脉冲电催化氧化处理染料废水研究
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摘要
电催化氧化法是一种高级电化学氧化技术，其主要利用具有催化性能的金属氧化物电极，产生具有强氧化能力的羟基自由基或其它自由基来氧化水中污染物，使其完全氧化分解为CO2和H2O，以达到去除废水中的有机物的目的。近些年来，电催化氧化法在处理难降解有机废水的方面引起了广泛关注。脉冲电解技术在节能和电极损耗方面有较强的优势。目前有关脉冲电解技术与电催化氧化技术相结合处理染料废水的报道颇少。本文提出构建脉冲电催化氧化体系，系统地考察了脉冲电催化氧化体系对酸性靛蓝染料模拟废水进行了降解处理；分析了酸性靛蓝在该体系中的反应动力学和矿化效果；研究了酸性靛蓝在该体系的降解途径和反应机理；对比该体系对不同染料的去除效率，考察了染料物化性质对处理效果的影响。论文取得了主要结论如下：
（1）采用脉冲电催化氧化体系对酸性靛蓝溶液进行处理过程中，溶液初始浓度、电解质浓度、施加电压、脉冲频率等因素对其脱色效果均有一定影响，在反应过程中脱色率均能较好地符合一级反应动力学规律。建立了总反应的动力学模型，影响反应速率常数由强到弱依次为电解质浓度>施加电压>脉冲频率>反应物初始浓度。
（2）pH值、酸性靛蓝初始浓度、电解质浓度、施加电压、脉冲频率和占空比对酸性靛蓝的矿化效果有一定的影响。得到最佳反应条件为：pH值为3，酸性靛蓝初始浓度为220mg/L，电解质NaCl浓度1.5g/L，施加电压15V，脉冲频率为4kHz，占空比为0.4。在最佳反应条件下处理180min，TOC去除率率为31.2%，废水的可生化性明显提高，单位处理TOC能耗为159kwh/kgTOC，电流效率为15.3%。
（3）酸性靛蓝分子在脉冲电催化氧化的矿化过程是先通过酸性靛蓝分子中的C=C双键断裂，使水溶液脱色；随后将里面C-N键和C-S键进一步氧化为简单的苯环芳香化合物；芳香化合物的苯环进一步被氧化打开，形成结构简单的脂肪酸类物质，直到最后彻底矿化为CO2、H2O、NH4+和NO3-。
（4）在脉冲电催化氧化体系对有机物去除是有羟基自由基和活性氯两种氧化机理共同作用的过程。反应180min后，TOC去除率为47.1%，其中为OH自由基氧化TOC去除率为13.8%，以活性氯氧化TOC所占的比例为33.3%。该反应体系中对有机物的去除过程以活性氯氧化机理为主。
（5）分析了脉冲电催化氧化体系对15种染料的处理效果，染料的骨架结构、磺酸基个数、芳香环、偶氮双键个数以及变极异构现象等因素对处理效果有一定影响。偶氮染料的分子结构中分子量与磺酸基个数比值、无机性与有机性比值以及偶氮双键数目与TOC去除率间存在较好的线性相关性。分子量与磺酸基个数比值的贡献最为显著。
Electrocatalytic oxidation is an advanced electrochemical oxidation processes and theuesd of some metal oxides as electrode was benificical to the electrogeneration ofhydroxyl radicals and other radicals which would destroy the pollutants to carbon dioxideand water.In the recent years, there has developed great interest in the development ofenvironmentally firendly electrochemical methods to degrade recalcitrant organicpollutants in wasterwaters.The pulse electrolysis processes has a advantage in terms ofthat can reduce both the energy and electrode consumption. Up to now, little attention waspaid to the treatment of dye wastewater using the combination of pulse electrolysis andelectrocatalytic oxidation. Therefore, electrocatalytic oxidation of the dye indigo carmine(IC) with pulse electrolysis was systematically investigated in the present paper. Thekinetics and mineralization of the processes was studied. The degradation pathway andreactive mechanism of IC in the electrocatalytic oxidation system with pulse electrolysiswas explored. The treatment of15kinds of dyes was performed in the system. The effectof dye physico-chemical properties on the treatment efficiency was further studied. Theprimary results obtained are as follows:
(1) During the processes, initial IC concentration, NaCl concentration, voltage andfrequency were observed to have effect on the discoloration efficiency. The reactionkinetics followed a pseudo-first order in the process. The total reaction kinetics equationwas established and the effect of the four parameters on the reaction rate followed theorder: NaCl concentration> voltage> frequency> IC concentration.
(2) Several factors have effect on the TOC removal efficiency, such as pH value,initial IC concentration, NaCl addition, voltage, frequency and duty ratio. Under theoptimization condition of the process was performed at pH3,220mg/L IC,1.5g/L NaCl,15V,4kHz and duty ratio of0.4decreases in the TOC of31.2%was achieved after180min. Furthermore, the biodegradability of the water was improved significantly. Theenergy consumption was159kwh/kgTOC and the current efficiency was15.3%.
(3) Decomposition of IC in the electrocatalytic oxidation reactor with pulseelectrolysis was proposed to be firstly initiated by the cleavage of C=C, which resulted in decolorization of the solution. Afterwards, the C-N and C-S were further oxidaized tosome benzene-type compounds and then to oxalic and oxamic acids resulted from thearomatic ring cleavage. Finally, these carboxylic acids were converted into CO2, H2O,NH4+and NO3-to accomplish an entire mineralization process.
(4) The TOC removal efficiency was47.1%after180min treatment with3.5g/L NaCl.The removal of organic compound in this system was the process combined the oxidationof hydroxyl radical (·OH) and active chlorine (Cl2, HClO, and ClO-), which respectivelycontrubute to13.8%and33.3%of TOC removal efficiency.
(5) Degradation of15kinds of dyes was performed in the system and found out thatsome factors such as dye stucture type, number of sulfonate group, number of azochromophore group and aromatic ring in the dye molecule had some effect on thetreatment efficiency. The quantitative relationship between the TOC removal efficiencyand molecular descriptors such as the ratio of the molecular weight to the number ofsulfonate group, the ratio of the hydrophilicity to the lipophilicity and the number of azochromophore group was studied. The results indicated that good linear correlations existbetween the TOC removal efficiency and their molecular descriptors. In particular, theratio of the molecular weight to the number of sulfonate group has most prominentcontribution to the TOC removal rate.
（1）采用脉冲电催化氧化体系对酸性靛蓝溶液进行处理过程中，溶液初始浓度、电解质浓度、施加电压、脉冲频率等因素对其脱色效果均有一定影响，在反应过程中脱色率均能较好地符合一级反应动力学规律。建立了总反应的动力学模型，影响反应速率常数由强到弱依次为电解质浓度>施加电压>脉冲频率>反应物初始浓度。
（2）pH值、酸性靛蓝初始浓度、电解质浓度、施加电压、脉冲频率和占空比对酸性靛蓝的矿化效果有一定的影响。得到最佳反应条件为：pH值为3，酸性靛蓝初始浓度为220mg/L，电解质NaCl浓度1.5g/L，施加电压15V，脉冲频率为4kHz，占空比为0.4。在最佳反应条件下处理180min，TOC去除率率为31.2%，废水的可生化性明显提高，单位处理TOC能耗为159kwh/kgTOC，电流效率为15.3%。
（3）酸性靛蓝分子在脉冲电催化氧化的矿化过程是先通过酸性靛蓝分子中的C=C双键断裂，使水溶液脱色；随后将里面C-N键和C-S键进一步氧化为简单的苯环芳香化合物；芳香化合物的苯环进一步被氧化打开，形成结构简单的脂肪酸类物质，直到最后彻底矿化为CO2、H2O、NH4+和NO3-。
（4）在脉冲电催化氧化体系对有机物去除是有羟基自由基和活性氯两种氧化机理共同作用的过程。反应180min后，TOC去除率为47.1%，其中为OH自由基氧化TOC去除率为13.8%，以活性氯氧化TOC所占的比例为33.3%。该反应体系中对有机物的去除过程以活性氯氧化机理为主。
（5）分析了脉冲电催化氧化体系对15种染料的处理效果，染料的骨架结构、磺酸基个数、芳香环、偶氮双键个数以及变极异构现象等因素对处理效果有一定影响。偶氮染料的分子结构中分子量与磺酸基个数比值、无机性与有机性比值以及偶氮双键数目与TOC去除率间存在较好的线性相关性。分子量与磺酸基个数比值的贡献最为显著。
Electrocatalytic oxidation is an advanced electrochemical oxidation processes and theuesd of some metal oxides as electrode was benificical to the electrogeneration ofhydroxyl radicals and other radicals which would destroy the pollutants to carbon dioxideand water.In the recent years, there has developed great interest in the development ofenvironmentally firendly electrochemical methods to degrade recalcitrant organicpollutants in wasterwaters.The pulse electrolysis processes has a advantage in terms ofthat can reduce both the energy and electrode consumption. Up to now, little attention waspaid to the treatment of dye wastewater using the combination of pulse electrolysis andelectrocatalytic oxidation. Therefore, electrocatalytic oxidation of the dye indigo carmine(IC) with pulse electrolysis was systematically investigated in the present paper. Thekinetics and mineralization of the processes was studied. The degradation pathway andreactive mechanism of IC in the electrocatalytic oxidation system with pulse electrolysiswas explored. The treatment of15kinds of dyes was performed in the system. The effectof dye physico-chemical properties on the treatment efficiency was further studied. Theprimary results obtained are as follows:
(1) During the processes, initial IC concentration, NaCl concentration, voltage andfrequency were observed to have effect on the discoloration efficiency. The reactionkinetics followed a pseudo-first order in the process. The total reaction kinetics equationwas established and the effect of the four parameters on the reaction rate followed theorder: NaCl concentration> voltage> frequency> IC concentration.
(2) Several factors have effect on the TOC removal efficiency, such as pH value,initial IC concentration, NaCl addition, voltage, frequency and duty ratio. Under theoptimization condition of the process was performed at pH3,220mg/L IC,1.5g/L NaCl,15V,4kHz and duty ratio of0.4decreases in the TOC of31.2%was achieved after180min. Furthermore, the biodegradability of the water was improved significantly. Theenergy consumption was159kwh/kgTOC and the current efficiency was15.3%.
(3) Decomposition of IC in the electrocatalytic oxidation reactor with pulseelectrolysis was proposed to be firstly initiated by the cleavage of C=C, which resulted in decolorization of the solution. Afterwards, the C-N and C-S were further oxidaized tosome benzene-type compounds and then to oxalic and oxamic acids resulted from thearomatic ring cleavage. Finally, these carboxylic acids were converted into CO2, H2O,NH4+and NO3-to accomplish an entire mineralization process.
(4) The TOC removal efficiency was47.1%after180min treatment with3.5g/L NaCl.The removal of organic compound in this system was the process combined the oxidationof hydroxyl radical (·OH) and active chlorine (Cl2, HClO, and ClO-), which respectivelycontrubute to13.8%and33.3%of TOC removal efficiency.
(5) Degradation of15kinds of dyes was performed in the system and found out thatsome factors such as dye stucture type, number of sulfonate group, number of azochromophore group and aromatic ring in the dye molecule had some effect on thetreatment efficiency. The quantitative relationship between the TOC removal efficiencyand molecular descriptors such as the ratio of the molecular weight to the number ofsulfonate group, the ratio of the hydrophilicity to the lipophilicity and the number of azochromophore group was studied. The results indicated that good linear correlations existbetween the TOC removal efficiency and their molecular descriptors. In particular, theratio of the molecular weight to the number of sulfonate group has most prominentcontribution to the TOC removal rate.
引文
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