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2013 Volume 30 Issue 7
2013, 30(7): 733-739
doi: 10.3724/SP.J.1095.2013.20548
Abstract:
The adhesion is an important characteristic of the superhydrophobic surface. With the studies of the superhydrophobic surfaces,the responsive intelligent superhydrophobic surface has attracted great interest. Meanwhile,superhydrophobic surfaces with high adhesion which can be used as"mechanical hands"to snatch micro-liter liquids have drawn close attention. The impacts of surface morphology and surface chemical composition on the superhydrophobic surface adhesion were discussed in the article. The research progress on preparation of high adhesive superhydrophobic surfaces was summarized and future research directions of high adhesive superhydrophobic surfaces were discussed as well.
The adhesion is an important characteristic of the superhydrophobic surface. With the studies of the superhydrophobic surfaces,the responsive intelligent superhydrophobic surface has attracted great interest. Meanwhile,superhydrophobic surfaces with high adhesion which can be used as"mechanical hands"to snatch micro-liter liquids have drawn close attention. The impacts of surface morphology and surface chemical composition on the superhydrophobic surface adhesion were discussed in the article. The research progress on preparation of high adhesive superhydrophobic surfaces was summarized and future research directions of high adhesive superhydrophobic surfaces were discussed as well.
2013, 30(7): 740-744
doi: 10.3724/SP.J.1095.2013.20390
Abstract:
Three chiral functional monomers containing L-phenylalanine(L-Phe),L-tryptophane(L-Trp) and L-leucine(L-Leu) were designed and synthesized and used as precursors for preparing of chiral polymers. After esterification and condensations,AAc-L-Phe(AAc:acrylic acid),AAc-L-Trp and AAc-L-Leu were obtained and characterized by IR and 1H NMR. Then the subsequent copolymerization between AAc-L-Phe and N-isopropylacrylamide(NIPAam) was carried out in different mass ratio. The resulted polymers were identified by IR and differential scanning calorimetry(DSC) and proved that all of them are optical active and thermo-sensitive materials. The successful synthesis of chiral polymers suggested that these chiral monomers can be applied to the preparation of chiral polymers.
Three chiral functional monomers containing L-phenylalanine(L-Phe),L-tryptophane(L-Trp) and L-leucine(L-Leu) were designed and synthesized and used as precursors for preparing of chiral polymers. After esterification and condensations,AAc-L-Phe(AAc:acrylic acid),AAc-L-Trp and AAc-L-Leu were obtained and characterized by IR and 1H NMR. Then the subsequent copolymerization between AAc-L-Phe and N-isopropylacrylamide(NIPAam) was carried out in different mass ratio. The resulted polymers were identified by IR and differential scanning calorimetry(DSC) and proved that all of them are optical active and thermo-sensitive materials. The successful synthesis of chiral polymers suggested that these chiral monomers can be applied to the preparation of chiral polymers.
2013, 30(7): 745-749
doi: 10.3724/SP.J.1095.2013.20397
Abstract:
Novel poly(aryl ether quinoxaline) s(PEQs) were prepared via a new two-step procedure. First,poly(ether benzil)(PEB) was synthesized by the polycondensation of 4,4'-difluorobenzil and 4,4'isopropylidenediphenol. Then,PEQ-1 was synthesized through chemical modification of PEB by 1,2diaminobenzene. The mass average relative molecular mass of the PEQs could be adjusted easily as 7.492 × 104 and 1.486 × 105 by the addition of 1.0% and 1.3% mass fraction of 4,4'-oxydibenzene-1,2-diamine,respectively. The total yield of this two-step method is above 90%. The polymers were characterized by IR,NMR and other measurements. The method is simple and has a potential application value.
Novel poly(aryl ether quinoxaline) s(PEQs) were prepared via a new two-step procedure. First,poly(ether benzil)(PEB) was synthesized by the polycondensation of 4,4'-difluorobenzil and 4,4'isopropylidenediphenol. Then,PEQ-1 was synthesized through chemical modification of PEB by 1,2diaminobenzene. The mass average relative molecular mass of the PEQs could be adjusted easily as 7.492 × 104 and 1.486 × 105 by the addition of 1.0% and 1.3% mass fraction of 4,4'-oxydibenzene-1,2-diamine,respectively. The total yield of this two-step method is above 90%. The polymers were characterized by IR,NMR and other measurements. The method is simple and has a potential application value.
2013, 30(7): 750-756
doi: 10.3724/SP.J.1095.2013.20378
Abstract:
The surface composition and morphology of polyester film irradiated by air corona discharge was analyzed. The results show that the active groups are more inclined to migrate to the surface rather than transfer to the subsurface or substrate body in a hydrophilic environment. The amounts of C=O and OH introduced is increased with the increase of the intensity of corona irradiation. The XPS results show an increased content of CO,C=O and O-C=O,the binding energy of the new peak in the O1s spectrum is 532.49 eV,corresponding to the -O-O-peroxide bond on the surface. Atomic force microscopy studies show that the initial structure of polyester film is replaced by a globular morphology,and the change in the surface roughness is in the range of about 10 nm.
The surface composition and morphology of polyester film irradiated by air corona discharge was analyzed. The results show that the active groups are more inclined to migrate to the surface rather than transfer to the subsurface or substrate body in a hydrophilic environment. The amounts of C=O and OH introduced is increased with the increase of the intensity of corona irradiation. The XPS results show an increased content of CO,C=O and O-C=O,the binding energy of the new peak in the O1s spectrum is 532.49 eV,corresponding to the -O-O-peroxide bond on the surface. Atomic force microscopy studies show that the initial structure of polyester film is replaced by a globular morphology,and the change in the surface roughness is in the range of about 10 nm.
2013, 30(7): 757-763
doi: 10.3724/SP.J.1095.2013.20375
Abstract:
Two new electron donate-withdraw structured porphyrin dyes(WP-1 and WP-2) with bis(9,9dihexyl-9H-fluoren-2-yl) amine as an electron donor were designed and synthesized. The structures of the two dyes were characterized by proton nuclear magnetic resonance and high resolution mass spectra technologies. The UV-visible absorption spectra of the two dyes were tested. Dye-sensitized solar cells(DSSCs) using the two dyes gave high power conversion efficiencies of 4.01% and 7.07% under 100 × 10-3 W/cm2 illumination, respectively. The sealed DSSCs sensitized with dye WP-2 could keep more than 98% of the initial efficiency under natural sunlight irradiation for 500 h,which illustrated that the bis(9,9-dihexyl-9H-fluoren-2-yl) amine is suitable in the electron donate-withdraw structured porphyrin dyes as an electron donor. This not only enriched the types of electron donors,but also built the foundation for further research on bisfluorenamine derivative as electron donor in porphyrin dyes.
Two new electron donate-withdraw structured porphyrin dyes(WP-1 and WP-2) with bis(9,9dihexyl-9H-fluoren-2-yl) amine as an electron donor were designed and synthesized. The structures of the two dyes were characterized by proton nuclear magnetic resonance and high resolution mass spectra technologies. The UV-visible absorption spectra of the two dyes were tested. Dye-sensitized solar cells(DSSCs) using the two dyes gave high power conversion efficiencies of 4.01% and 7.07% under 100 × 10-3 W/cm2 illumination, respectively. The sealed DSSCs sensitized with dye WP-2 could keep more than 98% of the initial efficiency under natural sunlight irradiation for 500 h,which illustrated that the bis(9,9-dihexyl-9H-fluoren-2-yl) amine is suitable in the electron donate-withdraw structured porphyrin dyes as an electron donor. This not only enriched the types of electron donors,but also built the foundation for further research on bisfluorenamine derivative as electron donor in porphyrin dyes.
2013, 30(7): 764-768
doi: 10.3724/SP.J.1095.2013.20388
Abstract:
A new isophorone derivative(2-(3-(4-(bis(2-(2-nitrophenoxy) ethyl) amino) styryl)-5,5dimethylcyclohex-2-en-1-ylidene) malononitrile) of donor-π-acceptor(D-π-A) type which yield was 80.7% was synthesized by Knoevenagel reaction and characterized by FT-IR and 1H NMR. Its UV-Vis absorption spectrum and fluorescent properties,thermal stability and electrochemical properties were preliminarily investigated. The results showed that the target compound had good fluorescence properties and thermal stability and demonstrated instructive explorations for pursuing new luminescent materials.
A new isophorone derivative(2-(3-(4-(bis(2-(2-nitrophenoxy) ethyl) amino) styryl)-5,5dimethylcyclohex-2-en-1-ylidene) malononitrile) of donor-π-acceptor(D-π-A) type which yield was 80.7% was synthesized by Knoevenagel reaction and characterized by FT-IR and 1H NMR. Its UV-Vis absorption spectrum and fluorescent properties,thermal stability and electrochemical properties were preliminarily investigated. The results showed that the target compound had good fluorescence properties and thermal stability and demonstrated instructive explorations for pursuing new luminescent materials.
2013, 30(7): 769-775
doi: 10.3724/SP.J.1095.2013.20516
Abstract:
A series of piperidine derivatives was synthesized using 1,5-diols as starting materials. The procedures include the sulfonylation of 1,5-diols to active 1,5-disulfonates followed by the cyclization of the 1,5-disulfonates with primary amines. The effects of reaction temperature,time on the annulation were further explored. It was disclosed that when the solvent was primary amine,reaction temperature was 90~100℃,and reaction time was 18 h,the yields of 74%~94% for annulations could be reached.
A series of piperidine derivatives was synthesized using 1,5-diols as starting materials. The procedures include the sulfonylation of 1,5-diols to active 1,5-disulfonates followed by the cyclization of the 1,5-disulfonates with primary amines. The effects of reaction temperature,time on the annulation were further explored. It was disclosed that when the solvent was primary amine,reaction temperature was 90~100℃,and reaction time was 18 h,the yields of 74%~94% for annulations could be reached.
2013, 30(7): 776-781
doi: 10.3724/SP.J.1095.2013.20411
Abstract:
A yellow-fluorescent hydrotalcite-like(HTlc) composite,Zn-(HQ-4-biPh)-HTlc,was prepared by a one-pot synthesis. In this composite,the magnesium(Ⅱ) was partially replaced by zinc(Ⅱ) in the hydrotalcite-like layers and 2-biphenyl-4'-yl-8-quinolinolato was dispersed into the anions among the interlayer region to coordinate the zinc(Ⅱ) ion through its oxygen and nitrogen atoms. The structure,morphology,and optical properties of the composite were characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM),FT-IR spectroscopy,thermogravimetry(TG) and photoluminescence(PL). Compared with Zn[2-(p-biph)-8-Q-O]2,the resultant composite Zn-(HQ-4-biPh)-HTlc exhibits much stronger fluorescence and higher thermal stability,although the contents of metals and ligands were decreased greatly. Thus,Zn-(HQ-4-biPh)-HTlc is a promising yellow-fluorescent material for applications in the photoelectronic area.
A yellow-fluorescent hydrotalcite-like(HTlc) composite,Zn-(HQ-4-biPh)-HTlc,was prepared by a one-pot synthesis. In this composite,the magnesium(Ⅱ) was partially replaced by zinc(Ⅱ) in the hydrotalcite-like layers and 2-biphenyl-4'-yl-8-quinolinolato was dispersed into the anions among the interlayer region to coordinate the zinc(Ⅱ) ion through its oxygen and nitrogen atoms. The structure,morphology,and optical properties of the composite were characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM),FT-IR spectroscopy,thermogravimetry(TG) and photoluminescence(PL). Compared with Zn[2-(p-biph)-8-Q-O]2,the resultant composite Zn-(HQ-4-biPh)-HTlc exhibits much stronger fluorescence and higher thermal stability,although the contents of metals and ligands were decreased greatly. Thus,Zn-(HQ-4-biPh)-HTlc is a promising yellow-fluorescent material for applications in the photoelectronic area.
2013, 30(7): 782-788
doi: 10.3724/SP.J.1095.2013.20401
Abstract:
N-(Ethoxycarbonyl acyl)-N'-(2,4-dinitrophenyl amino) thiourea was synthesized using 2,4dinitrophenylhydrazine,potassium thiocyanate and ethyl chloroformate as precursors in ethyl acetate in the presence of Macrogol-400 catalyst. The structure was characterized by elemental analysis and FI-IR. Single crystal of the title compound was obtained by slowly evaporating solvents at the room temperature. The crystal structure was determined with single crystal X-ray diffractometer. Crystal data are:monoclinic,P2(1)/c space group,a=4.1919(2) nm,b=12.295(6) nm,c=23.828(11) nm,α=γ=90.00°,β=92.467(10)°,V=1439.7(12),Dc=1.519 g/cm3,μ=0.263 cm-1,F(000)=680,Z=4,R1=0.1121,wR2=0.2540. The thermal behavior of the title compound was studied under a non-isothermal condition by DSC method. The specific heat capacity of the title compound was determined with continuous Cp mode of mircocalorimeter. The structure analysis and thermodynamic properties proved that the title compound has good stability,which is good for transportation and storage.
N-(Ethoxycarbonyl acyl)-N'-(2,4-dinitrophenyl amino) thiourea was synthesized using 2,4dinitrophenylhydrazine,potassium thiocyanate and ethyl chloroformate as precursors in ethyl acetate in the presence of Macrogol-400 catalyst. The structure was characterized by elemental analysis and FI-IR. Single crystal of the title compound was obtained by slowly evaporating solvents at the room temperature. The crystal structure was determined with single crystal X-ray diffractometer. Crystal data are:monoclinic,P2(1)/c space group,a=4.1919(2) nm,b=12.295(6) nm,c=23.828(11) nm,α=γ=90.00°,β=92.467(10)°,V=1439.7(12),Dc=1.519 g/cm3,μ=0.263 cm-1,F(000)=680,Z=4,R1=0.1121,wR2=0.2540. The thermal behavior of the title compound was studied under a non-isothermal condition by DSC method. The specific heat capacity of the title compound was determined with continuous Cp mode of mircocalorimeter. The structure analysis and thermodynamic properties proved that the title compound has good stability,which is good for transportation and storage.
2013, 30(7): 789-793
doi: 10.3724/SP.J.1095.2013.20377
Abstract:
A new tungstosilicates polyoxometalate(C2H10N2)3(SiW2ⅤW10ⅥO40)·3H2O was prepared under hydrothermal conditions,and characterized by elemental analysis,IR and single crystal X-ray diffraction analysis. The title compound crystallized in a triclinic system,P-1 space group,a=1.3193(3) nm,b=1.3198(3) nm,c=1.3193(3) nm,α=76.05(3)°,β=76.13(3)°,γ=76.05(3)°,V=2.1231(7) nm3,Z=1,R1=0.0518,wR2=0.1355. The title compound is comprised of silica tungsten Keggin polyoxoanion,three ethylenediamine and water molecules. The hydrogen bonds among polyoxoanion,ethylenediamine and water molecules are responsible for the formation of its extended three dimensional structure. Magnetic measurement indicates that there exists antiferromagnetic interaction in the molecule.
A new tungstosilicates polyoxometalate(C2H10N2)3(SiW2ⅤW10ⅥO40)·3H2O was prepared under hydrothermal conditions,and characterized by elemental analysis,IR and single crystal X-ray diffraction analysis. The title compound crystallized in a triclinic system,P-1 space group,a=1.3193(3) nm,b=1.3198(3) nm,c=1.3193(3) nm,α=76.05(3)°,β=76.13(3)°,γ=76.05(3)°,V=2.1231(7) nm3,Z=1,R1=0.0518,wR2=0.1355. The title compound is comprised of silica tungsten Keggin polyoxoanion,three ethylenediamine and water molecules. The hydrogen bonds among polyoxoanion,ethylenediamine and water molecules are responsible for the formation of its extended three dimensional structure. Magnetic measurement indicates that there exists antiferromagnetic interaction in the molecule.
2013, 30(7): 794-800
doi: 10.3724/SP.J.1095.2013.20354
Abstract:
Silica (SiO2) nanoparticle coatings were fabricated using tetraethoxysilane(TEOS),cetyltrimethylammonium bromide(CTAB),hydrochloric acid(HCl),ethanol and water via the sol-gel process followed by dynamic hardening at 700℃ for 200 s. Effects of the CTAB concentration,withdrawing speed,retaining time and the number of withdrawing were investigated on the transmittance of fabricated coatings. It was found that the fabricated coating achieved the maximum transmittance of 95.9% when a CTAB mass percentage of 2.5%,a withdrawing speed of 100 mm/min,a retaining time of 60 s and one withdrawing were used. The coating was superhydrophilic,and could endure a 6H pencil hardness test. It was also shown that the CTAB added in the SiO2 sol might interact with partially hydrolyzed species of TEOS,improving the nanostructure of SiO2 sol formed by acid-catalysis,and eventually enhanced the transmittance and hydrophilicity of fabricated coatings.
Silica (SiO2) nanoparticle coatings were fabricated using tetraethoxysilane(TEOS),cetyltrimethylammonium bromide(CTAB),hydrochloric acid(HCl),ethanol and water via the sol-gel process followed by dynamic hardening at 700℃ for 200 s. Effects of the CTAB concentration,withdrawing speed,retaining time and the number of withdrawing were investigated on the transmittance of fabricated coatings. It was found that the fabricated coating achieved the maximum transmittance of 95.9% when a CTAB mass percentage of 2.5%,a withdrawing speed of 100 mm/min,a retaining time of 60 s and one withdrawing were used. The coating was superhydrophilic,and could endure a 6H pencil hardness test. It was also shown that the CTAB added in the SiO2 sol might interact with partially hydrolyzed species of TEOS,improving the nanostructure of SiO2 sol formed by acid-catalysis,and eventually enhanced the transmittance and hydrophilicity of fabricated coatings.
2013, 30(7): 801-807
doi: 10.3724/SP.J.1095.2013.20393
Abstract:
A new synthetic approach based on the co-precipitation method was explored to synthesize regularly hexagonal Mg-Al-NO3-LDHs nanoparticles by taking the advantages of the conventional urea hydrolysis method. The effects of precipitator,solvent,reaction time and the dropping speed of precipitator on the crystallinity and morphologies of LDHs were systematically studied.Nearly monodispersed and regularly hexagonal morphology of LDHs with high crystallinity and particle size in the range of 100~250 nm could be obtained using NH4OH as precipitator and a mixture of alcohol and water as solvent. The addition of alcohol might slow down the ionization rate of NH4OH into OH- and benefit the reduction of the supersaturation degree. In addition,the alcohol could be absorbed on the surface of LDHs particles and the hydroxyl groups play a steric repulsion effect,which prevent the aggregation of the particles. Our results also show that an incomplete particle growth occurred at short reaction time(1 h) will lead to the formation of irregular and hexagonal particles,while the aggregation of particles tends to take place when the reactions are prolonged(4 h). Furthermore,the effect of dropping speed of precipitators was also investigated. A low dropping speed(0.025 mL/s) of precipitator favors the formation of regularly hexagonal particles with good monodispersity,and the particle size increases with the decrement of dropping speed.
A new synthetic approach based on the co-precipitation method was explored to synthesize regularly hexagonal Mg-Al-NO3-LDHs nanoparticles by taking the advantages of the conventional urea hydrolysis method. The effects of precipitator,solvent,reaction time and the dropping speed of precipitator on the crystallinity and morphologies of LDHs were systematically studied.Nearly monodispersed and regularly hexagonal morphology of LDHs with high crystallinity and particle size in the range of 100~250 nm could be obtained using NH4OH as precipitator and a mixture of alcohol and water as solvent. The addition of alcohol might slow down the ionization rate of NH4OH into OH- and benefit the reduction of the supersaturation degree. In addition,the alcohol could be absorbed on the surface of LDHs particles and the hydroxyl groups play a steric repulsion effect,which prevent the aggregation of the particles. Our results also show that an incomplete particle growth occurred at short reaction time(1 h) will lead to the formation of irregular and hexagonal particles,while the aggregation of particles tends to take place when the reactions are prolonged(4 h). Furthermore,the effect of dropping speed of precipitators was also investigated. A low dropping speed(0.025 mL/s) of precipitator favors the formation of regularly hexagonal particles with good monodispersity,and the particle size increases with the decrement of dropping speed.
2013, 30(7): 808-814
doi: 10.3724/SP.J.1095.2013.30049
Abstract:
Composite anodes made of activated carbon powder/nano Fe3O4/stainless steel mesh(SSM) were fabricated with a mass percentage of 0,2.5%,5.0% and 7.5% of nano Fe3O4,and named as AcM,AcFeM1,AcFeM2 and AcFeM3,respectively. The SSM was used as both matrix and current collector. Effect of the nano Fe3O4 content on the performance of SSM was investigated in single-chamber membrane-less air cathode microbial fuel cell(MFC). The electrochemical behavior of each anode was studied by Tafel tests and charge-discharge experiments. The results indicate that the maximum power density and net capacitance charge increase from 664 mW/m2 and 293.9 C(AcM) to 731 mW/m2 and 300.4 C(AcFeM1),809 mW/m2 and 388.5 C(AcFeM2),where nano Fe3O4 content is increased from 0 to 2.5% and 5.0%,respectively. With further increase in content of nano Fe3O4 to 7.5%,the performance of MFC inversely decreases. Thus,when the content of nano Fe3O4 is 5.0%,the best performance is reached for MFC. The electrochemical measurement also displays that the kinetic activity is the highest for AcFem2 anode with nano Fe3O4 content of 5.0%.
Composite anodes made of activated carbon powder/nano Fe3O4/stainless steel mesh(SSM) were fabricated with a mass percentage of 0,2.5%,5.0% and 7.5% of nano Fe3O4,and named as AcM,AcFeM1,AcFeM2 and AcFeM3,respectively. The SSM was used as both matrix and current collector. Effect of the nano Fe3O4 content on the performance of SSM was investigated in single-chamber membrane-less air cathode microbial fuel cell(MFC). The electrochemical behavior of each anode was studied by Tafel tests and charge-discharge experiments. The results indicate that the maximum power density and net capacitance charge increase from 664 mW/m2 and 293.9 C(AcM) to 731 mW/m2 and 300.4 C(AcFeM1),809 mW/m2 and 388.5 C(AcFeM2),where nano Fe3O4 content is increased from 0 to 2.5% and 5.0%,respectively. With further increase in content of nano Fe3O4 to 7.5%,the performance of MFC inversely decreases. Thus,when the content of nano Fe3O4 is 5.0%,the best performance is reached for MFC. The electrochemical measurement also displays that the kinetic activity is the highest for AcFem2 anode with nano Fe3O4 content of 5.0%.
2013, 30(7): 815-820
doi: 10.3724/SP.J.1095.2013.20412
Abstract:
Cross-linked angiotensin converting enzyme aggregates(ACE-CLEAs) were prepared and their characteristics were compared with that of free ACE including optimal temperature and pH,Km,vmax,thermal and pH stabilities. Based on the relative activity of immobilized enzyme,the optimal preparation conditions should be as follows:precipitating the enzyme with 80% saturated ammonium sulfate for 0.5 h,and then cross-linking it with 0.02%(mass fraction) glutaraldehyde for 1 h. According to the comparison for enzymology property,ACE-CLEAs had better thermal and pH stabilities than free ACE,and the Km of ACE-CLEAs was close to that of free ACE,suggesting that ACE-CLEAs had an almost equal affinity to enzyme as the free ACE.
Cross-linked angiotensin converting enzyme aggregates(ACE-CLEAs) were prepared and their characteristics were compared with that of free ACE including optimal temperature and pH,Km,vmax,thermal and pH stabilities. Based on the relative activity of immobilized enzyme,the optimal preparation conditions should be as follows:precipitating the enzyme with 80% saturated ammonium sulfate for 0.5 h,and then cross-linking it with 0.02%(mass fraction) glutaraldehyde for 1 h. According to the comparison for enzymology property,ACE-CLEAs had better thermal and pH stabilities than free ACE,and the Km of ACE-CLEAs was close to that of free ACE,suggesting that ACE-CLEAs had an almost equal affinity to enzyme as the free ACE.
2013, 30(7): 821-825
doi: 10.3724/SP.J.1095.2013.20407
Abstract:
A new method for the determination of Cd in the water with a wireless magnetoelastic immunosensor was introduced. In the method,the specific binding of antigen with the antibody made precipitation adhere to the surface of the immunosensor and resulted in a decrease in the resonance frequency of the magnetoelastic foil. The shift of the resonance frequency was related to the concentration of Cd. The influence of some factors such as polyethylene imine dosage,glutaraldehyde dosage and reaction time on the determination was discussed. At the optimized conditions,the linear range for the determination of Cd was in the range of 0.90~10.0 μg/L,with the detection limit of 0.42 μg/L. The proposed method was applied successfully to the determination of Cd in water samples with the recoveries of 96.5%~103.6%. The determination results are basically consistent with that of dithizone colorimetric method.
A new method for the determination of Cd in the water with a wireless magnetoelastic immunosensor was introduced. In the method,the specific binding of antigen with the antibody made precipitation adhere to the surface of the immunosensor and resulted in a decrease in the resonance frequency of the magnetoelastic foil. The shift of the resonance frequency was related to the concentration of Cd. The influence of some factors such as polyethylene imine dosage,glutaraldehyde dosage and reaction time on the determination was discussed. At the optimized conditions,the linear range for the determination of Cd was in the range of 0.90~10.0 μg/L,with the detection limit of 0.42 μg/L. The proposed method was applied successfully to the determination of Cd in water samples with the recoveries of 96.5%~103.6%. The determination results are basically consistent with that of dithizone colorimetric method.
2013, 30(7): 826-833
doi: 10.3724/SP.J.1095.2013.20437
Abstract:
A kind of novel modified cotton was prepared by immersing raw cotton into modified silica hydrosol. The modified silica hydrosol was prepared via slo-gel reaction and subsequent hydrophobization with methoxytrimethylsilane. The prepared modified cotton was characterized by water contact angle measurement(CA) and scanning electron microscopy(SEM),respectively. Contact angles of redistilled water,acidic solution,and alkaline solution are all over 150° on the as-prepared modified cotton,which indicates the superhydrophobicity and acid and alkali resistance of the modified cotton. The modified cotton showed 8.3 g/g and 4.0 g/g of saturated absorption capacity for diesel oil at the first time used and the sequent five times used,respectively. The contact angles of the recycled modified cotton kept above 150°.The water absorption capacity of the modified cotton is only 1/45 times of the raw cotton in removing diesel oil from oil-water mixture,suggesting the high selectivity of the modified cotton to diesel oil. The modified cotton can be recovered easily by extruding the absorbed diesel oil and then can be reused. This study would provide a fast,simple,cheap,and environment friendly approach to the oil recovery from oil-water mixture.
A kind of novel modified cotton was prepared by immersing raw cotton into modified silica hydrosol. The modified silica hydrosol was prepared via slo-gel reaction and subsequent hydrophobization with methoxytrimethylsilane. The prepared modified cotton was characterized by water contact angle measurement(CA) and scanning electron microscopy(SEM),respectively. Contact angles of redistilled water,acidic solution,and alkaline solution are all over 150° on the as-prepared modified cotton,which indicates the superhydrophobicity and acid and alkali resistance of the modified cotton. The modified cotton showed 8.3 g/g and 4.0 g/g of saturated absorption capacity for diesel oil at the first time used and the sequent five times used,respectively. The contact angles of the recycled modified cotton kept above 150°.The water absorption capacity of the modified cotton is only 1/45 times of the raw cotton in removing diesel oil from oil-water mixture,suggesting the high selectivity of the modified cotton to diesel oil. The modified cotton can be recovered easily by extruding the absorbed diesel oil and then can be reused. This study would provide a fast,simple,cheap,and environment friendly approach to the oil recovery from oil-water mixture.
2013, 30(7): 834-839
doi: 10.3724/SP.J.1095.2013.20336
Abstract:
A molecularly imprinted polymer(MIP) of malachite green(MG) was prepared through bulk polymerization. Polymerization conditions,such as the kinds and the dosages of functional monomers,the dosages of cross linker,the concentrations of the template,as well as the polymerization time,were optimized. Static equilibrium binding method was employed to investigate the absorption ability of polymers to MG. The result showed that when using MAA as monomer and the molar ratio of MG,MAA,EGDMA was 1:4:20,the largest amount of absorption was achieved and the imprinting factor(α=QMIP/QNIP) could be as large as 3.6,indicating that the MIP prepared in this work had the excellent ability of recognition and enrichment for MG.
A molecularly imprinted polymer(MIP) of malachite green(MG) was prepared through bulk polymerization. Polymerization conditions,such as the kinds and the dosages of functional monomers,the dosages of cross linker,the concentrations of the template,as well as the polymerization time,were optimized. Static equilibrium binding method was employed to investigate the absorption ability of polymers to MG. The result showed that when using MAA as monomer and the molar ratio of MG,MAA,EGDMA was 1:4:20,the largest amount of absorption was achieved and the imprinting factor(α=QMIP/QNIP) could be as large as 3.6,indicating that the MIP prepared in this work had the excellent ability of recognition and enrichment for MG.
2013, 30(7): 840-845
doi: 10.3724/SP.J.1095.2013.20362
Abstract:
The interaction between ionic liquid surfactant,1-dodecyl-3-methylimidazolium bromine(C12mimBr) and anionic dye,methyl orange(MO) was studied using conductometric and surface tension methods in aqueous solutions. The equilibrium constants of the interaction between C12mimBr and MO were derived from the molar conductivities of C12mimBr,MO and mixtures of C12mimBr and MO. At the temperatures of 288.1,298.1 and 308.1 K,the equilibrium constants are 4.89 × 105,4.88 × 104 and 5.76 × 103L/mol,respectively. Thus,the binding process is an enthalpy driving and spontaneous exothermic reaction.Furthermore,the critical micelle concentrations(cmc) of the solutions of C12mimBr and the mixtures of C12mimBr and MO were measured to be 9.1 × 10-3 and 7.3 × 10-5mol/L,respectively. Thus the surface activity of C12mimBr in aqueous solution can be greatly enhanced by MO.
The interaction between ionic liquid surfactant,1-dodecyl-3-methylimidazolium bromine(C12mimBr) and anionic dye,methyl orange(MO) was studied using conductometric and surface tension methods in aqueous solutions. The equilibrium constants of the interaction between C12mimBr and MO were derived from the molar conductivities of C12mimBr,MO and mixtures of C12mimBr and MO. At the temperatures of 288.1,298.1 and 308.1 K,the equilibrium constants are 4.89 × 105,4.88 × 104 and 5.76 × 103L/mol,respectively. Thus,the binding process is an enthalpy driving and spontaneous exothermic reaction.Furthermore,the critical micelle concentrations(cmc) of the solutions of C12mimBr and the mixtures of C12mimBr and MO were measured to be 9.1 × 10-3 and 7.3 × 10-5mol/L,respectively. Thus the surface activity of C12mimBr in aqueous solution can be greatly enhanced by MO.
2013, 30(7): 846-851
doi: 10.3724/SP.J.1095.2013.20369
Abstract:
Near-infrared(NIR) spectroscopy technique was used to study the states of water in reversed micelle formed from gemini quaternary ammonium surfactants C12-S2-C12·2Br in chloroform. The NIR spectroscopy of water could be categorized into three subbands corresponding to different water states. These water states were calculated into three kinds with molecular number of each surfactant molecular corresponding to dispersed solvent water ns,bulk like water nf and bound water nb. By mixing ionic surfactants dodecyltrimethylammonium bromide(DTAB) or dodecyltriethlyammonium bromide(DTEB) to the C12-S2-C12·2Br/chloroform system,it showed that with the increase of the molar fraction of added agent αA,ns and nb were increased,while nf was reduced;when nonionic surfactant octyl polyethylene glycol phenyl ethers(OP-10) was added,it showed that ns was reduced,while nb and nf were increased as αA was increased. It was found that the water solubilizing ability and states were influenced by the size of head group,electric charge and hydrophilicity of the surfactants.
Near-infrared(NIR) spectroscopy technique was used to study the states of water in reversed micelle formed from gemini quaternary ammonium surfactants C12-S2-C12·2Br in chloroform. The NIR spectroscopy of water could be categorized into three subbands corresponding to different water states. These water states were calculated into three kinds with molecular number of each surfactant molecular corresponding to dispersed solvent water ns,bulk like water nf and bound water nb. By mixing ionic surfactants dodecyltrimethylammonium bromide(DTAB) or dodecyltriethlyammonium bromide(DTEB) to the C12-S2-C12·2Br/chloroform system,it showed that with the increase of the molar fraction of added agent αA,ns and nb were increased,while nf was reduced;when nonionic surfactant octyl polyethylene glycol phenyl ethers(OP-10) was added,it showed that ns was reduced,while nb and nf were increased as αA was increased. It was found that the water solubilizing ability and states were influenced by the size of head group,electric charge and hydrophilicity of the surfactants.
2013, 30(7): 852-854
doi: 10.3724/SP.J.1095.2013.20527
Abstract:
With the presence of nickel(Ⅱ) chloride as metal complex catalyst and N-heterocyclic carbene as organic catalyst effective one pot synthesis of allylated α-hydroxy carbonyl compound in 78% yield was developed using benzaldehyde and cinnamyl acetate as precursors in potassium carbonate THF solution. The involved reactions during the continuous reaction are benzoin condensation and allylic nucleophilic substitution.
With the presence of nickel(Ⅱ) chloride as metal complex catalyst and N-heterocyclic carbene as organic catalyst effective one pot synthesis of allylated α-hydroxy carbonyl compound in 78% yield was developed using benzaldehyde and cinnamyl acetate as precursors in potassium carbonate THF solution. The involved reactions during the continuous reaction are benzoin condensation and allylic nucleophilic substitution.
