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2003 Volume 20 Issue 6
2003, 20(6): 511-515
Abstract:
Separation of the neighboring rare earth elements from their binary oxide mixtures Ho2O3-Er2O3,Er2O3-Tm2O3,Tm2O3-Yb2O3 and Yb2O3-Lu2O3 has been carried out via the chemical vapor transport reaction based on the difference in thermodynamic characteristics of their vapor complexes LnAl3Cl3n+3.The results show ed that most rare earth chlorides of Ho,Er,Tm,Yb and Lu are deposited in the reactor zone of temperature ranged from 800 to 1050 K.The chlorides of rare earch with small atomic number are preferably deposited in the reactor zone of higher temperature and rice versa.The largest separation factors expressed as molar ratio for the resulting chlorides are SFEr/Ho=1.41,SFEr/Tm=1.60,SFTm/Yb=1.91,SF Lu/Yb=1.37.
Separation of the neighboring rare earth elements from their binary oxide mixtures Ho2O3-Er2O3,Er2O3-Tm2O3,Tm2O3-Yb2O3 and Yb2O3-Lu2O3 has been carried out via the chemical vapor transport reaction based on the difference in thermodynamic characteristics of their vapor complexes LnAl3Cl3n+3.The results show ed that most rare earth chlorides of Ho,Er,Tm,Yb and Lu are deposited in the reactor zone of temperature ranged from 800 to 1050 K.The chlorides of rare earch with small atomic number are preferably deposited in the reactor zone of higher temperature and rice versa.The largest separation factors expressed as molar ratio for the resulting chlorides are SFEr/Ho=1.41,SFEr/Tm=1.60,SFTm/Yb=1.91,SF Lu/Yb=1.37.
2003, 20(6): 516-519
Abstract:
A polymeric monomer,4-(6-(meth) acryloyloxyhexyloxy)-4'-(2S,3S)-(2-chloro-3-methyl pentanoyloxy)-biphenyl was synthesized from acrylic acid,4,4'-biphenyldiol,and (-)(2S,3S)-2-amino-3-methyl pentanoic acid.Novel poly (meth) acrylate containing two chiral centers was prepared through free-radical polymerization of the monomer by using azobisisobutyronitrile (AIBN) as an initiator and DMF as solvent.The structures of the intermediate,monomers and corresponding polymers were characterized by elemental analysis,FTIR and 1H NMR.Molecular weight and MW distribution were calculated by gel permeation chromatography.For polyacrylate they are Mn=12 000,Mw=15690,d=1.31,and that for polymethacrylate Mn=21255,Mw=38554 and d=1.81.
A polymeric monomer,4-(6-(meth) acryloyloxyhexyloxy)-4'-(2S,3S)-(2-chloro-3-methyl pentanoyloxy)-biphenyl was synthesized from acrylic acid,4,4'-biphenyldiol,and (-)(2S,3S)-2-amino-3-methyl pentanoic acid.Novel poly (meth) acrylate containing two chiral centers was prepared through free-radical polymerization of the monomer by using azobisisobutyronitrile (AIBN) as an initiator and DMF as solvent.The structures of the intermediate,monomers and corresponding polymers were characterized by elemental analysis,FTIR and 1H NMR.Molecular weight and MW distribution were calculated by gel permeation chromatography.For polyacrylate they are Mn=12 000,Mw=15690,d=1.31,and that for polymethacrylate Mn=21255,Mw=38554 and d=1.81.
2003, 20(6): 520-523
Abstract:
The mechanism of catalytic hy drogenation of rosin over Raney-nickel catalyst has been studied using 200# gasoline as a solvent.The optimal processing conditions for hydrogenation of rosin have been attained by the uniform design experiments as follows,temperature 443 K,pressure 5.0 MPa,catalyst content 5.0% (based on rosin),solvent content 50% (based on solution),reaction time 100 min,stirring rate 600 r/min,and the conditions for kinetics experiment were then obtained.The relation between reactant concentration and reaction time was traced on line,and the parameters have been reg ressed by using EVIEWS.Based on the experiment results,a suitable reaction model has been deduced from Hougen-Warson 17 reaction mechanism models.It appeared that a reaction occurrs between abietic acid molecules and hydrogen atom adsorbed on the catalyst surface,and the dissociation adsorption of hydrogen could be the controlling step,and the reaction rate is proportional to the pressure of hydrogen and inversely proportional to the square of product concentration.Comparisons undertaken between melting method and solvent process showed that the hydrogenation reaction rate of the solvent process is greater than that of the melting method.
The mechanism of catalytic hy drogenation of rosin over Raney-nickel catalyst has been studied using 200# gasoline as a solvent.The optimal processing conditions for hydrogenation of rosin have been attained by the uniform design experiments as follows,temperature 443 K,pressure 5.0 MPa,catalyst content 5.0% (based on rosin),solvent content 50% (based on solution),reaction time 100 min,stirring rate 600 r/min,and the conditions for kinetics experiment were then obtained.The relation between reactant concentration and reaction time was traced on line,and the parameters have been reg ressed by using EVIEWS.Based on the experiment results,a suitable reaction model has been deduced from Hougen-Warson 17 reaction mechanism models.It appeared that a reaction occurrs between abietic acid molecules and hydrogen atom adsorbed on the catalyst surface,and the dissociation adsorption of hydrogen could be the controlling step,and the reaction rate is proportional to the pressure of hydrogen and inversely proportional to the square of product concentration.Comparisons undertaken between melting method and solvent process showed that the hydrogenation reaction rate of the solvent process is greater than that of the melting method.
2003, 20(6): 524-527
Abstract:
Co-Al layered double hydroxides (LDH) were prepared by chemical co-precipitation.Part of them were treated by hydrothermal method at 130℃ for 16 h.The two materials are of layered structure and belong to hexagonal system as characterized by XRD,and the latter becomes further crystallized.Electrochemical measurements show that two Co-AlLDHs as electrode material have typical capacitance property in a 6 mol/LKOH aqueous electrolyte.The specific capacitance of single electrode is 400 F/g and 460 F/g respectively and the latter's impedance is only tens of mΩ.After 200 cycles the latter's capacitance decreases little.
Co-Al layered double hydroxides (LDH) were prepared by chemical co-precipitation.Part of them were treated by hydrothermal method at 130℃ for 16 h.The two materials are of layered structure and belong to hexagonal system as characterized by XRD,and the latter becomes further crystallized.Electrochemical measurements show that two Co-AlLDHs as electrode material have typical capacitance property in a 6 mol/LKOH aqueous electrolyte.The specific capacitance of single electrode is 400 F/g and 460 F/g respectively and the latter's impedance is only tens of mΩ.After 200 cycles the latter's capacitance decreases little.
2003, 20(6): 528-531
Abstract:
Calcium zincate as an active material in Zn/Ni secondary battery has been successfully synthesized by ball-milling method.Its chemical composition Ca(OH)2·2Zn(OH)2·2H2O was confirmed by DTATG and XRD.The SEM microphotos indicated that calcium zincate obtained by ball-milling not only has smaller particles but also larger specific surface area than that prepared by chemical method.The calcium zincate prepared by ball milling has a better cyclic behavior and a higher discharge capacity than that prepared by chemical method.
Calcium zincate as an active material in Zn/Ni secondary battery has been successfully synthesized by ball-milling method.Its chemical composition Ca(OH)2·2Zn(OH)2·2H2O was confirmed by DTATG and XRD.The SEM microphotos indicated that calcium zincate obtained by ball-milling not only has smaller particles but also larger specific surface area than that prepared by chemical method.The calcium zincate prepared by ball milling has a better cyclic behavior and a higher discharge capacity than that prepared by chemical method.
2003, 20(6): 532-536
Abstract:
Fourteen 2-(4-methylthiophenoxy)-4H-imidazolin-4-ones 3 were synthesized via tandem aza-Wittig reaction of viny liminophosphorane 1,aromatic isocynates and 4-methy lthiophenol.The structures of the compounds were characterized by elemental analysis,IR,MS and 1H NMR spectroscopy.The new compounds synthesized exhibited considerably good fungicidal activities,among them the compounds 2-(4-methylthiophenoxy)-3-(4-chlorophenyl)-5-(4-dichlorophenylmethylidene)-4H-imidazolin-4-one (3d) and 2-(4-methylthiophenoxy)-3-(4-chlorophenyl)-5-(3-bromophenylmethylidene)-4H-imidazolin-4-one (3e) exhibited 100% inhibition action against Pyricularia oryzae,Pellicularia sasakii,Cercospora asparagagas and Physalospora piricola in dosage of 5×10-5 (mass fraction).
Fourteen 2-(4-methylthiophenoxy)-4H-imidazolin-4-ones 3 were synthesized via tandem aza-Wittig reaction of viny liminophosphorane 1,aromatic isocynates and 4-methy lthiophenol.The structures of the compounds were characterized by elemental analysis,IR,MS and 1H NMR spectroscopy.The new compounds synthesized exhibited considerably good fungicidal activities,among them the compounds 2-(4-methylthiophenoxy)-3-(4-chlorophenyl)-5-(4-dichlorophenylmethylidene)-4H-imidazolin-4-one (3d) and 2-(4-methylthiophenoxy)-3-(4-chlorophenyl)-5-(3-bromophenylmethylidene)-4H-imidazolin-4-one (3e) exhibited 100% inhibition action against Pyricularia oryzae,Pellicularia sasakii,Cercospora asparagagas and Physalospora piricola in dosage of 5×10-5 (mass fraction).
2003, 20(6): 537-541
Abstract:
A soluble poly (2-methoxy-5-octyloxy)-p-phenylene vinylene (PMOCOPV) was synthesized through double etherification,chloromethylation and dehydrochlorination reactions.The structure of the PMOCOPV has been characterized by IR,UV-Vis,1H NMR and GPC.The conductivity of I2,Br2,FeCl3 and H2SO4 doped PMOCOPV was 47.2,21.6,32.5 and 2.7 S/cm,respectively.The third-order nonlinear optical property of PMOCOPV was studied by degenerate four-wave mixing (DFWM).The resonant value of 6.8×10-10 esu at 532 nm and the off-resonant value of 1.2×10-11 esu at 1064 nm of third-order optical nonlinear susceptibilities were measured respectively.
A soluble poly (2-methoxy-5-octyloxy)-p-phenylene vinylene (PMOCOPV) was synthesized through double etherification,chloromethylation and dehydrochlorination reactions.The structure of the PMOCOPV has been characterized by IR,UV-Vis,1H NMR and GPC.The conductivity of I2,Br2,FeCl3 and H2SO4 doped PMOCOPV was 47.2,21.6,32.5 and 2.7 S/cm,respectively.The third-order nonlinear optical property of PMOCOPV was studied by degenerate four-wave mixing (DFWM).The resonant value of 6.8×10-10 esu at 532 nm and the off-resonant value of 1.2×10-11 esu at 1064 nm of third-order optical nonlinear susceptibilities were measured respectively.
Electrochemical Behavior of 2, 5-Dimercapto-1, 3, 4-thiadiazole/Poly-o-toluidine Composite Electrode
2003, 20(6): 542-546
Abstract:
The electrochemical behavior of DMcT/POT composite electrode are studied by cyclic voltammetry.It suggested that copper could be more suitable for the current collector than other metals like Pt,Al,Ni.The current efficiency of electrode is enhanced with the increase of the POT content in the DMcT/POT composite.But the best reversibility of the DMcT/POT composite electrode appeared when DMcT/POT (wet.)=1.
The electrochemical behavior of DMcT/POT composite electrode are studied by cyclic voltammetry.It suggested that copper could be more suitable for the current collector than other metals like Pt,Al,Ni.The current efficiency of electrode is enhanced with the increase of the POT content in the DMcT/POT composite.But the best reversibility of the DMcT/POT composite electrode appeared when DMcT/POT (wet.)=1.
2003, 20(6): 547-551
Abstract:
HA/Ag composite coatings were prepared by two-step electrodeposition in aquatic electrolytes containing calcium and phosphate ions and subsequently electroplating of silver in nicotinic acid bath.The influence of different working process on the content of silver in the coating,the influences of silver plating on the bonding strength and composition and structure of coating were investigated.The results show that the content of silver in the coating reduces and the densification degree of the coatings increases with decrease of the salt concentration,current density and with prolonging of the deposition time.The bonding strength of HA/Ag composite coating sare much greater than that of pure HA coatings.HA in coatings could be decomposed when the sintering temperature above 750℃,the reaction is obviously catalyzed by presence of silver.
HA/Ag composite coatings were prepared by two-step electrodeposition in aquatic electrolytes containing calcium and phosphate ions and subsequently electroplating of silver in nicotinic acid bath.The influence of different working process on the content of silver in the coating,the influences of silver plating on the bonding strength and composition and structure of coating were investigated.The results show that the content of silver in the coating reduces and the densification degree of the coatings increases with decrease of the salt concentration,current density and with prolonging of the deposition time.The bonding strength of HA/Ag composite coating sare much greater than that of pure HA coatings.HA in coatings could be decomposed when the sintering temperature above 750℃,the reaction is obviously catalyzed by presence of silver.
2003, 20(6): 552-556
Abstract:
The doped spherical Ni(OH)2 was prepared by ammonia complexing liquid phase codeposition method,using graphite powder and acetylene-black as dopants.XRD and SEM results indicated the intercalation of carbon dopants within the spherical Ni(OH)2.The charge-discharge experiments showed that for Ni(OH)2 electrodes without using graphite powder and acetylene-black as dopants,the discharging capacity and voltage at plateau were 270 mA·h/g by 0.2C,220 mA·h/g by 2C and 302 mV,respectively;for electrodes doped with 5.0% graphite,the corresponding values were 253 mA·h/g,216 mA·h/g and 320 mV,respectively;for electrodes doped with 5.0% acetylene-black,the corresponding values were 258 mA·h/g,222 mA·h/g and 324 mV,respectively.With electronic conductor being increased,the discharge capacity is decreased and the plateau voltage and the discharge ability at high rate are increased.
The doped spherical Ni(OH)2 was prepared by ammonia complexing liquid phase codeposition method,using graphite powder and acetylene-black as dopants.XRD and SEM results indicated the intercalation of carbon dopants within the spherical Ni(OH)2.The charge-discharge experiments showed that for Ni(OH)2 electrodes without using graphite powder and acetylene-black as dopants,the discharging capacity and voltage at plateau were 270 mA·h/g by 0.2C,220 mA·h/g by 2C and 302 mV,respectively;for electrodes doped with 5.0% graphite,the corresponding values were 253 mA·h/g,216 mA·h/g and 320 mV,respectively;for electrodes doped with 5.0% acetylene-black,the corresponding values were 258 mA·h/g,222 mA·h/g and 324 mV,respectively.With electronic conductor being increased,the discharge capacity is decreased and the plateau voltage and the discharge ability at high rate are increased.
2003, 20(6): 557-561
Abstract:
The properties of the organic monolayers formed by grafting of alcohols on the Si(111)-H surface have been investigated by interface capacity analysis,combined with XPS and AFM technique.Some factors influencing the properties of the monolayers,their stability and passivation towards oxidation of silicon surface were examined.The results showed that under the reaction conditions used,the grafted molecules occupied about 0.80 volume fraction on the silicon surface modified by alcohol molecules of different chain length,with plat potential being about -1.00 V/(vs.SSE).The results demonstrated that the stability and passivation of these monolayers are deficient.
The properties of the organic monolayers formed by grafting of alcohols on the Si(111)-H surface have been investigated by interface capacity analysis,combined with XPS and AFM technique.Some factors influencing the properties of the monolayers,their stability and passivation towards oxidation of silicon surface were examined.The results showed that under the reaction conditions used,the grafted molecules occupied about 0.80 volume fraction on the silicon surface modified by alcohol molecules of different chain length,with plat potential being about -1.00 V/(vs.SSE).The results demonstrated that the stability and passivation of these monolayers are deficient.
2003, 20(6): 562-565
Abstract:
Fire-retardant acrylic ester was prepared by the radical copolymerizations.The effects of the amount of 2,4,6-tribromophernyl methacrylate and initiator,cross-linkable monomer,reaction temperature and reaction time on peeling strength of the polyacrylate were investigated.The composition of monomer,the synthetic technology and the properties of acrylic ester adhesive were investigated.The peeling strength (PS) of fire-retardant acrylic ester adhesives was 19.5 N/cm at room temperature.Fire-retardant polyacrylate adhesive have excellent fire-retarding property.
Fire-retardant acrylic ester was prepared by the radical copolymerizations.The effects of the amount of 2,4,6-tribromophernyl methacrylate and initiator,cross-linkable monomer,reaction temperature and reaction time on peeling strength of the polyacrylate were investigated.The composition of monomer,the synthetic technology and the properties of acrylic ester adhesive were investigated.The peeling strength (PS) of fire-retardant acrylic ester adhesives was 19.5 N/cm at room temperature.Fire-retardant polyacrylate adhesive have excellent fire-retarding property.
2003, 20(6): 566-569
Abstract:
A novel simultaneous interpenetrating polymer networks (SIN) damping material has been synthesized based on polyphenylsiloxane (PMPS) and poly (ethyl methacrylate)(PEMA).The average molecular weight between crosslinking point in SIN was found decreased with increase of the crosslinking agent polypropylene glycol diacrylate (PPDA),content in PEMA when ω(PMPS):ω(PEMA) was 50:50.According to the DMA,DSC and AFM results,the loss peak profits,heights and the temperature regions of tan δ≥0.3 all depended on the crosslinking agent content in PEMA,and it was also true for both the area under the curves of linear loss modulus vs temperature (LA) and the area under the linear loss factor vs temperature (TA).With mass fraction of crosslinking agent being 5%,the maximum TA and LA values were obtained and a damping platform appeared and the temperture region for tan δ≥0.3 could reach 170℃.
A novel simultaneous interpenetrating polymer networks (SIN) damping material has been synthesized based on polyphenylsiloxane (PMPS) and poly (ethyl methacrylate)(PEMA).The average molecular weight between crosslinking point in SIN was found decreased with increase of the crosslinking agent polypropylene glycol diacrylate (PPDA),content in PEMA when ω(PMPS):ω(PEMA) was 50:50.According to the DMA,DSC and AFM results,the loss peak profits,heights and the temperature regions of tan δ≥0.3 all depended on the crosslinking agent content in PEMA,and it was also true for both the area under the curves of linear loss modulus vs temperature (LA) and the area under the linear loss factor vs temperature (TA).With mass fraction of crosslinking agent being 5%,the maximum TA and LA values were obtained and a damping platform appeared and the temperture region for tan δ≥0.3 could reach 170℃.
2003, 20(6): 570-573
Abstract:
The oxidation of cyclohexene to adipic acid catalyzed by heteropolyacids has been investigated,using 30% aqueous hydrogen peroxide as an oxidant,and dicarboxy licacids or 8-hydroxyquinoline as cocatalyst.Adipic acid in yield up to 75.0% was obtained in 6 h,in the presence of 8-hydroxy quinoline.When oxalic acid was used as cocatalyst in condition of 92℃,6 h,n(cyclohexene):n(H3PW12O40):n(H2C2O4):n(H2O2)=100:1:1:538,the yield of adipic acid was 70.1%.When cetyltrimethyl ammonium bromide or cetylpyridinium bromide was used as phase transfer catalyst,the yield of adipic acid was 73.1% and 71.6% respectively.Catalytic oxidation of cyclohexene oxide or trans-1,2-cyclohexanediol to adipic acid over tungtophosphoric acid were also carried out in order to confirm the reported mechanism of the reaction.
The oxidation of cyclohexene to adipic acid catalyzed by heteropolyacids has been investigated,using 30% aqueous hydrogen peroxide as an oxidant,and dicarboxy licacids or 8-hydroxyquinoline as cocatalyst.Adipic acid in yield up to 75.0% was obtained in 6 h,in the presence of 8-hydroxy quinoline.When oxalic acid was used as cocatalyst in condition of 92℃,6 h,n(cyclohexene):n(H3PW12O40):n(H2C2O4):n(H2O2)=100:1:1:538,the yield of adipic acid was 70.1%.When cetyltrimethyl ammonium bromide or cetylpyridinium bromide was used as phase transfer catalyst,the yield of adipic acid was 73.1% and 71.6% respectively.Catalytic oxidation of cyclohexene oxide or trans-1,2-cyclohexanediol to adipic acid over tungtophosphoric acid were also carried out in order to confirm the reported mechanism of the reaction.
2003, 20(6): 574-577
Abstract:
The acrylic ester emulsifier-free emulsion was synthesized from methyl methacrylate、n-butyl acrylate and methacrylic acid and the effects of epoxysiloxane on the glossiness,water absorption and pencil hardness of the polymer and on the Ca2+ stability of the emulsion were studied.It was found that the glossiness of the polymer was reduced from 89.8% to 70.9%,Ca2+ stability from 9.7 mL to 2.7 mL,pencil hardness from 2B to 3H and the water absorption from 24.9% to 0.2% with the increase of epoxy siloxane,respectively.The optimum molar ratio of epoxysiloxane to MAA was found to be 1.The granding analysis demonstrated the cross-linking reaction between epoxy siloxane and methyl acrylic acid.A crosslinking mechanism is proposed.
The acrylic ester emulsifier-free emulsion was synthesized from methyl methacrylate、n-butyl acrylate and methacrylic acid and the effects of epoxysiloxane on the glossiness,water absorption and pencil hardness of the polymer and on the Ca2+ stability of the emulsion were studied.It was found that the glossiness of the polymer was reduced from 89.8% to 70.9%,Ca2+ stability from 9.7 mL to 2.7 mL,pencil hardness from 2B to 3H and the water absorption from 24.9% to 0.2% with the increase of epoxy siloxane,respectively.The optimum molar ratio of epoxysiloxane to MAA was found to be 1.The granding analysis demonstrated the cross-linking reaction between epoxy siloxane and methyl acrylic acid.A crosslinking mechanism is proposed.
2003, 20(6): 578-581
Abstract:
The precursor Ti(OEt)4 was prepared by anodic dissolution of Ti in absolute ethanol and directly hydrolyzed to give nanocrystalline TiO2 film on titanium electrode (Ti/nano-TiO2) by a sol-gel process.The nanocrystalline TiO2-Pt modified titanium (Ti/nano-TiO2-Pt) electrode was prepared by electrodeposition of Pt on nanocrystalline TiO2 film.Electrocatalytic activity of the Ti/nano-TiO2-Pt electrode for oxidation of Mn2+ to Mn3+ and synthesis of glyceraldehydes were investigated by cyclic voltammetry and indirect electro-oxidation methods.Mn3+ could be regenerated by electrolysis at Ti/nano-TiO2-Pt anode in heterogeneous MnSO4/H2SO4 medium with current efficiency over 90%.Glyceraldehyde was prepared in yield of 91% by the proposed method.
The precursor Ti(OEt)4 was prepared by anodic dissolution of Ti in absolute ethanol and directly hydrolyzed to give nanocrystalline TiO2 film on titanium electrode (Ti/nano-TiO2) by a sol-gel process.The nanocrystalline TiO2-Pt modified titanium (Ti/nano-TiO2-Pt) electrode was prepared by electrodeposition of Pt on nanocrystalline TiO2 film.Electrocatalytic activity of the Ti/nano-TiO2-Pt electrode for oxidation of Mn2+ to Mn3+ and synthesis of glyceraldehydes were investigated by cyclic voltammetry and indirect electro-oxidation methods.Mn3+ could be regenerated by electrolysis at Ti/nano-TiO2-Pt anode in heterogeneous MnSO4/H2SO4 medium with current efficiency over 90%.Glyceraldehyde was prepared in yield of 91% by the proposed method.
2003, 20(6): 582-585
Abstract:
2-Acetyl-pyridin ketazine and its complexes with Co2+,Ni2+,Fe3+,Zn2+ were synthesized respectively by refluxing it with conresponding salts [FeCl3,CoCl2,Ni(NO3)2,ZnCl2].The compositions and structures of the ligand and complexes have been characterized by the elemental analysis,IR spectra and UV spectra.Their inhibiting actions on the superoxide anions were examined by using nitroblue tetrazolium (NBT) method.Their bioactivities against P388-leucocythemia for rats were tested by using methyl-thiazoltetrazolium (MTT) method and against A-549 human lung cancer cells by sulforhodamine B(SRB) method,both in vitro.The ligand and all of the complexes were found to be bioactive,while Co-and Nicomplexes showed greater activities and Fe- and Zn-complexes were weaker than the ligand.It is deduced that the activities of the complexes may depend on the structure of the outermost d-orbital electrons.
2-Acetyl-pyridin ketazine and its complexes with Co2+,Ni2+,Fe3+,Zn2+ were synthesized respectively by refluxing it with conresponding salts [FeCl3,CoCl2,Ni(NO3)2,ZnCl2].The compositions and structures of the ligand and complexes have been characterized by the elemental analysis,IR spectra and UV spectra.Their inhibiting actions on the superoxide anions were examined by using nitroblue tetrazolium (NBT) method.Their bioactivities against P388-leucocythemia for rats were tested by using methyl-thiazoltetrazolium (MTT) method and against A-549 human lung cancer cells by sulforhodamine B(SRB) method,both in vitro.The ligand and all of the complexes were found to be bioactive,while Co-and Nicomplexes showed greater activities and Fe- and Zn-complexes were weaker than the ligand.It is deduced that the activities of the complexes may depend on the structure of the outermost d-orbital electrons.
2003, 20(6): 586-589
Abstract:
Granular CeO2/SiO2 capable of absorbing fluorine regents has been prepared by impregnation method followed by calcination.The samples are characterized by DTA-TG,XRD and IR and the F- adsorbi-lity measurements.The adsorptivity of CeO2/SiO2 tow ards F- is decreased with increase in calcination temperature in the range of 400 to 800℃.The isothermal adsorption of F- on CeO2/SiO2 conforms to Freundlich equation.CeO2 in CeO2/SiO2 sample obtained from calcination at 400℃ appeared to be a crystalline.
Granular CeO2/SiO2 capable of absorbing fluorine regents has been prepared by impregnation method followed by calcination.The samples are characterized by DTA-TG,XRD and IR and the F- adsorbi-lity measurements.The adsorptivity of CeO2/SiO2 tow ards F- is decreased with increase in calcination temperature in the range of 400 to 800℃.The isothermal adsorption of F- on CeO2/SiO2 conforms to Freundlich equation.CeO2 in CeO2/SiO2 sample obtained from calcination at 400℃ appeared to be a crystalline.
Synthesis of Glucosides XXⅠ Synthesis of 2-N-(β-D-Glucopyranos-1-yl)-6-(4-Halophenyl)-3-Pyridazinone
2003, 20(6): 590-593
Abstract:
Four pyridazinone glucosides 3 were synthesized by reaction of 2,3,4,6-tetra-O-acetyl-1-bromo-1-deoxy-α-D-glucopyranose 1 with 6-(4-halophenyl)-3(2H)-pyridazinone 2 under phase transfer catalysis conditions,followed by treatment with dry am monia at 0~-5℃ to yield title compounds 4.Their structures were characterized by IR,1H NMR,13C NMR and elemental analysis.
Four pyridazinone glucosides 3 were synthesized by reaction of 2,3,4,6-tetra-O-acetyl-1-bromo-1-deoxy-α-D-glucopyranose 1 with 6-(4-halophenyl)-3(2H)-pyridazinone 2 under phase transfer catalysis conditions,followed by treatment with dry am monia at 0~-5℃ to yield title compounds 4.Their structures were characterized by IR,1H NMR,13C NMR and elemental analysis.
2003, 20(6): 594-596
Abstract:
Eight N-5-(3-carboxy-1,2,4-triazolyl)-N'-aroyl ureas have been synthesized from 3-amino-1,2,4-triazolyl-5-carboxylic acid and substituted benzoylisocyanates in yields of 59.6%~55.9% with mp>300℃.The structures of the title compounds were confirmed by IR,1H NMR and elemental analysis.The room temperature biological activity tests showed that some target compounds have a good activity as plant grow th regulator,the best of them appeared compounds Ⅱb and Ⅱc (for auxin).
Eight N-5-(3-carboxy-1,2,4-triazolyl)-N'-aroyl ureas have been synthesized from 3-amino-1,2,4-triazolyl-5-carboxylic acid and substituted benzoylisocyanates in yields of 59.6%~55.9% with mp>300℃.The structures of the title compounds were confirmed by IR,1H NMR and elemental analysis.The room temperature biological activity tests showed that some target compounds have a good activity as plant grow th regulator,the best of them appeared compounds Ⅱb and Ⅱc (for auxin).
2003, 20(6): 597-599
Abstract:
A polymeric compound of urushiol-Al modified carbon paste electrode was examined for the determination of trace silver in water.In 0.1 mol/L KNO3 and HAc-NaAc solution (pH=5.5),silver is accumulated on the surface of the modified carbon paste electrode at -0.1 V(vs.SCE).In the following step,a sensitive oxidation peak of Ag+ at 0.22 V could be observed by anodic stripping voltammetry.The peak current is linearly related to the concentration of silver ranged from 4.0×10-9 mol/L to 2.5×10-7 mol/L.The detection limit (signal-to-noise=3) is 1.5×10-10 mol/L after 20 min accumulation,the average recovery is 100.3%.
A polymeric compound of urushiol-Al modified carbon paste electrode was examined for the determination of trace silver in water.In 0.1 mol/L KNO3 and HAc-NaAc solution (pH=5.5),silver is accumulated on the surface of the modified carbon paste electrode at -0.1 V(vs.SCE).In the following step,a sensitive oxidation peak of Ag+ at 0.22 V could be observed by anodic stripping voltammetry.The peak current is linearly related to the concentration of silver ranged from 4.0×10-9 mol/L to 2.5×10-7 mol/L.The detection limit (signal-to-noise=3) is 1.5×10-10 mol/L after 20 min accumulation,the average recovery is 100.3%.
2003, 20(6): 600-602
Abstract:
A preparation method of glutaraldehyde by one-step oxidation of cyclopentene with peroxyformic acid is reported.The preparation is carried out in a mild reaction condition,time saving and without catalyst.The product is identified by MS and IR measurements.The results showed that the highest yield of glutaraldehyde 56.7% is obtained at optimum molar ratio of n(hydrogen peroxide):n(cyclopentene):n(formic acid)=1:3:3,reaction temperature 35℃ and reaction time 1 h.
A preparation method of glutaraldehyde by one-step oxidation of cyclopentene with peroxyformic acid is reported.The preparation is carried out in a mild reaction condition,time saving and without catalyst.The product is identified by MS and IR measurements.The results showed that the highest yield of glutaraldehyde 56.7% is obtained at optimum molar ratio of n(hydrogen peroxide):n(cyclopentene):n(formic acid)=1:3:3,reaction temperature 35℃ and reaction time 1 h.
2003, 20(6): 603-605
Abstract:
Eight allyl thionophosphates were synthesized by the condensation reaction of PSCl3 with methanol or ethanol、sodium ally late and sodium nitrophenolate and identified by IR、1H NMR、31P NMR and elemental anaylsis.The title compounds had good insecticidal activity against aphid at dosage of 0.025%.
Eight allyl thionophosphates were synthesized by the condensation reaction of PSCl3 with methanol or ethanol、sodium ally late and sodium nitrophenolate and identified by IR、1H NMR、31P NMR and elemental anaylsis.The title compounds had good insecticidal activity against aphid at dosage of 0.025%.
2003, 20(6): 606-608
Abstract:
Exfoliated polystyrene/laponite nanocomposite was synthesized successfully.XRD patterns of nanocomposites showed the d001 diffraction peaks of organo-laponite disappeared,indicating that the laponite layers became exfoliated and disordered in result of the polymerization process;TEM photographs showed that the disordered laponite layers or primary particles with sizes about 30~100 nm were dispersed in the polystyrene matrix.TGA and DSC results showed the thermal stability and glass transition temperature of the polystyrene/organo-laponite nanocom posites were obviously improved compared to that of the polystyrene.
Exfoliated polystyrene/laponite nanocomposite was synthesized successfully.XRD patterns of nanocomposites showed the d001 diffraction peaks of organo-laponite disappeared,indicating that the laponite layers became exfoliated and disordered in result of the polymerization process;TEM photographs showed that the disordered laponite layers or primary particles with sizes about 30~100 nm were dispersed in the polystyrene matrix.TGA and DSC results showed the thermal stability and glass transition temperature of the polystyrene/organo-laponite nanocom posites were obviously improved compared to that of the polystyrene.
2003, 20(6): 609-610
Abstract:
A series of urethane acrylate anionomers (PU) in molar ratio of n(PEG):n(DMPA):n(HMDI):n(2-HPA)=0.3:0.7:(1.2~1.5):(0.44~1.1) were prepared in 3 steps.The structure of the prepolymer was confirmed by FT-IR and 1H NM R analysis.pH-sensitive cross-linked films were then obtained by UV polymerization of UAA.The swelling property of the films with respect to pH was much affected by the composition of the prepolymer.The film could swell and deswell rapidly and reversibly in buffer solutions of pH=3 and pH=11.
A series of urethane acrylate anionomers (PU) in molar ratio of n(PEG):n(DMPA):n(HMDI):n(2-HPA)=0.3:0.7:(1.2~1.5):(0.44~1.1) were prepared in 3 steps.The structure of the prepolymer was confirmed by FT-IR and 1H NM R analysis.pH-sensitive cross-linked films were then obtained by UV polymerization of UAA.The swelling property of the films with respect to pH was much affected by the composition of the prepolymer.The film could swell and deswell rapidly and reversibly in buffer solutions of pH=3 and pH=11.
2003, 20(6): 611-612
Abstract:
N-Hydroxy succinimide was synthesized from succinic anhydride and hydroxylamine in yield 58%~61% with purity ≥97%.The method has advantages of simplicity and high yield and purity.
N-Hydroxy succinimide was synthesized from succinic anhydride and hydroxylamine in yield 58%~61% with purity ≥97%.The method has advantages of simplicity and high yield and purity.
