掺杂含氟β-PbO_2电极的制备及电催化性能研究
摘要
电化学氧化方法作为一种环境友好型技术,在处理有毒难生物降解有机污水时呈现了其他水处理技术难以比拟的优越性,应用前景极佳。电化学氧化降解技术的核心问题是高性能阳极的制备。在常见的几种阳极材料中,二氧化铅电极由于其高性价比而得到人们的青睐,但离实际应用还有一定的差距。已有文献研究表明,在镀制β-PbO_2过程中,掺入少量添加剂可以改善电极的表面微观结构,从而改变电极的催化性能。基于上述研究现状,考虑到稀土元素所具有的特殊性质,本工作制备不同稀土氧化物掺杂的PbO_2电极,并对其在无机水溶液和有机水溶液中的电化学性能进行了详细的研究。
本工作制备了稀土氧化物CeO_2和La_2O_3掺杂的含氟β-PbO_2电极,考察了不同电沉积条件下电极强化电解的失重情况,在此基础上优化了这两类掺杂电极的电沉积工艺。利用相关表面测试技术和电化学测试方法考察了改性前后电极物化性质及电化学性能的差异。研究并探讨了稀土掺杂改性电极镀层结构、电极寿命、无机水溶液中的析氧活性、有机水溶液中的电氧化效率等因素之间的相关性规律。上述结果为进一步开发性能优异的二氧化铅电极提供理论依据,从而有效地推广电化学技术在实际废水处理中的应用。
研究表明,镀液中添加一定量的稀土氧化物,搅速为1300r/min,温度为80℃,在160mA/cm~2下电沉积1h,所制得的电极表面镀层均匀致密,失重较慢。掺杂后二氧化铅电极表面晶相仍以β-PbO_2为主,活性表面积及铅氧非计量比均有所增大。稀土氧化物颗粒均匀地分布并嵌入电极镀层。相关测试结果表明,F-PbO_2、CeO_2-F-PbO_2、La_2O_3-F-PbO_2三电极活性表面积分别为:3.0、4.88、5.12cm~2(基体的表观面积1cm~2)。比较这些电极在硫酸溶液中的析氧行为发现,掺杂后电极的Tafle斜率减小,两电极的交换电流密度减小,析氧反应表观活化能提高。说明稀土氧化物降低电极的析氧活性,干扰了析氧过程中活性中间物的转化过程,在电氧化降解过程中抑制了析氧副反应。
以对氯苯酚为目标有机物,考察了稀土掺杂前后电极的电催化氧化特性、吸附特性和失活行为。结果表明,稀土掺杂弱化了掺杂电极直接电催化氧化4-CP反应的响应电流,这可能与电极表面反应活性点的变化有关。CeO_2-F-PbO_2电极对有机物吸附量几乎是掺杂前的两倍。电极的稳定性测试表明,在酸性或中性溶液中,峰电流缓慢减小,但在碱性溶液中,峰电流快速减小。无论溶液的酸碱度如何变化,多次扫描后CeO_2-F-PbO_2电极的剩余电流都较大,具有较高的抗失活性。与F-PbO_2电极相比,La_2O_3-F-PbO_2电极吸附量变化不明显,而且也易失活。
电极对目标有机物电氧化降解特性的研究结果表明,稀土掺杂能有效地提高二氧化铅的电氧化特性。掺杂后电极反应表观动力学参数增大,说明掺杂稀土有利于改善含氟PbO_2电极的降解性能,降低能耗。在相同条件下电解8个小时后,三种电极COD的去除率分别为34.2%、53.87%、71.61%。电极的瞬时电流效率在电解开始的2小时内下降较快,但总体上还是要高出未掺杂电极,CeO_2-F-PbO_2电极提高一倍多,La_2O_3-F-PbO_2电极高出3倍多。从现有的结果看,稀土氧化物可能影响了中间活性物种(如·OH等)的寿命,但这个推论有待于相关实验结果的进一步证实。
Being compared with the existing technologies on treating toxic bio-refactory organic in wastewater,electrochemical oxidation method has showed superiority with its environmental friendliness and application prospect.At present,the popular issue of this method is to prepare a high-performance anode.Among common applied materials lead dioxide electrode has been attached a close attention because of its cost-effective. However,there is still a gap between exprimental test and practical application.It has been reported that doping a bit of additives can change the microstructure ofβ-PbO_2 and improve its elctro-catalytic properties.On the basis of special nature of rare earth elements,some modified PbO_2 anodes were prepared and their electrochemical properties in the inorganic and organic aqueous solution were also investigated in detail.
CeO_2 and La_2O_3 particles were selected as dopants to modify F-β-PbO_2 electrodes in this study.Weight loss of the anode under accelerating electrolysis was carried out to optimize the plating conditions.The physicalchemical property and electro-catalytic characteristic of the modified anode were investigated using different surface analysis technologies and electrochemical tests.The intrinsic relations between electrode surface structure,service life,electro-catalytic activity of oxygen evolution(OE) in inorganic aqueous solution and the efficiency of electro-oxidation in organic aqueous solution were investigated and discussed.The results of this work could supply a theoretical basis for the further preparation PbO_2 electrode with an excellent performance,and then could effectively promote the electrochemical technology in practical application of wastewater treatment.
The experiemtnal results indicated that dense and even electrode surface coating could be obtained and its weight loss slowed down under the following plating conditions:a suitable concentration of rare earth oxide,the plating solution agitated by magnetic bar with an 1300r/min, temperature at 80℃,current density under 160mA/cm~2,electrodepostion for 1h.The main crystal of modified electrode was stillβ-PbO_2.Oxide adulteration could increase active surface and oxygen vacancy defect of PbO_2,and oxide particle evenly distributed and embedded in the electrode coating.The active surface area of F-PbO_2,CeO_2-F-PbO_2,La_2O_3-F-PbO_2 electrode were 3.0,4.88,5.12cm~2(the apparent area of the matrix 1cm~2), respectively.In comparision of behaviors of their OE reaction in H_2SO_4 aqueous solution,exchange current density and tafle slope of modified electrodes obviously decreased while apparent activation energy of OE reaction increased.The above results indicated that addition of rare earth oxide may disturb kinetic process of OE reaction and weaken formation of O_2 as competitive reaction during electro-oxidative degradation of organics.
The electro-catalytic properties,adsorption and deactivation behavior of modified electrodes in the 4-chlorophenol(4-CP) aqueous solution were investigated.The experimental results showed that rare earth oxide dopant could probably affect the existence of active intermediates on the electrode surface.The organic absorption capacity of CeO_2-F-PbO_2 electrode was almost twice than the undoped.The oxidative peak current(i_p) of 4-CP on CeO_2-F-PbO_2 electrode remained high regardless of pH of solution after scanning for many times,showing high anti-deactivation.The adsorption capacity of La_2O_3-F-PbO_2 electrode changed little in comparison with F-PbO_2 electrode,and the i_p of 4-CP decreased rapidly for four times,indicating its easy deactivation.
4-CP degradation properties of different anodes were studied.The experimental results showed that doping of rare earth oxides could effectively improve the electro-oxidation characteristics of PbO_2.The appearent kinetic parameter of 4-CP by different anodes increased because of an addition of rare oxide,thus leading to reduce energy consumption. For example,the COD removal rates of three electrodes under the same conditions were 34.2%,53.87%,71.61%after 8h electrolysis,respectively. The instantaneous current efficiency(ICE) declined rapidly during the first 2h of electrolysis.In general,CeO_2-F-PbO_2 and La_2O_3-β-PbO_2 anode had one and three times ICE higher thanβ-PbO_2 electrode had,respectively. From the present results,rare earth oxide may affect the existing life of the active intermediate species(·OH,etc.),which should be further confirmed by interrelated experimental evidences.
本工作制备了稀土氧化物CeO_2和La_2O_3掺杂的含氟β-PbO_2电极,考察了不同电沉积条件下电极强化电解的失重情况,在此基础上优化了这两类掺杂电极的电沉积工艺。利用相关表面测试技术和电化学测试方法考察了改性前后电极物化性质及电化学性能的差异。研究并探讨了稀土掺杂改性电极镀层结构、电极寿命、无机水溶液中的析氧活性、有机水溶液中的电氧化效率等因素之间的相关性规律。上述结果为进一步开发性能优异的二氧化铅电极提供理论依据,从而有效地推广电化学技术在实际废水处理中的应用。
研究表明,镀液中添加一定量的稀土氧化物,搅速为1300r/min,温度为80℃,在160mA/cm~2下电沉积1h,所制得的电极表面镀层均匀致密,失重较慢。掺杂后二氧化铅电极表面晶相仍以β-PbO_2为主,活性表面积及铅氧非计量比均有所增大。稀土氧化物颗粒均匀地分布并嵌入电极镀层。相关测试结果表明,F-PbO_2、CeO_2-F-PbO_2、La_2O_3-F-PbO_2三电极活性表面积分别为:3.0、4.88、5.12cm~2(基体的表观面积1cm~2)。比较这些电极在硫酸溶液中的析氧行为发现,掺杂后电极的Tafle斜率减小,两电极的交换电流密度减小,析氧反应表观活化能提高。说明稀土氧化物降低电极的析氧活性,干扰了析氧过程中活性中间物的转化过程,在电氧化降解过程中抑制了析氧副反应。
以对氯苯酚为目标有机物,考察了稀土掺杂前后电极的电催化氧化特性、吸附特性和失活行为。结果表明,稀土掺杂弱化了掺杂电极直接电催化氧化4-CP反应的响应电流,这可能与电极表面反应活性点的变化有关。CeO_2-F-PbO_2电极对有机物吸附量几乎是掺杂前的两倍。电极的稳定性测试表明,在酸性或中性溶液中,峰电流缓慢减小,但在碱性溶液中,峰电流快速减小。无论溶液的酸碱度如何变化,多次扫描后CeO_2-F-PbO_2电极的剩余电流都较大,具有较高的抗失活性。与F-PbO_2电极相比,La_2O_3-F-PbO_2电极吸附量变化不明显,而且也易失活。
电极对目标有机物电氧化降解特性的研究结果表明,稀土掺杂能有效地提高二氧化铅的电氧化特性。掺杂后电极反应表观动力学参数增大,说明掺杂稀土有利于改善含氟PbO_2电极的降解性能,降低能耗。在相同条件下电解8个小时后,三种电极COD的去除率分别为34.2%、53.87%、71.61%。电极的瞬时电流效率在电解开始的2小时内下降较快,但总体上还是要高出未掺杂电极,CeO_2-F-PbO_2电极提高一倍多,La_2O_3-F-PbO_2电极高出3倍多。从现有的结果看,稀土氧化物可能影响了中间活性物种(如·OH等)的寿命,但这个推论有待于相关实验结果的进一步证实。
Being compared with the existing technologies on treating toxic bio-refactory organic in wastewater,electrochemical oxidation method has showed superiority with its environmental friendliness and application prospect.At present,the popular issue of this method is to prepare a high-performance anode.Among common applied materials lead dioxide electrode has been attached a close attention because of its cost-effective. However,there is still a gap between exprimental test and practical application.It has been reported that doping a bit of additives can change the microstructure ofβ-PbO_2 and improve its elctro-catalytic properties.On the basis of special nature of rare earth elements,some modified PbO_2 anodes were prepared and their electrochemical properties in the inorganic and organic aqueous solution were also investigated in detail.
CeO_2 and La_2O_3 particles were selected as dopants to modify F-β-PbO_2 electrodes in this study.Weight loss of the anode under accelerating electrolysis was carried out to optimize the plating conditions.The physicalchemical property and electro-catalytic characteristic of the modified anode were investigated using different surface analysis technologies and electrochemical tests.The intrinsic relations between electrode surface structure,service life,electro-catalytic activity of oxygen evolution(OE) in inorganic aqueous solution and the efficiency of electro-oxidation in organic aqueous solution were investigated and discussed.The results of this work could supply a theoretical basis for the further preparation PbO_2 electrode with an excellent performance,and then could effectively promote the electrochemical technology in practical application of wastewater treatment.
The experiemtnal results indicated that dense and even electrode surface coating could be obtained and its weight loss slowed down under the following plating conditions:a suitable concentration of rare earth oxide,the plating solution agitated by magnetic bar with an 1300r/min, temperature at 80℃,current density under 160mA/cm~2,electrodepostion for 1h.The main crystal of modified electrode was stillβ-PbO_2.Oxide adulteration could increase active surface and oxygen vacancy defect of PbO_2,and oxide particle evenly distributed and embedded in the electrode coating.The active surface area of F-PbO_2,CeO_2-F-PbO_2,La_2O_3-F-PbO_2 electrode were 3.0,4.88,5.12cm~2(the apparent area of the matrix 1cm~2), respectively.In comparision of behaviors of their OE reaction in H_2SO_4 aqueous solution,exchange current density and tafle slope of modified electrodes obviously decreased while apparent activation energy of OE reaction increased.The above results indicated that addition of rare earth oxide may disturb kinetic process of OE reaction and weaken formation of O_2 as competitive reaction during electro-oxidative degradation of organics.
The electro-catalytic properties,adsorption and deactivation behavior of modified electrodes in the 4-chlorophenol(4-CP) aqueous solution were investigated.The experimental results showed that rare earth oxide dopant could probably affect the existence of active intermediates on the electrode surface.The organic absorption capacity of CeO_2-F-PbO_2 electrode was almost twice than the undoped.The oxidative peak current(i_p) of 4-CP on CeO_2-F-PbO_2 electrode remained high regardless of pH of solution after scanning for many times,showing high anti-deactivation.The adsorption capacity of La_2O_3-F-PbO_2 electrode changed little in comparison with F-PbO_2 electrode,and the i_p of 4-CP decreased rapidly for four times,indicating its easy deactivation.
4-CP degradation properties of different anodes were studied.The experimental results showed that doping of rare earth oxides could effectively improve the electro-oxidation characteristics of PbO_2.The appearent kinetic parameter of 4-CP by different anodes increased because of an addition of rare oxide,thus leading to reduce energy consumption. For example,the COD removal rates of three electrodes under the same conditions were 34.2%,53.87%,71.61%after 8h electrolysis,respectively. The instantaneous current efficiency(ICE) declined rapidly during the first 2h of electrolysis.In general,CeO_2-F-PbO_2 and La_2O_3-β-PbO_2 anode had one and three times ICE higher thanβ-PbO_2 electrode had,respectively. From the present results,rare earth oxide may affect the existing life of the active intermediate species(·OH,etc.),which should be further confirmed by interrelated experimental evidences.
引文
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