulfonylation,nitro-reduction,amino-bromideacetylation and N-alkylation from 2-amino-5-nitrophenol.Simple experimental operation,short period and purified products could be obtained under optimized conditions.The structures of all the compounds were confirmed by 1H NMR,IR and MS.The purity of the target compound was over 98% as given by HPLC result.The target product could be used for future labeling studies.This synthesis is promising in the exploration of new imaging reagent for breast cancer.
2012, 29(7): 762-768
doi: 10.3724/SP.J.1095.2012.00339
Abstract:
Thirteen novel bisamides compounds containing methoxy and benzothiazole were synthesized.Their structures were characterized by 1H NMR,13C NMR,IR and elemental analyses.Preliminary bioassay showed that some of them exhibited certain anti-CMV activities,and some compounds posed antitumor activity toward PC3 cells in vitro by MTT method.The antiproliferation activity of compound 4f to PC3 cells was 74.2% at the concentration of 10 μmol/L.
Thirteen novel bisamides compounds containing methoxy and benzothiazole were synthesized.Their structures were characterized by 1H NMR,13C NMR,IR and elemental analyses.Preliminary bioassay showed that some of them exhibited certain anti-CMV activities,and some compounds posed antitumor activity toward PC3 cells in vitro by MTT method.The antiproliferation activity of compound 4f to PC3 cells was 74.2% at the concentration of 10 μmol/L.
2012, 29(7): 769-774
doi: 10.3724/SP.J.1095.2012.00360
Abstract:
To discover an efficient modification for shifting from an antibacterial fluoroquinolone to an antitumor one based on the topological similarities between targeting topoisomerases as the eukaryotic ones and mammals,using oxadiazole heterocycle as an intermediate for the isostere of C-3 carboxylic group of norfloxacin(1),1-ethyl-6-fluoro-7-piperazin-1-yl-3-(5-mercapto-1,3,4-oxadiazol-2-yl)-quinolin-4(1H)-one(3) was subjected to thioetherfication with each of chloromethyl oxadiazole(4a~4e) to give bis-oxadiazole methylsulfides(5a~5e),respectively.The following N-methylations and quaternizations yielded the corresponding N-methyl bis-oxadiazole methylsulfides(6a~6e) and N,N-dimethyl bis-oxadiazole methylsulfide iodides(7a~7e).The structures of fifteen 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 with a MTT assay.The results reveal that fifteen title compounds show higher cytotoxicity than that of comparison 1,in which quaternary ammonium salts exhibit potential anticancer activity with IC50 values below 25.0 μmol/L.
To discover an efficient modification for shifting from an antibacterial fluoroquinolone to an antitumor one based on the topological similarities between targeting topoisomerases as the eukaryotic ones and mammals,using oxadiazole heterocycle as an intermediate for the isostere of C-3 carboxylic group of norfloxacin(1),1-ethyl-6-fluoro-7-piperazin-1-yl-3-(5-mercapto-1,3,4-oxadiazol-2-yl)-quinolin-4(1H)-one(3) was subjected to thioetherfication with each of chloromethyl oxadiazole(4a~4e) to give bis-oxadiazole methylsulfides(5a~5e),respectively.The following N-methylations and quaternizations yielded the corresponding N-methyl bis-oxadiazole methylsulfides(6a~6e) and N,N-dimethyl bis-oxadiazole methylsulfide iodides(7a~7e).The structures of fifteen 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 with a MTT assay.The results reveal that fifteen title compounds show higher cytotoxicity than that of comparison 1,in which quaternary ammonium salts exhibit potential anticancer activity with IC50 values below 25.0 μmol/L.
2012, 29(7): 775-779
doi: 10.3724/SP.J.1095.2012.00349
Abstract:
The Eu(Ⅲ) complex and new Schiff base ligand of taurine and 2-acetylbenzimidazole were synthesized in methyl alcohol.The structure of the complex was determined as Eu2L3(NO3)3(L=C11H12N3O3S) by chemical and elemental analysis,1H NMR,IR,mass spectrometry,laser Raman and three-dimension fluorescene spectrometry.The main fluorescence emission of the complex was Eu3+ perturbation ligand to light-emitting,along with the Eu3+ center narrow-band luminescence.When the λex=330.0 nm,the Eu3+ ion narrow-band fluorescence is emitted;when λex=410.0 nm,the Eu3+ produces the 525.0 nm emission band.
The Eu(Ⅲ) complex and new Schiff base ligand of taurine and 2-acetylbenzimidazole were synthesized in methyl alcohol.The structure of the complex was determined as Eu2L3(NO3)3(L=C11H12N3O3S) by chemical and elemental analysis,1H NMR,IR,mass spectrometry,laser Raman and three-dimension fluorescene spectrometry.The main fluorescence emission of the complex was Eu3+ perturbation ligand to light-emitting,along with the Eu3+ center narrow-band luminescence.When the λex=330.0 nm,the Eu3+ ion narrow-band fluorescence is emitted;when λex=410.0 nm,the Eu3+ produces the 525.0 nm emission band.
2012, 29(7): 780-783
doi: 10.3724/SP.J.1095.2012.00336
Abstract:
Condensation of β-ionone and 5,6-epoxyl-β-ionone with aromatic aldehydes by sodium carbonate and sodium hydroxide was carried out to afford eight novel ionone-containing chalcones at room temperature for 1~15 min by grinding,and their structures were characterized by 1H NMR,MS,IR and elemental analysis.The effects of substituents,the types and amounts of catalysts on the reaction were studied.The results show that the yield is 87.1%~94.8% when the molar ratio of β-ionone,benzalaldehyde,sodium carbonate and sodium hydroxide is 20: 20: 5: 15,and electron withdrawing group promotes the condensation.
Condensation of β-ionone and 5,6-epoxyl-β-ionone with aromatic aldehydes by sodium carbonate and sodium hydroxide was carried out to afford eight novel ionone-containing chalcones at room temperature for 1~15 min by grinding,and their structures were characterized by 1H NMR,MS,IR and elemental analysis.The effects of substituents,the types and amounts of catalysts on the reaction were studied.The results show that the yield is 87.1%~94.8% when the molar ratio of β-ionone,benzalaldehyde,sodium carbonate and sodium hydroxide is 20: 20: 5: 15,and electron withdrawing group promotes the condensation.
2012, 29(7): 784-787
doi: 10.3724/SP.J.1095.2012.00364
Abstract:
The extraction behavior of Ce(Ⅳ) from HNO3 medium by ionic liquid [C10mim][NTf2] was investigated.The effects of various parameters including time,feed concentration,HNO3 concentration,alkyl chain length,salt concentration and temperature on the extraction efficiency of Ce(Ⅳ) was measured.Enthalpy value of the extraction was calculated,which indicated the extraction of Ce(Ⅳ) is a spontaneously exothermic process.A plausible anion exchange mechanism was proposed for this process.The backward extraction efficiency of the Ce(Ⅳ) was 85.1% using 1.0 mol/L H2SO4 as strippant.
The extraction behavior of Ce(Ⅳ) from HNO3 medium by ionic liquid [C10mim][NTf2] was investigated.The effects of various parameters including time,feed concentration,HNO3 concentration,alkyl chain length,salt concentration and temperature on the extraction efficiency of Ce(Ⅳ) was measured.Enthalpy value of the extraction was calculated,which indicated the extraction of Ce(Ⅳ) is a spontaneously exothermic process.A plausible anion exchange mechanism was proposed for this process.The backward extraction efficiency of the Ce(Ⅳ) was 85.1% using 1.0 mol/L H2SO4 as strippant.
2012, 29(7): 788-793
doi: 10.3724/SP.J.1095.2012.00343
Abstract:
Mg-Al hydrotalcite-like compound(HTlc) was prepared by a coprecipitation method.The adsorption behaviors of o-,m-and p-cresol on the Mg-Al HTlc were investigated.The results indicated that the adsorption isotherms of o-,m-and p-cresol on HTlc could be well fitted with the Freundlich equation and the adsorption kinetics could be well described by a pseudo-second-order kinetic.The adsorption rate and adsorption amount of p-cresol on the HTlc is slightly higher than that of o-cresol,which is higher than that of m-cresol at the same equilibrium cresol concentration.The adsorption amounts of o-,m-and p-cresol increased firstly and then decreased with the increasing pH in the rang of 5.00~13.00,increased with the increase of temperature and electrolyte(NaCl) concentration.The adsorption mechanism of cresol on HTlc and the effect of substituent CH3 position on the adsorption were discussed.
Mg-Al hydrotalcite-like compound(HTlc) was prepared by a coprecipitation method.The adsorption behaviors of o-,m-and p-cresol on the Mg-Al HTlc were investigated.The results indicated that the adsorption isotherms of o-,m-and p-cresol on HTlc could be well fitted with the Freundlich equation and the adsorption kinetics could be well described by a pseudo-second-order kinetic.The adsorption rate and adsorption amount of p-cresol on the HTlc is slightly higher than that of o-cresol,which is higher than that of m-cresol at the same equilibrium cresol concentration.The adsorption amounts of o-,m-and p-cresol increased firstly and then decreased with the increasing pH in the rang of 5.00~13.00,increased with the increase of temperature and electrolyte(NaCl) concentration.The adsorption mechanism of cresol on HTlc and the effect of substituent CH3 position on the adsorption were discussed.
2012, 29(7): 794-800
doi: 10.3724/SP.J.1095.2012.00353
Abstract:
Fe3O4 nanoparticles,which were prepared by chemical coprecipitation,were modified by 2,2,6,6-tetramethylpiperidinyl-1-oxy bromic salt to form peroxide initiators.The poly[styrene-co-(maleic anhydride)]/Fe3O4 hybrid materials were prepared by "living"/controllable free radical polymerization of styrene(St) and maleic anhydride(MA) in the presence of modified Fe3O4.Nano-Fe3O4 and the hybrid materials were characterized by FT-IR,XRD,TGA,TEM,GPC.The results indicate that its average diameter is about 70 nm.The polymer chains increase with the polymerization time.The results of magnetic performance by vibrating sample magnetometer indicate that the hybrid materials exhibit superparamagnetic properties at room temperature under applied magnetic field.Saturation magnetization decreases with the increasing amount of encapsulated polymers.
Fe3O4 nanoparticles,which were prepared by chemical coprecipitation,were modified by 2,2,6,6-tetramethylpiperidinyl-1-oxy bromic salt to form peroxide initiators.The poly[styrene-co-(maleic anhydride)]/Fe3O4 hybrid materials were prepared by "living"/controllable free radical polymerization of styrene(St) and maleic anhydride(MA) in the presence of modified Fe3O4.Nano-Fe3O4 and the hybrid materials were characterized by FT-IR,XRD,TGA,TEM,GPC.The results indicate that its average diameter is about 70 nm.The polymer chains increase with the polymerization time.The results of magnetic performance by vibrating sample magnetometer indicate that the hybrid materials exhibit superparamagnetic properties at room temperature under applied magnetic field.Saturation magnetization decreases with the increasing amount of encapsulated polymers.
Synthesis of Covalent Bonded PW11/TiO2 Mesoporous Hybrid Materials and Their Photocatalytic Activity
2012, 29(7): 801-807
doi: 10.3724/SP.J.1095.2012.00345
Abstract:
Covalent bonded PW11/TiO2 mesoporous hybrid materials were prepared by grafting a lacunary tungstophosphate PW11 with Keggin structure onto the surface of mesoporous TiO2 that was synthesized using evaporation-induced self-assembly(EISA) method.The structure,PW11 loading and the mechanism for grafting were characterized and studied by means of IR,N2 adsorption-desorption,XRD,TEM and ICP-AES techniques.The photocatalytic activities of the hybrid samples for methyl orange degradation were also investigated.It was shown that as-prepared TiO2 via EISA method before calcinations had an incompact framework.It can partially hydrolyze and react with PW11 to form PW11Ti species,which could condense with TiO2 framework to lead to covalent linkage of PW11 on TiO2.Compared with pure TiO2 support,the crystallinity of anatase was lowered slightly,the pore size and the pore volume decreased in the hybrid samples.However,the activities for methyl orange degradation increased significantly,which can be attributed to the synergistic effect between polyoxometalate and TiO2.
Covalent bonded PW11/TiO2 mesoporous hybrid materials were prepared by grafting a lacunary tungstophosphate PW11 with Keggin structure onto the surface of mesoporous TiO2 that was synthesized using evaporation-induced self-assembly(EISA) method.The structure,PW11 loading and the mechanism for grafting were characterized and studied by means of IR,N2 adsorption-desorption,XRD,TEM and ICP-AES techniques.The photocatalytic activities of the hybrid samples for methyl orange degradation were also investigated.It was shown that as-prepared TiO2 via EISA method before calcinations had an incompact framework.It can partially hydrolyze and react with PW11 to form PW11Ti species,which could condense with TiO2 framework to lead to covalent linkage of PW11 on TiO2.Compared with pure TiO2 support,the crystallinity of anatase was lowered slightly,the pore size and the pore volume decreased in the hybrid samples.However,the activities for methyl orange degradation increased significantly,which can be attributed to the synergistic effect between polyoxometalate and TiO2.
Synthesis, Characterization and Catalytical Properties of Ti-AlKIT-1 Mesostructured Molecular Sieves
2012, 29(7): 808-813
doi: 10.3724/SP.J.1095.2012.00363
Abstract:
The mixed mesoporous sieves Ti-AlKIT-1 materials were prepared through Ti grafting on AlKIT-1 obtained either directly or by post-synthesis using relatively inexpensive aluminium and titanium precursors,and characterized by FT-IR,XRD,MAS NMR,DRS,EDS and physical adsorption-desorption of nitrogen and used as catalysts toward the oxidation of cyclohexanol in 30% H2O2.XRD and N2 adsorption-desorption showed that the original mesoporous structure of the Ti-AlKIT-1 was retained with a lower BET surface area,pore volume and smaller pore size.Based on the combined FT-IR and DRS studies,it was concluded that the infrared spectroscopy can result a powerful tool to verify the Ti(Ⅳ) incorporation into the framework of AlKIT-1.27Al MAS NMR spectra indicated that the ammoniun-washed samples present only tetracoordinated aluminium.All Ti-AlKIT-1 catalysts showed significant activity in the oxidation of cyclohexanol due to the cooperative action of Ti and Al.Ti-Al(ds)KIT-1 with higher Ti/Al molar ratio and BET surface area and pore volume showed better catalytic activity than Ti-Al(ps)KIT-1.The as-prepared catalyst is stable and reusable.The conversion of cyclohexanol was 51.3% after three runs,only decreased by 4.31% after 48 h catalytic reaction at 80℃.
The mixed mesoporous sieves Ti-AlKIT-1 materials were prepared through Ti grafting on AlKIT-1 obtained either directly or by post-synthesis using relatively inexpensive aluminium and titanium precursors,and characterized by FT-IR,XRD,MAS NMR,DRS,EDS and physical adsorption-desorption of nitrogen and used as catalysts toward the oxidation of cyclohexanol in 30% H2O2.XRD and N2 adsorption-desorption showed that the original mesoporous structure of the Ti-AlKIT-1 was retained with a lower BET surface area,pore volume and smaller pore size.Based on the combined FT-IR and DRS studies,it was concluded that the infrared spectroscopy can result a powerful tool to verify the Ti(Ⅳ) incorporation into the framework of AlKIT-1.27Al MAS NMR spectra indicated that the ammoniun-washed samples present only tetracoordinated aluminium.All Ti-AlKIT-1 catalysts showed significant activity in the oxidation of cyclohexanol due to the cooperative action of Ti and Al.Ti-Al(ds)KIT-1 with higher Ti/Al molar ratio and BET surface area and pore volume showed better catalytic activity than Ti-Al(ps)KIT-1.The as-prepared catalyst is stable and reusable.The conversion of cyclohexanol was 51.3% after three runs,only decreased by 4.31% after 48 h catalytic reaction at 80℃.
2012, 29(7): 814-818
doi: 10.3724/SP.J.1095.2012.00355
Abstract:
Polymerization of aniline on nanoTiO2 complex film electrode was achieved by sol-gel method and electrochemical polymerization technique.XRD,SEM and CV were used to characterize the structure and image of the nanoTiO2-PAn complex film.Loose short fiber and porous structure could be observed by SEM.The average particle size of crystal grains was 150 nm.The COD removal efficiency reached 41.2% for an artificial wastewater containing 50 mg/L 2,4,6-tri-nitrophenol under the conditions of 2 cm distance between the electrodes,pH=7~8 and 25℃.
Polymerization of aniline on nanoTiO2 complex film electrode was achieved by sol-gel method and electrochemical polymerization technique.XRD,SEM and CV were used to characterize the structure and image of the nanoTiO2-PAn complex film.Loose short fiber and porous structure could be observed by SEM.The average particle size of crystal grains was 150 nm.The COD removal efficiency reached 41.2% for an artificial wastewater containing 50 mg/L 2,4,6-tri-nitrophenol under the conditions of 2 cm distance between the electrodes,pH=7~8 and 25℃.
2012, 29(7): 819-823
doi: 10.3724/SP.J.1095.2012.00493
Abstract:
Multiple-species BODseed was used for fabricating biochemical oxygen demand(BOD) biosensors for rapid online BOD determination.Some factors to accuracy were studied such as calibration solution selection,sample self-biodegradation,and thermostatic device.Good results were obtained when wastewater was used as calibration solution instead of glucose and glutimic acid(GGA).The self-biodegradation process made the rapid measurements inaccurate.Besides,thermostatic device used only for biosensors is defective,and it should be applied for maintaining a constant temperature of the samples and buffer,promoting the efficiency and accuracy of online monitoring.
Multiple-species BODseed was used for fabricating biochemical oxygen demand(BOD) biosensors for rapid online BOD determination.Some factors to accuracy were studied such as calibration solution selection,sample self-biodegradation,and thermostatic device.Good results were obtained when wastewater was used as calibration solution instead of glucose and glutimic acid(GGA).The self-biodegradation process made the rapid measurements inaccurate.Besides,thermostatic device used only for biosensors is defective,and it should be applied for maintaining a constant temperature of the samples and buffer,promoting the efficiency and accuracy of online monitoring.
2012, 29(7): 824-829
doi: 10.3724/SP.J.1095.2012.00350
Abstract:
A glassy carbon electrode was modified with graphene by casting.The modified electrode showed an excellent electrocatalytical effect on the oxidation of acetaminophen(ACOP).The voltammetric behavior and electrochemical analysis method of ACOP were studied on the modified electrode.The effect of pH value on the response of ACOP was studied in phosphate buffer solution(PBS).The results showed that the redox peak potential of ACOP shifted negatively with increasing pH value,and a pair of well-defined redox waves were obtained in PBS of pH=6.0.The oxidation peak currents of ACOP increased linearly with the concentration,in the range of 6.00×10-7~4.00×10-5 mol/L,the linear regression equation was ipa(A)=3.00c+1.21×10-5,with correlation coefficient 0.9940.The detection limit(S/N=3) was 5.00×10-8 mol/L.The graphene modified electrode showed a good sensitivity,selectivity and stability.It was applied to the ACOP tablets analysis.
A glassy carbon electrode was modified with graphene by casting.The modified electrode showed an excellent electrocatalytical effect on the oxidation of acetaminophen(ACOP).The voltammetric behavior and electrochemical analysis method of ACOP were studied on the modified electrode.The effect of pH value on the response of ACOP was studied in phosphate buffer solution(PBS).The results showed that the redox peak potential of ACOP shifted negatively with increasing pH value,and a pair of well-defined redox waves were obtained in PBS of pH=6.0.The oxidation peak currents of ACOP increased linearly with the concentration,in the range of 6.00×10-7~4.00×10-5 mol/L,the linear regression equation was ipa(A)=3.00c+1.21×10-5,with correlation coefficient 0.9940.The detection limit(S/N=3) was 5.00×10-8 mol/L.The graphene modified electrode showed a good sensitivity,selectivity and stability.It was applied to the ACOP tablets analysis.
2012, 29(7): 830-835
doi: 10.3724/SP.J.1095.2012.00448
Abstract:
Hydrophobic Cu-polytetrafluoroethlyene(Cu-PTFE) and Zn-PTFE composite electrodes were prepared by composite electroplating with copper and zinc as substrates,respectively.The electrochemical reduction behavior of benzoic acid on hydrophobic composite electrodes was studied.The electrochemical parameters such as Tafel polarization curve,cyclic voltammogram(CV),electrode stability and electrochemical impedance spectroscopy(EIS) were investigated.The results show that the Cu-PTFE composite electrode possesses a higher catalytic activity in the preparation of benzaldehyde from benzoic acid than that of Zn-PTFE composite electrode,the yields of the electrochemical reduction on Cu-PTFE and Zn-PTFE composite electrodes are 88.4% and 79.2%,respectively.The Cu-PTFE composite electrode is promising as an electrode for preparation of benzaldehyde via electrochemical approach.The result shows that the electrochemical reduction of benzoic acid on the composite electrodes may be exclusively controlled by electron transfer process.
Hydrophobic Cu-polytetrafluoroethlyene(Cu-PTFE) and Zn-PTFE composite electrodes were prepared by composite electroplating with copper and zinc as substrates,respectively.The electrochemical reduction behavior of benzoic acid on hydrophobic composite electrodes was studied.The electrochemical parameters such as Tafel polarization curve,cyclic voltammogram(CV),electrode stability and electrochemical impedance spectroscopy(EIS) were investigated.The results show that the Cu-PTFE composite electrode possesses a higher catalytic activity in the preparation of benzaldehyde from benzoic acid than that of Zn-PTFE composite electrode,the yields of the electrochemical reduction on Cu-PTFE and Zn-PTFE composite electrodes are 88.4% and 79.2%,respectively.The Cu-PTFE composite electrode is promising as an electrode for preparation of benzaldehyde via electrochemical approach.The result shows that the electrochemical reduction of benzoic acid on the composite electrodes may be exclusively controlled by electron transfer process.
2012, 29(7): 836-843
doi: 10.3724/SP.J.1095.2012.00331
Abstract:
Two sebacic acid imidazoline quaternary ammonium salts,sebacic acid-salicylic acid imidazoline quaternary ammonium salts(SSAI) and sebacic acid imidazoline quaternary ammonium salts(SAI),were synthesized and their inhibition action and adsorption behavior on N80 steel in 1 mol/L hydrochloric solution were investigated by means of mass loss and electrochemical techniques.It was showed that the two compounds had good corrosion inhibition for N80 steel in 1 mol/L HCl solution.SSAI was found to have a superior inhibition efficiency to SAI.Both SSAI and SAI were mixed-type inhibitors and mainly inhibited anode process against N80 steel in 1 mol/L HCl solution.The experimental results revealed that the adsorption processes were exothermic reaction and belong to chemical adsorption.
Two sebacic acid imidazoline quaternary ammonium salts,sebacic acid-salicylic acid imidazoline quaternary ammonium salts(SSAI) and sebacic acid imidazoline quaternary ammonium salts(SAI),were synthesized and their inhibition action and adsorption behavior on N80 steel in 1 mol/L hydrochloric solution were investigated by means of mass loss and electrochemical techniques.It was showed that the two compounds had good corrosion inhibition for N80 steel in 1 mol/L HCl solution.SSAI was found to have a superior inhibition efficiency to SAI.Both SSAI and SAI were mixed-type inhibitors and mainly inhibited anode process against N80 steel in 1 mol/L HCl solution.The experimental results revealed that the adsorption processes were exothermic reaction and belong to chemical adsorption.
2012, 29(7): 844-851
doi: 10.3724/SP.J.1095.2012.00352
Abstract:
The structural parameters of complex systems of seven kinds of aryl sulfonate(synthesized in the laboratory) alkyl aryl sulfonate(AAS)/n-butanol/n-decane/water microemulsions were obtained by means of a dilution method.We also calculated the standard free energy ΔGo→i0 of transfer from the continuous oil phase to the interfacial region,the standard enthalpy ΔHo→i0 and the standard entropy ΔSo→i0 values.The effects of the average molecular mass and its distribution of AAS on the structural parameters and thermodynamic functions were investigated.The results show that the effective radius of dispersive phase Re,the radius of inner sphere water Rw,their difference di,the average aggerate number of surfactant molecules per drop n,have the tendency of normal distributionNd、and the total interface area of dispersion phase outer sphere Ad appear to be contrary to the above consequence.The values of -ΔGo→i0 exhibit the tendency of normal distribution(5.36 kJ/mol) So→i0 have the tendency of normal distribution(26.88 J/(mol·K)) Rw,Re,n,di,-ΔGo→i0,ΔHo→i0,ΔSo→i0 increase while the values of Nd,Ad decrease.In addition,the values of structural parameters,-ΔGo→i0 and ΔSo→i0 change linearly with the average molecular mass of the AAS,the latter two are y=0.0586x=-17.916 and y=0.2203x=-61.275,respectively.
The structural parameters of complex systems of seven kinds of aryl sulfonate(synthesized in the laboratory) alkyl aryl sulfonate(AAS)/n-butanol/n-decane/water microemulsions were obtained by means of a dilution method.We also calculated the standard free energy ΔGo→i0 of transfer from the continuous oil phase to the interfacial region,the standard enthalpy ΔHo→i0 and the standard entropy ΔSo→i0 values.The effects of the average molecular mass and its distribution of AAS on the structural parameters and thermodynamic functions were investigated.The results show that the effective radius of dispersive phase Re,the radius of inner sphere water Rw,their difference di,the average aggerate number of surfactant molecules per drop n,have the tendency of normal distribution
2012, 29(7): 852-854
doi: 10.3724/SP.J.1095.2012.00358
Abstract:
In order to improve the yield of synthesizing silafluorene,a plastic multiple-tank reaction bottle was designed and fabricated.It was well-known that the reaction of 4,4'-dibromo-2,2'-diiodobiphenyl(1) with butyllithium formed a key active intermediate 4,4'-dibromo-2,2'-dilithiumbiphenyl(2),which should be kept under low temperature.In our previous work,we added a large excess of SiCl4(20 fold in molar ratio) into the solution of compound 2 to suppress the formation of spirosilafluorene(4).In this contribution,the use of a plastic multiple-tank reaction bottle made it possible to add the solution of compound 2 into SiCl4 because it provides compound 2 with a container in the bottom of the bottle.By leaning the reaction bottle,compound 2 can be transferred into the storage tank or transfer into the reaction tank under low temperature.This new apparatus can improve the yield of the silafluorene from 20% to 35%~40% with a much less SiCl4 feed ratio(4 fold in molar ratio).This plastic multiple-tank reaction bottle might be widely used in the organometallic chemistry.
In order to improve the yield of synthesizing silafluorene,a plastic multiple-tank reaction bottle was designed and fabricated.It was well-known that the reaction of 4,4'-dibromo-2,2'-diiodobiphenyl(1) with butyllithium formed a key active intermediate 4,4'-dibromo-2,2'-dilithiumbiphenyl(2),which should be kept under low temperature.In our previous work,we added a large excess of SiCl4(20 fold in molar ratio) into the solution of compound 2 to suppress the formation of spirosilafluorene(4).In this contribution,the use of a plastic multiple-tank reaction bottle made it possible to add the solution of compound 2 into SiCl4 because it provides compound 2 with a container in the bottom of the bottle.By leaning the reaction bottle,compound 2 can be transferred into the storage tank or transfer into the reaction tank under low temperature.This new apparatus can improve the yield of the silafluorene from 20% to 35%~40% with a much less SiCl4 feed ratio(4 fold in molar ratio).This plastic multiple-tank reaction bottle might be widely used in the organometallic chemistry.
