TiO_2光催化氧化As（Ⅲ）机理及其对碳钢的光电化学防护
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摘要
在环境污染物中,砷是最毒的元素之一,饮用未处理的地下水带来的慢性砷中毒,能造成各种健康损害,包括皮肤,肝,肾,肺等癌症。在自然水体中,砷主要以三价砷(As(Ⅲ))和五价砷(As(Ⅴ))的形式存在。许多水处理技术,能有效的脱除As(V),而常常对毒性更大的As(Ⅲ)无能为力。为了提高砷的去除效率,有必要将As(Ⅲ)氧化为易处理的As(V)。TiO2光催化氧化技术可以有效的将As(Ⅲ)氧化为As(V)。但是,在光催化过程中光生空穴、羟基自由基和超氧自由基等活性物种对As(Ⅲ)氧化的贡献,至今还存在争议。如何准确地区分这些物种在污染物氧化过程中的作用,不仅是光催化降解污染物技术的关键科学问题之一,也是该领域的研究难点。本论文针对上述科学问题,以砷为目标污染物,首次结合光(电)化学方法系统地研究了其氧化动力学、机理,并初步研究了As(Ⅲ)光催化氧化对典型金属碳钢的光电化学保护效果。论文分三部分,第一部分定量区分了超氧自由基及其衍生物和光生空穴在As(Ⅲ)光催化氧化过程中的作用;第二部分研究了As(Ⅲ)光催化氧化过程中光生空穴界面转移动力学和机理笫三部分以As(Ⅲ)为电子供体,初步研究了TiO2及其表面氟化改性TiO2对碳钢的光电化学保护行为。
第一部分结合光(电)化学方法系统地研究了As(Ⅲ)光催化氧化动力学并定量区分了超氧自由基及其衍生物和光生空穴氧化As(Ⅲ)的机理。在无光照、有氧和负偏压的条件下,证实了超氧自由基可以氧化As(Ⅲ),但氧化效率低,表明超氧自由基是一种较弱的氧化剂。光照时超氧自由基可生成更强的氧化剂,从而能够有效地氧化As(Ⅲ)。在缺氧、阳极偏压和光照时,光生空穴的电流效率几乎为100%,表明其对As(Ⅲ)具有很强的氧化能力。在通常的光催化条件下(有氧、开路),光生空穴和超氧自由基及其衍生物对As(Ⅲ)的氧化贡献分别为57%和43%,起着几乎同等的作用。
第二部分采用数学模型和饱和光电流测试实验,数学模型和不同As(Ⅲ)浓度时降解实验相结合的研究方法,研究了光生空穴和羟基自由基对As(Ⅲ)氧化的贡献。实验结果表明,在所研究的试验条件下羟基自由基对As(Ⅲ)的氧化起主要作用。采用空穴和羟基自由基捕获剂,及电极表面改性等常规研究方法,定性的探讨了As(Ⅲ)的氧化机理。实验结果辅助证实了As(Ⅲ)的羟基自由基氧化机理。
第三部分考察了Ti02电极表面氟化改性,溶液中As(Ⅲ)的加入和02的去除对电极光电性能和对碳钢的阴极保护性能的影响。试验结果表明,电极表面氟化溶液中As(Ⅲ)的加入和O2的去除,均可以显著的提高电极的光电流,降低电极的光电势,从而提高了光电极对金属的光电化学防护性能。在As(Ⅲ)存在下和N2氛围中,氟化Ti02可以对腐蚀电位很负的碳钢进行有效地阴极保护。
Arsenic is one of the most poisonous elements in environmental pollutants. Studies on long-term human exposure reported that arsenic in drinking water was associated with liver, lung, kidney, bladder, and skin cancers. Arsenic in groundwater occurs primarily in inorganic form, either as arsenite (As(Ⅲ)), or arsenate (As(Ⅴ)). As(V) could be efficiently removed by common water treatment methods. However, the removal of As(Ⅲ) by such processes is often substantially less efficient. The oxidation of As(Ⅲ) to As(V), is required for the efficient removal of arsenic.TiO2photo-catalysis has been shown to be effective in oxidizing As(Ⅲ) to As(V) in the presence of oxygen. However, the As(Ⅲ) photo-oxidation mechanism is complex, has been an issue of considerable controversy. Lines of evidence supporting As(Ⅲ) oxidation by super-oxide, hydroxyl radicals, valence band holes have been reported.
To unequivocally answer who, among the photo-hole, super-oxide, and its photo-induced derivates, is the main oxidant in the normal aerated aqueous solutions and at open circuit conditions, their respective contribution to As(Ⅲ) oxidation was studied. The contribution of photo-hole to As(Ⅲ) oxidation was investigated under conditions of anodic bias potentials and under illumination. The role of super-oxide in the dark and its photo-induced derivates under illumination were studied respectively under the conditions of negative bias potentials and air-saturated which conditions no photo-holes would be involved in the oxidation of As(Ⅲ). The results show the sum contribution of super-oxide and its derivates is considerably high (up to43%), it is not more than that of photo-hole (57%).
In order to Distinguish between the direct and indirect interfacial hole transfer, the experiments of electrochemical measurements and As(Ⅲ) oxidation were conducted in the conditions of anodic potential and N2saturated when no super-oxide was involved in the oxidation of As(Ⅲ). An Kinetics model was established and used to reveal the photocatalytic oxidation of As(Ⅲ). The measurements of photocurrent and expeneriments of As(Ⅲ) oxidation were carrird out in different light intensities and As(Ⅲ) concentrations. Based on the Kinetic model, the results showed hydroxyl radicals were mainly responsible for the photocatalytic oxidation of As(Ⅲ). Fluorinated TiO2, Hydroxyl radical and valence band hole scavenger were also used to to seek for clearer evidences for the role of hydroxyl radicals and valence band holes in the course of As(Ⅲ) oxidation. The results also confirmed that hydroxyl radicals is the main oxidant for the oxidation of As(Ⅲ).
The effect of fluorinated TiO2, the addition of As(Ⅲ) and the romovel of O2on the anticorrosion performances of TiO2electrodes have been investigated by the electrochemical methods. The results showed that fluorinated TiO2, the addition of As(Ⅲ) and the romovel of O2could obviously enhanced photocurrent and decrease the potential under illumination, thus improve the anticorrosion performances for carbon steel. Fluorinated TiO2, could produce an efficient photocathodic protection for carbon steel under the condition of N2saturated and the solution with As(Ⅲ).
第一部分结合光(电)化学方法系统地研究了As(Ⅲ)光催化氧化动力学并定量区分了超氧自由基及其衍生物和光生空穴氧化As(Ⅲ)的机理。在无光照、有氧和负偏压的条件下,证实了超氧自由基可以氧化As(Ⅲ),但氧化效率低,表明超氧自由基是一种较弱的氧化剂。光照时超氧自由基可生成更强的氧化剂,从而能够有效地氧化As(Ⅲ)。在缺氧、阳极偏压和光照时,光生空穴的电流效率几乎为100%,表明其对As(Ⅲ)具有很强的氧化能力。在通常的光催化条件下(有氧、开路),光生空穴和超氧自由基及其衍生物对As(Ⅲ)的氧化贡献分别为57%和43%,起着几乎同等的作用。
第二部分采用数学模型和饱和光电流测试实验,数学模型和不同As(Ⅲ)浓度时降解实验相结合的研究方法,研究了光生空穴和羟基自由基对As(Ⅲ)氧化的贡献。实验结果表明,在所研究的试验条件下羟基自由基对As(Ⅲ)的氧化起主要作用。采用空穴和羟基自由基捕获剂,及电极表面改性等常规研究方法,定性的探讨了As(Ⅲ)的氧化机理。实验结果辅助证实了As(Ⅲ)的羟基自由基氧化机理。
第三部分考察了Ti02电极表面氟化改性,溶液中As(Ⅲ)的加入和02的去除对电极光电性能和对碳钢的阴极保护性能的影响。试验结果表明,电极表面氟化溶液中As(Ⅲ)的加入和O2的去除,均可以显著的提高电极的光电流,降低电极的光电势,从而提高了光电极对金属的光电化学防护性能。在As(Ⅲ)存在下和N2氛围中,氟化Ti02可以对腐蚀电位很负的碳钢进行有效地阴极保护。
Arsenic is one of the most poisonous elements in environmental pollutants. Studies on long-term human exposure reported that arsenic in drinking water was associated with liver, lung, kidney, bladder, and skin cancers. Arsenic in groundwater occurs primarily in inorganic form, either as arsenite (As(Ⅲ)), or arsenate (As(Ⅴ)). As(V) could be efficiently removed by common water treatment methods. However, the removal of As(Ⅲ) by such processes is often substantially less efficient. The oxidation of As(Ⅲ) to As(V), is required for the efficient removal of arsenic.TiO2photo-catalysis has been shown to be effective in oxidizing As(Ⅲ) to As(V) in the presence of oxygen. However, the As(Ⅲ) photo-oxidation mechanism is complex, has been an issue of considerable controversy. Lines of evidence supporting As(Ⅲ) oxidation by super-oxide, hydroxyl radicals, valence band holes have been reported.
To unequivocally answer who, among the photo-hole, super-oxide, and its photo-induced derivates, is the main oxidant in the normal aerated aqueous solutions and at open circuit conditions, their respective contribution to As(Ⅲ) oxidation was studied. The contribution of photo-hole to As(Ⅲ) oxidation was investigated under conditions of anodic bias potentials and under illumination. The role of super-oxide in the dark and its photo-induced derivates under illumination were studied respectively under the conditions of negative bias potentials and air-saturated which conditions no photo-holes would be involved in the oxidation of As(Ⅲ). The results show the sum contribution of super-oxide and its derivates is considerably high (up to43%), it is not more than that of photo-hole (57%).
In order to Distinguish between the direct and indirect interfacial hole transfer, the experiments of electrochemical measurements and As(Ⅲ) oxidation were conducted in the conditions of anodic potential and N2saturated when no super-oxide was involved in the oxidation of As(Ⅲ). An Kinetics model was established and used to reveal the photocatalytic oxidation of As(Ⅲ). The measurements of photocurrent and expeneriments of As(Ⅲ) oxidation were carrird out in different light intensities and As(Ⅲ) concentrations. Based on the Kinetic model, the results showed hydroxyl radicals were mainly responsible for the photocatalytic oxidation of As(Ⅲ). Fluorinated TiO2, Hydroxyl radical and valence band hole scavenger were also used to to seek for clearer evidences for the role of hydroxyl radicals and valence band holes in the course of As(Ⅲ) oxidation. The results also confirmed that hydroxyl radicals is the main oxidant for the oxidation of As(Ⅲ).
The effect of fluorinated TiO2, the addition of As(Ⅲ) and the romovel of O2on the anticorrosion performances of TiO2electrodes have been investigated by the electrochemical methods. The results showed that fluorinated TiO2, the addition of As(Ⅲ) and the romovel of O2could obviously enhanced photocurrent and decrease the potential under illumination, thus improve the anticorrosion performances for carbon steel. Fluorinated TiO2, could produce an efficient photocathodic protection for carbon steel under the condition of N2saturated and the solution with As(Ⅲ).
引文
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