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2014 Volume 31 Issue 9
2014, 31(9): 993-1009
doi: 10.3724/SP.J.1095.2014.30536
Abstract:
In this paper, the synthesis and reaction mechanism of hexachlorocyclotriphosphazene were briefly introduced. The flame-retardant mechanism of cyclotriphosphazene-based flame retardants was also summarized. The reactive-type hydroxyl, amino, epoxy, alkenyl, and carboxyl, cyclotriphosphazene and the additive-type alkoxy and aryloxy cyclotriphosphazene flame retardants were elaborated on their synthesis and application. The thermal stability and flame retardant properties of cyclotriphosphazene-based flame retardant materials were summarized. The development trend of cyclotriphosphazene-based flame retardants was also summarized and prospected.
In this paper, the synthesis and reaction mechanism of hexachlorocyclotriphosphazene were briefly introduced. The flame-retardant mechanism of cyclotriphosphazene-based flame retardants was also summarized. The reactive-type hydroxyl, amino, epoxy, alkenyl, and carboxyl, cyclotriphosphazene and the additive-type alkoxy and aryloxy cyclotriphosphazene flame retardants were elaborated on their synthesis and application. The thermal stability and flame retardant properties of cyclotriphosphazene-based flame retardant materials were summarized. The development trend of cyclotriphosphazene-based flame retardants was also summarized and prospected.
2014, 31(9): 1010-1018
doi: 10.3724/SP.J.1095.2014.30634
Abstract:
Recently, the liquid-liquid interfacial synthesis is emerging as an efficient strategy for the preparation of nanomaterials, which exhibits several outstanding characteristics:mild, inexpensive, convenient and template-free. Owing to the unusual physicochemical properties, the liquid-liquid interface possesses unique advantages in the synthesis of nanomaterials and thin films. In this paper, the recent advances in the preparation of nanomaterials at the liquid-liquid interface were reviewed in details. By applying this simple strategy, a variety of nanomaterials were easily obtained, including metal, metal oxides, metal chalcogenides, polymers, heterodimers, and metal-organic frameworks. Particularly, the new protocol of "tunable ionic liquids-H2O interfacial synthesis" was commented. Finally, the advantages and problems in the liquid-liquid interfacial synthesis of nanomaterials were also discussed, and the future development in this research area was presented.
Recently, the liquid-liquid interfacial synthesis is emerging as an efficient strategy for the preparation of nanomaterials, which exhibits several outstanding characteristics:mild, inexpensive, convenient and template-free. Owing to the unusual physicochemical properties, the liquid-liquid interface possesses unique advantages in the synthesis of nanomaterials and thin films. In this paper, the recent advances in the preparation of nanomaterials at the liquid-liquid interface were reviewed in details. By applying this simple strategy, a variety of nanomaterials were easily obtained, including metal, metal oxides, metal chalcogenides, polymers, heterodimers, and metal-organic frameworks. Particularly, the new protocol of "tunable ionic liquids-H2O interfacial synthesis" was commented. Finally, the advantages and problems in the liquid-liquid interfacial synthesis of nanomaterials were also discussed, and the future development in this research area was presented.
2014, 31(9): 1019-1023
doi: 10.3724/SP.J.1095.2014.30599
Abstract:
Sodium n-butylxanthate obtained from n-butyl alcohol, sodium hydroxide and carbon disulfide in water was converted to symmetrical dibutyl xanthate disulfide by reacting with disulfur dichloride(S2Cl2) at room temperature. The effects of reaction conditions on the yields of the sodium n-butylxanthate and dibutyl xanthate disulfide were investigated respectively. Characterizations of dibutyl xanthate disulfide were done using Fourier transform infrared(FT-IR) spectroscopy, 1H nuclear magnetic resonance(1H NMR) spectroscopy, mass spectroscopy(MS) and elemental analysis techniques. In optimized reaction conditions, the molar ratio of sodium n-butylxanthate to S2Cl2 is 1:1.1 in THF solvent. The reaction completes within 2 min at room temperature to give up to 83.2% yield.
Sodium n-butylxanthate obtained from n-butyl alcohol, sodium hydroxide and carbon disulfide in water was converted to symmetrical dibutyl xanthate disulfide by reacting with disulfur dichloride(S2Cl2) at room temperature. The effects of reaction conditions on the yields of the sodium n-butylxanthate and dibutyl xanthate disulfide were investigated respectively. Characterizations of dibutyl xanthate disulfide were done using Fourier transform infrared(FT-IR) spectroscopy, 1H nuclear magnetic resonance(1H NMR) spectroscopy, mass spectroscopy(MS) and elemental analysis techniques. In optimized reaction conditions, the molar ratio of sodium n-butylxanthate to S2Cl2 is 1:1.1 in THF solvent. The reaction completes within 2 min at room temperature to give up to 83.2% yield.
2014, 31(9): 1024-1030
doi: 10.3724/SP.J.1095.2014.30585
Abstract:
A phosphated polyester polyol with a 1500 number average relative molecular mass was synthesized by 2-phosphono-1,2,4-butanetricarboxylic acid and 2,2-dimethyl-1,3-propane diol. Then the polyester polyol was reacted with isophorone diisocyanate to obtain the prepolymer. The prepolymer was extended by 1,4-butanediol and terminated by coupling agent KH550. At last nanosilica was added into the waterborne polyurethane(WPU) to obtain WPU/nanosilica composite. Fourier transform-infrared spectroscopy(FT-IR), thermal gravimetric analysis(TGA) and transmission electron microscopy(TEM) were used to study the structure and characteristics of the composite. In the TEM image of PWPU/SiO2, plenty of composite particles(~110 nm diameter) were observed. Combined analysis with the FI-IR, it was concluded that the nanosilica was linked with WPU by chemical bond. TGA, char yield and extension test showed that the fire retardancy property, thermostability and tensile strength of the composite increase significantly with tnanosilica modification. These results indicate that there is a good application prospect of the composite in the future.
A phosphated polyester polyol with a 1500 number average relative molecular mass was synthesized by 2-phosphono-1,2,4-butanetricarboxylic acid and 2,2-dimethyl-1,3-propane diol. Then the polyester polyol was reacted with isophorone diisocyanate to obtain the prepolymer. The prepolymer was extended by 1,4-butanediol and terminated by coupling agent KH550. At last nanosilica was added into the waterborne polyurethane(WPU) to obtain WPU/nanosilica composite. Fourier transform-infrared spectroscopy(FT-IR), thermal gravimetric analysis(TGA) and transmission electron microscopy(TEM) were used to study the structure and characteristics of the composite. In the TEM image of PWPU/SiO2, plenty of composite particles(~110 nm diameter) were observed. Combined analysis with the FI-IR, it was concluded that the nanosilica was linked with WPU by chemical bond. TGA, char yield and extension test showed that the fire retardancy property, thermostability and tensile strength of the composite increase significantly with tnanosilica modification. These results indicate that there is a good application prospect of the composite in the future.
2014, 31(9): 1031-1036
doi: 10.3724/SP.J.1095.2014.30604
Abstract:
The magnetic cross-linked chitosan microspheres were prepared using Fe3O4 nanoparticles as cores and chitosan(CS) as polymeric shell with diisobutylamine(FCS-DIBA) modification. For the Re(Ⅶ) species coexisting with Fe(Ⅲ), Zn(Ⅱ), Mn(Ⅶ) and Cu(Ⅱ), the FCS-DIBA adsorbent exhibits selectivity only for Re(Ⅶ) among coexisting heavy metals in pH=2. The maximum adsorption capacity for Re(Ⅶ) is up to 185 mg/g, The adsorption behavior fits the Langmuir isotherm model. The mechanism for these excellent adsorption characteristics was discussed.
The magnetic cross-linked chitosan microspheres were prepared using Fe3O4 nanoparticles as cores and chitosan(CS) as polymeric shell with diisobutylamine(FCS-DIBA) modification. For the Re(Ⅶ) species coexisting with Fe(Ⅲ), Zn(Ⅱ), Mn(Ⅶ) and Cu(Ⅱ), the FCS-DIBA adsorbent exhibits selectivity only for Re(Ⅶ) among coexisting heavy metals in pH=2. The maximum adsorption capacity for Re(Ⅶ) is up to 185 mg/g, The adsorption behavior fits the Langmuir isotherm model. The mechanism for these excellent adsorption characteristics was discussed.
2014, 31(9): 1037-1043
doi: 10.3724/SP.J.1095.2014.30582
Abstract:
Butylene fipronil-loaded microcapsules were prepared by layer-by-layer self-assembly of oppositely charged chitosan and sodium alginate as shell materials. Sodium dodecyl benzene sulfonate was selected as the dispersant by flowing point method. The prepared microcapsules were characterized. The effect of drug loadings, entrapment efficiency, release profiles and photo degradation rate with the increase of layers was systematically studied. The results show that microcapsules with six to eight layers are the best with the entrapment efficiency up to 80%, the release time of 60 h and the photolysis rate down to 20%.
Butylene fipronil-loaded microcapsules were prepared by layer-by-layer self-assembly of oppositely charged chitosan and sodium alginate as shell materials. Sodium dodecyl benzene sulfonate was selected as the dispersant by flowing point method. The prepared microcapsules were characterized. The effect of drug loadings, entrapment efficiency, release profiles and photo degradation rate with the increase of layers was systematically studied. The results show that microcapsules with six to eight layers are the best with the entrapment efficiency up to 80%, the release time of 60 h and the photolysis rate down to 20%.
2014, 31(9): 1044-1049
doi: 10.3724/SP.J.1095.2014.30554
Abstract:
A preliminary study was performed on the main influence factors of the hydrolysis of racemic ibuprofen n-octyl ester catalyzed by lipase immobilized in cetyl trimethyl ammonium bromide(CTAB)/p-octyl polyethylene glycol phenyl ether(TX-100) microemulsion-based gel(MBG). The lipase immobilized in CTAB/TX-100 MBG could smoothly catalyze the hydrolysis of S-ibuprofen n-octyl ester to S-ibuprofen in aqueous solution. As the content of TX-100 in EM(the mixture of n-butanol and TX-100) increased gradually, the reaction conversion(X) always increased correspondingly, but the enantiomeric excess of produced S-ibuprofen(eei) decreased slightly. The curve of X vs eei all showed bell shape with the content of water in MBG increasing and the optimum water content of MBG was 27.3%. The influence of phosphate buffer on X and ee i was generally greater than that of water dissolving gelatin. X increased significantly in the early reaction stage(before 16 h) and then increased slowly till 24 h and didn't change any more even though the reaction was prolonged, but the eei decreased slightly in whoe reaction process. No significant change on X was observed in the first 3 recycle of immobilized lipase, but X decreased obviously in the following recycles. The ee i also decreased as the recycle times increased. After 10 reusage, X and the eei decreased by 36.55% and 0.52%, respectively.
A preliminary study was performed on the main influence factors of the hydrolysis of racemic ibuprofen n-octyl ester catalyzed by lipase immobilized in cetyl trimethyl ammonium bromide(CTAB)/p-octyl polyethylene glycol phenyl ether(TX-100) microemulsion-based gel(MBG). The lipase immobilized in CTAB/TX-100 MBG could smoothly catalyze the hydrolysis of S-ibuprofen n-octyl ester to S-ibuprofen in aqueous solution. As the content of TX-100 in EM(the mixture of n-butanol and TX-100) increased gradually, the reaction conversion(X) always increased correspondingly, but the enantiomeric excess of produced S-ibuprofen(eei) decreased slightly. The curve of X vs eei all showed bell shape with the content of water in MBG increasing and the optimum water content of MBG was 27.3%. The influence of phosphate buffer on X and ee i was generally greater than that of water dissolving gelatin. X increased significantly in the early reaction stage(before 16 h) and then increased slowly till 24 h and didn't change any more even though the reaction was prolonged, but the eei decreased slightly in whoe reaction process. No significant change on X was observed in the first 3 recycle of immobilized lipase, but X decreased obviously in the following recycles. The ee i also decreased as the recycle times increased. After 10 reusage, X and the eei decreased by 36.55% and 0.52%, respectively.
2014, 31(9): 1050-1057
doi: 10.3724/SP.J.1095.2014.30583
Abstract:
A series of novel S-β-D-acetylglucosides of double heterocyclic 1,2,3-thiadiazole and 1,2,4-triazole compounds(6a~6d) was synthesized from substituted 1,2,3-thiadiazoles. The structures of target compounds were confirmed by 1H NMR, 13C NMR and IR spectroscopy. The antimicrobial activities of S-glucoside Schiff base and its corresponding reduced structure were compared emphatically. The data of in vitro antimicrobial activities show that most of the tested compounds display good antimicrobial activities against Staphylococcus aureus(S.a.)(ATCC 6538), Escherichia coli(E.c.)(ATCC 8099) as well as Monilia albican(M.a.)(ATCC 10231). The antimicrobial activities of S-glucoside Schiff base are better than that of the corresponding reduced structures. Especially, compound 5d shows stronger antibacterial activities than others, and the minimum value of MIC to 5d is better than that of fluconazole. The minimum values of MIC to all target compounds against S.a. are less than or equal to 32 mg/L.
A series of novel S-β-D-acetylglucosides of double heterocyclic 1,2,3-thiadiazole and 1,2,4-triazole compounds(6a~6d) was synthesized from substituted 1,2,3-thiadiazoles. The structures of target compounds were confirmed by 1H NMR, 13C NMR and IR spectroscopy. The antimicrobial activities of S-glucoside Schiff base and its corresponding reduced structure were compared emphatically. The data of in vitro antimicrobial activities show that most of the tested compounds display good antimicrobial activities against Staphylococcus aureus(S.a.)(ATCC 6538), Escherichia coli(E.c.)(ATCC 8099) as well as Monilia albican(M.a.)(ATCC 10231). The antimicrobial activities of S-glucoside Schiff base are better than that of the corresponding reduced structures. Especially, compound 5d shows stronger antibacterial activities than others, and the minimum value of MIC to 5d is better than that of fluconazole. The minimum values of MIC to all target compounds against S.a. are less than or equal to 32 mg/L.
2014, 31(9): 1058-1062
doi: 10.3724/SP.J.1095.2014.30517
Abstract:
The title complex, tris(2-methyl-2-phenyl) propyl tin trichloroacetic acid ester(CCDC:932139), was synthesized by the reaction of bis[tris(2-methyl-2-phenyl) propyl]tin oxide with trichloroacetic acid and characterized by IR, 1H NMR spectroscopy and elemental analysis, respectively. The crystal structure was determined by X-ray diffraction to be monoclinic with a P21/n space group with a=1.1186(4) nm, b=1.8366(7) nm, c=1.6020(6) nm, α=90°, β=91.316(10) °, γ=90°, V=3.2902(19) nm3, Z=4, Dc=1.374 g/cm3, μ(MoKα)=1.046 mm-1, F(000)=1392, and R1=0.0589, wR2=0.1619. The crystal structure shows that the central Sn atom is four-coordinated to assume a distorted tetrahedral configuration. Bioassay results show that the complex displays good in vitro antitumor activities against five human tumor cell lines, HT-29, HepG-2, MCF-7, KB and A549, and has selective antibacterial property.
The title complex, tris(2-methyl-2-phenyl) propyl tin trichloroacetic acid ester(CCDC:932139), was synthesized by the reaction of bis[tris(2-methyl-2-phenyl) propyl]tin oxide with trichloroacetic acid and characterized by IR, 1H NMR spectroscopy and elemental analysis, respectively. The crystal structure was determined by X-ray diffraction to be monoclinic with a P21/n space group with a=1.1186(4) nm, b=1.8366(7) nm, c=1.6020(6) nm, α=90°, β=91.316(10) °, γ=90°, V=3.2902(19) nm3, Z=4, Dc=1.374 g/cm3, μ(MoKα)=1.046 mm-1, F(000)=1392, and R1=0.0589, wR2=0.1619. The crystal structure shows that the central Sn atom is four-coordinated to assume a distorted tetrahedral configuration. Bioassay results show that the complex displays good in vitro antitumor activities against five human tumor cell lines, HT-29, HepG-2, MCF-7, KB and A549, and has selective antibacterial property.
2014, 31(9): 1063-1068
doi: 10.3724/SP.J.1095.2014.40056
Abstract:
The bis-β-diketone molecule incorporating 1,3-propanedithioether bridge between the γ-carbons of respective β-diketone units of 1,3-bis(3-thio-2,4-pentanedionate) propane(L1) was designed and synthesized via the Williamson reaction. The structure of bis-β-diketone L1 was characterized by elemental analysis, 1H NMR,13C NMR, MS, IR, UV and X-ray single crystal diffraction analysis. The analysis results show that the crystal of bis-β-diketone L1 belongs to monoclinic, space group C2/c with cell parameters a=1.40679(9) nm, b=0.76521(5) nm, c=1.43213(10) nm, α=γ=90°, β=94.552°, V=1.53681(18) nm3, Z=4, Dc=1.316 g/cm3, μ=0.353 mm-1, F(000)=648, and bis-β-diketone L1 exists in the enol form in both solid state and chloroform solution. The recognition and extraction properties of the target compound L1 with metal ions were investigated by the ultraviolet spectroscopy. The results show that bis-β-diketone L1 has a good selective recognition and extraction property for Ni(Ⅱ) ion.
The bis-β-diketone molecule incorporating 1,3-propanedithioether bridge between the γ-carbons of respective β-diketone units of 1,3-bis(3-thio-2,4-pentanedionate) propane(L1) was designed and synthesized via the Williamson reaction. The structure of bis-β-diketone L1 was characterized by elemental analysis, 1H NMR,13C NMR, MS, IR, UV and X-ray single crystal diffraction analysis. The analysis results show that the crystal of bis-β-diketone L1 belongs to monoclinic, space group C2/c with cell parameters a=1.40679(9) nm, b=0.76521(5) nm, c=1.43213(10) nm, α=γ=90°, β=94.552°, V=1.53681(18) nm3, Z=4, Dc=1.316 g/cm3, μ=0.353 mm-1, F(000)=648, and bis-β-diketone L1 exists in the enol form in both solid state and chloroform solution. The recognition and extraction properties of the target compound L1 with metal ions were investigated by the ultraviolet spectroscopy. The results show that bis-β-diketone L1 has a good selective recognition and extraction property for Ni(Ⅱ) ion.
2014, 31(9): 1069-1075
doi: 10.3724/SP.J.1095.2014.30606
Abstract:
Methylimidazole and 3-chloro-1 propanol were used as materials to synthesize ionic liquids(1-hydroxypropyl-3-methylimidazolium tetrafluoroborate, NpmimBF4), and its graft was immobilized to mesoporous materials(FDU-15), thus for synthesizing and preparing mesoporous catalyst(NpmimBF4-FDU). Techniques such as thermogravimetry, X-ray diffraction, infra-red spectrum and transmission electron microscope were employed to characterize the structure of catalyst. The catalytic activity of the catalyst was investigated in the hydrolysis reaction of propylene carbonate(PC). The result shows that the catalyst can effectively catalyze the hydrolysis of propylene carbonate to 1,2-propanediol glycol at normal pressure. When mass fraction of the catalyst is 4%, temperature is 80℃ and the reaction time is 2 h, the yield of 1,2-propanediol glycol is more than 99%. The catalyst can be repeatedly used for 5 times after simple separation but its activity changes greatly. A reaction mechanism is proposed.
Methylimidazole and 3-chloro-1 propanol were used as materials to synthesize ionic liquids(1-hydroxypropyl-3-methylimidazolium tetrafluoroborate, NpmimBF4), and its graft was immobilized to mesoporous materials(FDU-15), thus for synthesizing and preparing mesoporous catalyst(NpmimBF4-FDU). Techniques such as thermogravimetry, X-ray diffraction, infra-red spectrum and transmission electron microscope were employed to characterize the structure of catalyst. The catalytic activity of the catalyst was investigated in the hydrolysis reaction of propylene carbonate(PC). The result shows that the catalyst can effectively catalyze the hydrolysis of propylene carbonate to 1,2-propanediol glycol at normal pressure. When mass fraction of the catalyst is 4%, temperature is 80℃ and the reaction time is 2 h, the yield of 1,2-propanediol glycol is more than 99%. The catalyst can be repeatedly used for 5 times after simple separation but its activity changes greatly. A reaction mechanism is proposed.
2014, 31(9): 1076-1082
doi: 10.3724/SP.J.1095.2014.30592
Abstract:
The catalyst molybdenyl acetylacetonate(MoO2(acac)2) was prepared by reaction of ammonium molybdate and acetylacetone. The effects of solvents, temperature, oxidants, co-catalysts and the ratio of substrate on the dihydroxylation of styrene were investigated. Under the optimized condition, conversion, chemoselectivity and isolated yield of dihydroxylation reaction are 85.2%, 70.7% and 53.3%, respectively. The possible catalytic mechanism and improving directions of catalytic reaction were also discussed.
The catalyst molybdenyl acetylacetonate(MoO2(acac)2) was prepared by reaction of ammonium molybdate and acetylacetone. The effects of solvents, temperature, oxidants, co-catalysts and the ratio of substrate on the dihydroxylation of styrene were investigated. Under the optimized condition, conversion, chemoselectivity and isolated yield of dihydroxylation reaction are 85.2%, 70.7% and 53.3%, respectively. The possible catalytic mechanism and improving directions of catalytic reaction were also discussed.
2014, 31(9): 1083-1088
doi: 10.3724/SP.J.1095.2014.30623
Abstract:
The effect of surfactants on the viscosity of low concentration nano-SiO2 fluids was studied. Specifically, we studied the effect of different carbon chain lengths of cationic and nonionic surfactants for the nano-SiO2 fluids viscosity. The results show that the anionic surfactant of sodium dodecyl benzene sulfonate(SDBS) has a slight effect on the viscosity of nanofluids, it's relative viscosity value maintaining of about 1.23; while the cationic surfactants of tetradecyl trimethyl ammonium bromide(TTAB), cetyl trimethyl ammonium bromide(CTAB), octadecyl trimethyl ammonium bromide(OTAB), cetyl chloride pyridinium(CPC), nonionic surfactants of OP-8, OP-10, zwitterionic surfactants of DXS14, DXS18 have a greater influence on the viscosity, and it's maximum relative viscosity values can reach 3.42, 1.82 and 8.87, respectively, have a greater influence on the viscosity. At the same time, we found that the longer carbon chain in cationic surfactants, the greater the viscosity of nanofluids. The highest viscosity of nanofluids is obtained at the concentration of the surfactants near the critical micelle concentration value.
The effect of surfactants on the viscosity of low concentration nano-SiO2 fluids was studied. Specifically, we studied the effect of different carbon chain lengths of cationic and nonionic surfactants for the nano-SiO2 fluids viscosity. The results show that the anionic surfactant of sodium dodecyl benzene sulfonate(SDBS) has a slight effect on the viscosity of nanofluids, it's relative viscosity value maintaining of about 1.23; while the cationic surfactants of tetradecyl trimethyl ammonium bromide(TTAB), cetyl trimethyl ammonium bromide(CTAB), octadecyl trimethyl ammonium bromide(OTAB), cetyl chloride pyridinium(CPC), nonionic surfactants of OP-8, OP-10, zwitterionic surfactants of DXS14, DXS18 have a greater influence on the viscosity, and it's maximum relative viscosity values can reach 3.42, 1.82 and 8.87, respectively, have a greater influence on the viscosity. At the same time, we found that the longer carbon chain in cationic surfactants, the greater the viscosity of nanofluids. The highest viscosity of nanofluids is obtained at the concentration of the surfactants near the critical micelle concentration value.
2014, 31(9): 1089-1095
doi: 10.3724/SP.J.1095.2014.30543
Abstract:
Mesoporous silica and its copper oxide doped composite materials were synthesized by sol-gel and hydrothermal methods, using polyethylene glycol(PEG) as template. The target products were characterized by FTIR, HRTEM, XRD, BET and so on. The influences of reaction condition, such as copper oxide quality and reaction temperature, on porous structure were investigated in details. The samples used as adsorption material for adsorption of methylene blue(MB) in wastewater were studied. CuO/SiO2 mesoporous oxide composite has good absorbability of MB. The maximum removal rate reaches 97.17% for 10 mL of 4 mg/L MB solution at pH9 in the presence of 0.015 g sorbent. The process and mechanism of adsorption were also studied.
Mesoporous silica and its copper oxide doped composite materials were synthesized by sol-gel and hydrothermal methods, using polyethylene glycol(PEG) as template. The target products were characterized by FTIR, HRTEM, XRD, BET and so on. The influences of reaction condition, such as copper oxide quality and reaction temperature, on porous structure were investigated in details. The samples used as adsorption material for adsorption of methylene blue(MB) in wastewater were studied. CuO/SiO2 mesoporous oxide composite has good absorbability of MB. The maximum removal rate reaches 97.17% for 10 mL of 4 mg/L MB solution at pH9 in the presence of 0.015 g sorbent. The process and mechanism of adsorption were also studied.
2014, 31(9): 1096-1100
doi: 10.3724/SP.J.1095.2014.30559
Abstract:
The β-PbO2/TiO2 nanotubes(β-PbO2/TiO2NTs) electrode was prepared using the anodic oxidation method and pulsed electrochemical deposition(PED). The properties of β-PbO2/TiO2NTs electrode were characterized by scanning electron microscopy(SEM), X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS). The results indicate that β-PbO2 nanoparticles are successfully dispersed inside the TiO2 nanotubes. The degradation of phenol was carried out to test the electrocatalytic performance of the β-PbO2/TiO2 NTs electrode, which indicated that the β-PbO2/TiO2NTs electrode had high electrocatalytic activities and the COD removal rate of phenol reached up to 83%.
The β-PbO2/TiO2 nanotubes(β-PbO2/TiO2NTs) electrode was prepared using the anodic oxidation method and pulsed electrochemical deposition(PED). The properties of β-PbO2/TiO2NTs electrode were characterized by scanning electron microscopy(SEM), X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS). The results indicate that β-PbO2 nanoparticles are successfully dispersed inside the TiO2 nanotubes. The degradation of phenol was carried out to test the electrocatalytic performance of the β-PbO2/TiO2 NTs electrode, which indicated that the β-PbO2/TiO2NTs electrode had high electrocatalytic activities and the COD removal rate of phenol reached up to 83%.
2014, 31(9): 1101-1106
doi: 10.3724/SP.J.1095.2014.30609
Abstract:
Lead-silver anodes with different contents of silver were prepared on the surface of Al substrates by electrodeposition. The impact of the silver concentration on the electrochemical properties of electrodeposited lead-silver alloys was investigated by the anodic polarization curves, cyclic voltammetry, EIS, XRD and SEM. The results show that the increase of silver contents to the lead-silver anodes can enhance the corrosion resistance and decrease the impedance of the corrosion film and oxygen overpotential.
Lead-silver anodes with different contents of silver were prepared on the surface of Al substrates by electrodeposition. The impact of the silver concentration on the electrochemical properties of electrodeposited lead-silver alloys was investigated by the anodic polarization curves, cyclic voltammetry, EIS, XRD and SEM. The results show that the increase of silver contents to the lead-silver anodes can enhance the corrosion resistance and decrease the impedance of the corrosion film and oxygen overpotential.
2014, 31(9): 1107-1114
doi: 10.3724/SP.J.1095.2014.30577
Abstract:
Based on the Sudan Ⅰ-responsive shrinkage of the Sudan Ⅰ-imprinted gel film, a new imprinted gel-surface plasmon resonance(SPR) sensor for the detection of Sudan I was prepared. The Sudan I-imprinted soft gel film was synthesized on the surface of a SPR chip. The SPR sensor was characterized with an electrochemical method and swelling measurements. The method exhibits a linear response in the range of 8.0×10-10 to 1.0×10-8 mol/L(R2=0.9987) for the detection of Sudan Ⅰ. It was used to determine Sudan I in the paprika and salted products. The detection limits are 3.4×10-10 mol/L and 2.5×10-10 mol/L, respectively, and the relative standard deviations(RSD) are 1.38% and 2.10% for two paprika samples and 1.13% for the salted product. This SPR sensor shows high sensitivity and good reproducibility.
Based on the Sudan Ⅰ-responsive shrinkage of the Sudan Ⅰ-imprinted gel film, a new imprinted gel-surface plasmon resonance(SPR) sensor for the detection of Sudan I was prepared. The Sudan I-imprinted soft gel film was synthesized on the surface of a SPR chip. The SPR sensor was characterized with an electrochemical method and swelling measurements. The method exhibits a linear response in the range of 8.0×10-10 to 1.0×10-8 mol/L(R2=0.9987) for the detection of Sudan Ⅰ. It was used to determine Sudan I in the paprika and salted products. The detection limits are 3.4×10-10 mol/L and 2.5×10-10 mol/L, respectively, and the relative standard deviations(RSD) are 1.38% and 2.10% for two paprika samples and 1.13% for the salted product. This SPR sensor shows high sensitivity and good reproducibility.
