In this work the Bamberger rearrangement reaction for p-aminophenol(PAP)prepared by electrochemical reduction of nitrobenzene was investigated.Cyclic voltammetry was used to investigate the catalytic effect of several catalysts,and the peak current of the reduction of nitrobenzene obviously increased when kieselguhr,sulphated zirconia and beta zeolite were added,respectively.The rearrangement of phenylhydroxylamine(PHA)was studied in the presence of catalysts.It has been found that the best experimental conditions in acid solution were:the concentration of H+was 0.5 mol·
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Catalytic behavior of Au-Pt hollow nanospheres towards electro-oxidation of methanol
- ZHONG Yan,WEN Feipeng,XU Jinlong,CHENG Meiqin,DENG Xiaocong,YAN Liangliang,ZHANG Xiantu,ZHONG Qiling,
2010, 61(S1):
24-28.
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Abstract
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918 )
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Au-Pt hollow nanospheres were synthesized by using amorphous selenium spherical colloids as templates.Surface morphology,structure,composition of samples were characterized by SEM,HR-TEM,UV-Vis,XRD and electrochemical cyclic voltammetry.Conventional electrochemical method was used to study electro-catalytic oxidation to methanol of(Au-Pt)HN/GC in alkaline solution.The influence of catalytic activity was also investigated with different ratios of gold to platinum.It indicated that the order of catalytic activity with different ratios of gold to platinum is 20∶1>50∶1>100∶1>10∶1>5∶
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Electrocatalytic oxidation of glucose at Ti/nanoTiO2-ZrO2 electrode
- FANG Wenyan, WANG Fengwu, XU Mai, ZHU Chuangao, WEI Yijun, ZHU Qiyong
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2010, 61(S1):
29-32.
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Abstract
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847 )
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316
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The precursor Ti(OCH2CH3)(4-y)(acac)y was synthesized by electrolysis of titanium and in absolute ethanol and acetyl-acetone solution.0.5 g ZrCl4 was added into the above.Nano-crystalline TiO2-ZrO2 powder was prepared by directs sol-gel method from the precursor and then calcined for 2 h at 400℃. XRD and TEM results showed that the nano-TiO2-ZrO2 of 30—40 nm was obtained.The highly active Ti/nanoTiO2-ZrO2 modified electrode was prepared by using daubing and drying.The results of cyclic voltammetry showed that Ti/nanoTiO2-ZrO2 modified electrode as anode exhibited high electrocatalytic activity for electro-oxidation of glucose.
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Influence of proline on electrochemical oxidation reaction of adrenaline
- ZHANG Yan,CAO Kewei,YU Zhangyu
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2010, 61(S1):
33-37.
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Abstract
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1192 )
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268
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The influence of L-proline on the electrochemical oxidation of adrenaline was investigated by cyclic voltammetry and electrochemical impedance spectroscopy at a platinum electrode.Simultaneously the structure of complexes of protonated adrenaline with proline is optimized by means of the density function theory method at B3LYP/6-31++G(2 d)level.The experimental results show that proline has stabilization on adrenaline and to some extent inhibits the oxidation of adrenaline.Cyclic voltammetry display that oxidation peak potential shift positively,the reduction peak potential to shift negatively,peak currents decreased.Nyquist plot showed that the electrochemical reaction resistance is accreted.The calculation results indicated that stronger hydrogen bond complexes were formed by the interaction between adrenaline and proline.
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Preparation of nano-Cu electrode and application in electrocatalytic reduction of CO2
- CHEN Qiong,WANG Huan,LI Zhuo,LI Miaomiao,WU Laxia,LU Jiaxing
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2010, 61(S1):
38-42.
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Abstract
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1124 )
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429
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Cu electrode is very efficient for electroreduction of CO2,while electrodeposited nano-Cu is much better.With the aim of optimizing the electrochemical catalytic behavior of nano-Cu electrode material toward electrochemical reduction of CO2,the electrodeposition conditions,such as deposition time,H2SO4 concentration,deposition potential and Cu2+ concentration,have been investigated.SEM was used to characterize the morphology of nano-Cu.Finally,the nano-Cu was used to the electrochemical synthesis of propylene carbonate from CO2 and propylene oxide.The investigation indicates that the nano-Cu has greater catalytic ability toward the electrochemical reduction of CO2 and higher yield of propylene carbonate can accomplish by using nano-Cu electrode.
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Separation of system of glyoxylic acid by electrodialysis
- SU Rui,ZHANG Xinsheng,CHEN Chi
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2010, 61(S1):
43-50.
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Abstract
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910 )
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364
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This paper attempted to separate glyoxylic acid from the system of the electro-oxidation of glyoxal by electrodialysis.The influences of current density,flow velocity,temperature and nature of anion membrane on electrodialysis were studied.The results showed that flow rate at 4.21 cm·s-1,temperature at 30℃,AHT as anion membrane and the process with current density 628.7 A·m-2 at early stage and 456.6 A·m-2at later stage benefitted the separation of the system of glyoxylic acid.
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Effect of QSAR model parameters on current efficiency in electroreduction of oxalic acid
- JIN Ling,ZHANG Xinsheng
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2010, 61(S1):
63-67.
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Abstract
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909 )
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337
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The relationship between current efficiency of electroreduction of oxalic acid and each parameter of quantitative structure-activity relationship(QSAR)model including concentration of oxalic acid,pH,temperature,current density and topological index of additive molecule structure,has been studied through experiments.The results prove that the model has the capability to predict the effect of each parameter on current efficiency.Additionally,pH value of solution is controlled by oxalic acid,current efficiency will increasing with increasing current density,Am2-index and Am3-index as well as lowering temperature andAm1index.
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Application of dimensionally stable anodes in electro-synthesis of adiponitrile
- FENG Baicheng,GUAN Xianwen,WANG Guangxin
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2010, 61(S1):
68-71.
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Abstract
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1047 )
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709
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Adiponitrile was produced through the electroreduced coupling of acrylonitrile in a cell employing dimensionally stable anode(DSA)as anode and Cd or Pb as cathode without diaphragm.Under the optimized conditions,electroredutive coupling of acrylonitrile for 48 h,the yield of adiponitrile and total efficiency are up to 85.7% and 86.6% in the DSA-Cd cell; 80.1% and 77.7% in the DSA-Pb cell.Since DSA is possessed of excellent anti-corrosion,employing DSA as anode for electro-synthesis of adiponitrile is one of the favorable selections.
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Preparation and corrosion resistance of silane-based composite film on surface of cold rolled steel
- NIU Yunfeng,LU Daorong
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2010, 61(S1):
72-76.
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Abstract
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949 )
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618
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The γ-glycidoxy-propyl tri-methoxy silane-based composite film with cerium and chromium ions was prepared on the surface of cold rolled steel(CRS) using the immersion technique in this paper.The corrosion resistance of the composite silane film was studied in 3.50% NaCl solution by electrochemistry method.The change in the shape of the composite silane film before and after corrosion testing was researched by employing the scanning electron microscope.The result indicates that the silane solution with cerium and chromium ions, which reacts at 50℃ with the pH value 4 for 8h, has the best hydrolyzation effect.Furthermore, the corrosion current density of the CRS with composite silane films decreases to 1.584×10-7 A·cm-2 in 3.50% NaCl solution,and a positive shift for the corrosion potential can be observed.Test result indicates that the shape of the composite silane film with cerium and chromium ions on the CRS remains nearly unchanged after corrosion, and the corrosion resistance is apparently superior to the CRS with pure silane film.
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Preparation of electronic tetrabutylammonium hydroxide by ion-exchange membrane electrolysis
- YANG Jiao,ZHANG Xinsheng
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2010, 61(S1):
77-81.
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Abstract
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1303 )
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672
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The electronic tetrabutylammonium hydroxide (TBAH) using tetrabutyl amonium bromide(TBAB) as raw material was prepared.At first, the elimination of the metal ions in tetrabutyl amonium bromide (TBAB) solution by the cation exchange resins was systematically studied.The WU-64 cation exchange resin was the most efficient for the elimination of metal ions in tetrabutylamonium bromide solution among the four investigated resins.Then, the preparation of tetrabutylammonium hydroxide was carried out in an electrolyser with tri-chambers and sec-membranes, the current efficiency reached the maximum when the current density was 1000 A·m-2 and concentration of the raw material was 0.7 mol·L-1. Finally, the purification of the product was conducted in a divided cell separated by cation exchange membrane.The contents of Br- and Cl- residued in 15%(mass) TBAH solution after purification were 0.138 mg·kg-1 and 0.784 mg·kg-1 respectively.The results of the experiment can be references for microelectronics industry.
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Effects of sodium dodecylbenzenesulfonate on electro-oxidation of 2-methylpyridine
- WANG Haitao,ZHANG Yumin, GAO Shujuan,JIANG Xueying, ZHU Zhixin1, ZHANG Hengbin,LI Kechang,GENG Aifang
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2010, 61(S1):
82-85.
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Abstract
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903 )
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508
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The electro-oxidation of 2-methylpyridine(2-picoline) was investigated at a PbO2 electrode in the presence of sodium dodecylbenzenesulfonate(SDBS) in water/acetone solvents by cyclic voltammetry and controlled-potential coulometry.It was found that the selectivity and the current efficiency of the electro-oxidation from 2-picoline to 2-pyridinecarboxylic acid were obviously higher than that in aqueous and water/acetone mixed solvents when SDBS was added in acetone /water mixed solvents.The results indicate that under the optimal conditions, the reaction can obtain a selectivity of 81.98% and a current efficiency of 59.32%.The present method provides a simple method for electro-oxidation of 2-methylpyridine.
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Additives structure in electroreduction of oxalic acid
- JIN Ling, ZHANG Xinsheng
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2010, 61(S1):
86-90.
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Abstract
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1245 )
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368
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As the background of the preparation of glyoxylic acid by the electroreduction of oxalic acid on Pb electrodes, the effects of additives structure on electrode reaction have been studied.The results show that the cation of the additives has the most influence on current efficiency and the reaction selectivity.Furthermore, cation radicle is more symmetrical or the longest alkyl chain is shorter, the current efficiency and the reaction selectivity are higher.The tetraethyl quarternary ammonium salt has the best active effect.
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Electrochemical process of heteroatom degradation by DC corona discharge
- ZOU Fang, WU Zucheng, KANG Ying, MA Xiangjuan
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2010, 61(S1):
91-95.
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Abstract
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1165 )
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657
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The degradation process of heteroatom organics by high active hydroxyl radicals generated from DC corona discharge plasma was investigated using pyridine as a model pollutant.The electrochemical process could be fully elucidated from the point of view of water droplets,water droplet or cloudy droplet formed the small electrolytic cell.90.4% of pyridine could be removed at 20.75 kV and the initial concentration of pyridine was 8287 mg·m-3.Intermediates in droplet were detected by HPLC,indicating that fumaric acid and oxalic acid were the main intermediates,and nitrate was detected by ion chromatographic.Based on the above results,the possible degradation pathway of pyridine was proposed.
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CO poisoning properties during methanol electro-oxidation onpolypyrrole modified by platinum
- ZHU Wanxia, WANG Wuyang, LI Meichao, MO Weimin
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2010, 61(S1):
96-100.
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Abstract
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1504 )
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387
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Cyclic voltammetry and in situ electrochemical FTIR spectroscopy techniques have been combined to study the methanol electro-oxidation on polypyrrole modified by platinum(nm-Pt/PPy).The nm-Pt/PPy shows good electrocatalytic activity for methanol electro-oxidation,and the final product CO2 can be observed at 1000mV.However,CO poisoning of Pt particles can’t be avoided despite the presence of polypyrrole film.At low potentials,the linearly absorbed CO and the bridge-bonded CO form on the nm-Pt/PPy,respectively.With the potential increasing,there is only the linearly absorbed CO.At high potentials,the PPy is overoxidized and the electrocatalytic activity of nm-Pt/PPy is decreased.
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Preparation of FePt/GC nanocatalysts and their electrocatalytic activities for ethanol oxidation
- WANG Jieying,CHEN Shengpei,WANG Peng,HUANG Rui,LI Mingxuan,SUN Shigang
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2010, 61(S1):
101-105.
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Abstract
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833 )
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361
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Iron nanoparticles were uniformly deposited on glassy carbon electrode by electrochemical cyclic voltammetry,and the Fe core/Pt shell nanoparticles were further obtained through “galvanic replacement”.SEM observation illustrated that the cuboid nanoparticles dispersing uniformly on GC surface.The electrocatalytical properties for ethanol oxidation of the nano-Pt/GC,nano-FePt/GC were studied by cyclic voltammetry(CV).The nano-FePt/GC electrode shows high electrocatalytical activity.The catalytic activity is in the order of:nano-Pt/GC<nano-FePt/GC.The onset potential(Ei)of ethanol oxidation on nano-FePt/GC electrode is negatively shifted 0.044 V,and the steady oxidation current density(jp)is enhanced about 2.16 times,compared with nano-Pt/GC electrode.
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Electrosynthesis of electrode board material LiAlO2
- FANG Wenyan, WANG Fengwu, ZHU Chuangao, XU Mai
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2010, 61(S1):
116-119.
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Abstract
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883 )
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256
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0.18 g Li slice was put into 100 ml ethanol and 1 ml acetyl-acetone solution and then the precursor of nano-LiAlO2 was synthesized by electrolysis of aluminum for 6 h at the current of 0.2 A in the above.Nano-LiAlO2 was obtained at 550℃ for 2 h after drying and hydrolysis of the precursor.The products were characterized by XRD, TEM and Raman.The results indicate that the precursor should be calcined at 550℃ in order to make the nano-sized LiAlO2 of 30 nm.In molten carbonate fuel cell stack(MCFC), the average opening circuit voltage of individual cell is about 1.15 V.The density of the electric current reaches 187 mA·cm-2 .The output power of stack is 217.8 W.The cell was operated for 10 thermal circles without reducing its performance.
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Unipolar pulse electrochemical polymerization of polyaniline nanofiber films for supercapacitor applications
- LI Yue,HAO Xiaogang,WANG Zhongde,ZHANG Zhonglin,LIANG Zhenhai,LIU Shibin
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2010, 61(S1):
120-125.
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1273 )
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1070
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Polyaniline (PANI) naonfiber films with three-dimensional network structure were successfully prepared on platinum substrates using unipolar pulse electrochemical polymerization.The composition and morphology of PANI films prepared by pulse and CV polymerization were characterized by Fourier transfer infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM).The supercapacitive performances of the PANI films were also investigated in 0.5 mol·L-1 H2SO4solution with cyclic voltammetry (CV) cycling in the range -0.2 V to 0.55 V (vs SCE),charge/discharge tests and electrochemical impedance spectroscopy (EIS).Results show that three-dimensional porous network PANI films with uniform distribution on Pt are formed by this new method.The PANI films of pulse electrochemical polymerization display much higher ion exchange capacity,better stability and more excellent supercapacitive performances than the PANI films produced by the more common CV method.The highest specific capacitance value of 699 F·g-1 is obtained for PANI film when the pulse potential,aniline concentration,pulse frequency and duty cycle are 1.0 V,0.2 mol·L-1,1.25 s-1 and 50%,respectively.
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SA/CS bipolar membrane modified by metallophthalocyaninederivatives with different substituents
- CHEN Riyao,CHEN Zhen,CHEN Xiao,ZHENG Xi,CHEN Qiaoping ,XIE Hongfang
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2010, 61(S1):
126-131.
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Abstract
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1094 )
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455
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The sodium alginate (SA) cation layer was modified by copper octocarboxyphthalocyanine or copper phthalocyanine tetrasulfonic acid, and the chitosan (CS) anion layer was modified by copper tetraaminophthalocyanine to prepare the modified SA/CS bipolar membranes (BPMs).The BPMs were characterized using TG, electric universal testing machine, contact angle measurer and J-V investigation.Experimental results showed that the thermal stability, mechanical properties and hydrophilicity of the BPMs were increased.After modification, high charge density area formed in the interlayer.As the catalytic centers of water splitting in the interlayer, metallophthalocyanine derivatives sped up water splitting into hydrogen ions and hydroxide ions, and lowered the IR drop of the BPMs.The metallophthalocyanine derivatives with dissimilar substituents showed different catalytic ability to water splitting in BPMs, which was in connection with the hydrophilicity of the relevant modified membranes.
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Electrocatalytic properties of acrylamide and acrylic acidcopolymerization on Ti/PbO2 electrode
- ZHANG Liqin, LIANG Zhenhai, LI Wanjie, LIU Chengcen
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2010, 61(S1):
132-136.
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Abstract
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907 )
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382
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The Ti/PbO2 electrode was prepared by the thermal decomposition and electro-deposition method.The acrylamide(AM)and acrylic acid(AA)were polymerized to prepare poly(acrylamide-co-acrylic acid)on the Ti/PbO2 electrode.The reaction products and kinetics of the process were discussed.The molecular weight of the poly(acrylamide-co-acrylic acid)was measured by viscosity method.The product was discussed by infrared spectroscopy(IR)and cyclic voltammetry curves(CV).The influence on concentration of monomer,current density and initiator concentration were investigated.The results showed that acrylamide and acrylic acid can be polymerized to poly(acrylamide-co-acrylic acid)by electrocatalytic polymerization under the effects of both cerium Ce(Ⅳ)and electrocatalytic systems.The best technological parameters were obtained:T=20℃,n(AM)∶n(AA)=2.3∶1,ω[Ce(Ⅳ)]=0.8%,I=0.125 A·cm-2,ω(H2SO4)=0.5 mol·L-1.The molecular weight of polyacrylamide was 6.5×105.The conversion rate could be increased to 70%.