有机污染物电化学氧化反应器的流体动力学和传质性能研究
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摘要
有机污染物的电化学氧化指的是在外电场的作用下污染物在阳极表面上发生直接电化学反应,或利用在电极表面产生的强氧化性活性物种使污染物发生转化。电化学氧化法处理有机污染物具有无二次污染、环境兼容性好、反应条件温和、易于自动控制等优点,是一种具有应用前景的有机污染物处理技术。但是,该技术在实际应用过程中还存在一些亟待解决的问题,如电化学反应器的电流效率低、传质性能差等。因此,本论文以电化学法处理有机污染物的“绿色”技术实现工业化为目的,对有机污染物降解动力学、电化学反应器流动和传质的工程问题开展一系列应用基础研究。
(1)电催化氧化技术处理实际化工废水的研究
使用二维或三维电极反应器对某炼油厂的反渗透浓缩水和某氯醇法生产环氧丙烷过程中产生的皂化废水进行处理,取得了良好效果。反应器型式、电流密度、通电时间、电解液流速、电极材料和相对面积等都是影响处理效果的重要因素,但实际有机废水的处理过程中存在能耗高、电极“堵塞”、有机污染物的降解机理及降解过程动力学等问题,需要我们开展相关的电化学工程理论研究。
(2)有机污染物的电催化氧化降解动力学的研究
研究了有机物草酸在采用活性Ti/IrO2-Ta2O5电极为阳极的圆柱形电化学反应器中的整个降解过程。由于有机污染物的电催化降解包含两条都属于“直接电氧化”的反应路径,建立了能描述整个降解过程的瞬时电流效率与溶液本体有机物浓度的关系式,并通过有机物降解实验对上述模型进行了验证,实验结果与模型计算结果一致。另外,还通过参数分析探讨了有机污染物在电极表面直接电催化氧化降解的两条路径的竞争关系。
研究了氯离子存在条件下,使用Ti/IrO2-Ta2O5阳极时,有机物草酸在圆柱形电化学反应器中的间接电氧化降解过程。有机物在该体系中的电催化降解是典型的电化学反应-化学反应串联过程。当氯离子的添加浓度太少时,反应体系发生的主要是直接电氧化或氧气析出反应,电流效率很低。只有当有机废水中含有适量的氯离子时,间接电氧化才能体现出明显的降解效果。降解过程的pH值变化表明,反应开始阶段电解液呈强酸性不变,直到草酸的去除率达到80%以上,反应体系的pH值才有明显的增大。
草酸在圆柱形电化学反应器中的间接电氧化过程符合一级反应动力学规律。由于Hatta准数的大小在0.1左右,草酸与活性氯的反应主要发生在溶液本体和电极表面扩散层／反应层中,这为电化学反应器的选型、设计和优化提供了有用的信息。
(3)电化学反应器的流动特性和传质性能研究
使用常见的脉冲响应技术测定了实验室规模的滤压式电化学反应器的停留时间分布。停留时间分布的拖尾现象说明反应器存在“死区”,随着流速的增大,拖尾现象减弱；在两条流动路径的假设基础上建立的组合流动模型可以较好的描述具有双峰现象的停留时间分布。其中路径1是指穿过电极的流体,路径2是指是沿着滤压式电化学反应器的内部壁面流动的流体。组合流动模型的参数受流速和电极结构的影响。与具有较大平均停留时间的路径2有关的模型参数受流速的影响较大,这是由于反应器中的流体流动起强化对流和减小水力边界层厚度的作用,而电极结构对流动性能的影响体现在路径1上。
用极限电流法对竖直放置的管式电极反应器的平均传质系数的测定结果表明,反应器的平均传质系数随着入口扩大系数的减小而增大,但与入口流道的数量和分布无关。CFD模拟结果解释了传质提高的原因：当入口扩大系数减小时,反应器入口的下游出现了射流,并且由于射流的卷吸和扩展,电解液的湍流程度加剧,起到了强化传质的作用。
网状电极对管式平行电极反应器传质强化的研究表明,使用网状电极后,电解液的流动模式由平板电极的层流变为湍流,电极表面的水力边界层厚度减小网状电极通过强化对流提高了管式平行电极反应器的传质性能。
CFD数值模拟结果与实验结果的比较表明,CFD模拟过程中所做出的关于Nernst扩散层的假设是正确的。CFD数值模拟方法可以弥补实验条件的不足,对电化学反应器单相流动的数值模拟能够较好的反映和预测反应器的传质性能。
本论文基于有机污染物电化学降解机理,克服了已有文献中按照反应控制步骤分段讨论的缺点,建立了能描述整个降解过程的数学模型；并针对电催化氧化技术对反应器的特殊要求,提出了研究电极附近液层特征的新方法,完善了相关的电化学工程基础理论,为用于有机废水处理的电化学反应器的的设计和优化提供了有效的信息。
Electrochemical oxidation means conversion or destruction of organic substrates in wastewater under the influence of the electric field. It can take place through two different oxidation mechanisms:(1) direct anodic oxidation, where the pollutants are destroyed at the anode surface;(2) indirect oxidation where a mediator is electrochemically generated to carry out the oxidation. Electrochemical oxidation method is a perspective technology for organic wastewater treatment because its advantages such as free secondary pollution, environmental compatibility, mild reaction conditions, easy automation, etc. However, the practical application of this technology still faces some urgent problems such as low current efficiency and weak mass transfer performance. The purpose of this thesis is accelerating the industrialization of the "green" electrochemical wastewater treatment technology. Aiming to the above existing problems, we make a series of fundamental engineering researches on the electrochemical reaction kinetics for organic pollutant degradation, flow characteristic and mass transport process in the electrochemical reactor.
(1) Application of electrochemical oxidation technology for practical chemical produce wastewater treatment
Good effect was achieved by the treatment of reverse osmosis concentrated wastewater from refinery and saponification wastewater from propylene oxide production using two-dimension or three-dimension electrochemical reactor. Type of electrochemical reactor, current density, electrolysis time, electrolyte flow rate, electrode materials and their opposite area were important factors that effects the organic pollutant degradation results. However, some problem such as high energy consumption, block of three-dimension electrode, mechanism and kinetic of organic degradation was appeared. The solution of these problems needs our theoretical study about electrochemical engineering.
(2) Kinetic of organic electrochemical oxidation
The whole degradation process of oxalic acid in a cylindrical electrochemical reactor with active Ti/IrO2-Ta2O5 anode was studied. The relation between instantaneous current efficiency and organic concentration was established base on the two paths for direct electrochemical oxidation, and the kinetic model was verified by experiments. The experimental results are consistent with the established kinetic model. Furthermore, the competition between the two paths was explored with model parameter analysis.
The indirect electrochemical oxidation process of oxalic acid under the condition of chloride ion existence was studies. Organic degradation in this system is a typical series electrochemical-chemical process. When the amount of chloride ion is too little, the current efficiency is very low, that is because the reaction system occurs mainly direct electrochemical oxidation or oxygen generation. Only the indirect electro-oxidation reflects significant degradation effect when organic wastewater containing some amount of chloride ions. The variety of pH showed that, electrolyte maintains strong acid until the removal percentage of oxalic acid larger than 80%.
The indirect electrochemical degradation of oxalic acid is agreed with the role of first order reaction kinetics. The value of the Hatta number, which approximated to 0.1 indicates that, most of the reactions between the organic and the active chlorine take place both in the bulk solution and in the reaction zone near the anode.
(3) Flow characteristics and mass transfer performance of electrochemical reactor
The residence time distribution in a laboratory scale filter-press type electrochemical reactor was determined using common impulse-response technique. The phenomenon of tailing indicated the existence of "dead zone" in the reactor. This phenomenon reduces and even disappears at high flow rate. The two peaks for RTD curves can be well expressed by the composite flow model about two paths. And path-1 is the flow moves through the holes of the electrode; path-2 is the fluid flows along the internal walls of the filter-press type electrochemical reactor. The effect of flow rate and electrode configuration on the flow model parameters was investigated. Because of the enhancement of convection and the decrease of boundary layer thickness, the parameters for path-2 are significantly influenced by flow rate. And the model parameters of path-1 reflected the effect of electrode configuration on the total flow characteristics.
Determination of mass transfer coefficient for vertical tubular electrochemical reactor with parallel electrodes has shown that mass transfer coefficient increased with the decrease of expansion ratio, but it is little related to distribution and amount of circular arranged holes in baffles. The CFD simulation result showed the appearance of jet flow downstream the sudden expansion entrance. In effect, the high rates of shear induce the rotation of the solution and small eddies are formed, the level of electrolyte turbulence enhances and plays a role in improving mass transfer performance.
The study of mass transfer enhancement for mesh electrode in a tubular electrochemical reactor indicated that, the insert of mesh electrode has changed the flow pattern from laminar to turbulence, and the thickness of boundary layer gets smaller. This leads to the improvement of force convection and enhancement of mass transfer performance.
The comparison of CFD simulation and experimental results showed that the assumption related to Nernst diffusion layer is correct. The single-phase CFD simulation method is a useful tool to describe the flow characteristic and predict the local mass transfer performance in such an electrochemical reactor.
In this thesis, a kinetic model described the whole degradation process of organic pollutants was established based on the mechanism of electrochemical oxidation. And this model overcomes the shortage of former literatures discussed by control steps. Furthermore, according to the special requirements for electrochemical oxidation reactor, we have raised a novel method investigating the electrolyte layer near the electrode. These studies have provided some useful information on the selection, design and optimization of electrochemical oxidation reactor for organic pollutants.
(1)电催化氧化技术处理实际化工废水的研究
使用二维或三维电极反应器对某炼油厂的反渗透浓缩水和某氯醇法生产环氧丙烷过程中产生的皂化废水进行处理,取得了良好效果。反应器型式、电流密度、通电时间、电解液流速、电极材料和相对面积等都是影响处理效果的重要因素,但实际有机废水的处理过程中存在能耗高、电极“堵塞”、有机污染物的降解机理及降解过程动力学等问题,需要我们开展相关的电化学工程理论研究。
(2)有机污染物的电催化氧化降解动力学的研究
研究了有机物草酸在采用活性Ti/IrO2-Ta2O5电极为阳极的圆柱形电化学反应器中的整个降解过程。由于有机污染物的电催化降解包含两条都属于“直接电氧化”的反应路径,建立了能描述整个降解过程的瞬时电流效率与溶液本体有机物浓度的关系式,并通过有机物降解实验对上述模型进行了验证,实验结果与模型计算结果一致。另外,还通过参数分析探讨了有机污染物在电极表面直接电催化氧化降解的两条路径的竞争关系。
研究了氯离子存在条件下,使用Ti/IrO2-Ta2O5阳极时,有机物草酸在圆柱形电化学反应器中的间接电氧化降解过程。有机物在该体系中的电催化降解是典型的电化学反应-化学反应串联过程。当氯离子的添加浓度太少时,反应体系发生的主要是直接电氧化或氧气析出反应,电流效率很低。只有当有机废水中含有适量的氯离子时,间接电氧化才能体现出明显的降解效果。降解过程的pH值变化表明,反应开始阶段电解液呈强酸性不变,直到草酸的去除率达到80%以上,反应体系的pH值才有明显的增大。
草酸在圆柱形电化学反应器中的间接电氧化过程符合一级反应动力学规律。由于Hatta准数的大小在0.1左右,草酸与活性氯的反应主要发生在溶液本体和电极表面扩散层／反应层中,这为电化学反应器的选型、设计和优化提供了有用的信息。
(3)电化学反应器的流动特性和传质性能研究
使用常见的脉冲响应技术测定了实验室规模的滤压式电化学反应器的停留时间分布。停留时间分布的拖尾现象说明反应器存在“死区”,随着流速的增大,拖尾现象减弱；在两条流动路径的假设基础上建立的组合流动模型可以较好的描述具有双峰现象的停留时间分布。其中路径1是指穿过电极的流体,路径2是指是沿着滤压式电化学反应器的内部壁面流动的流体。组合流动模型的参数受流速和电极结构的影响。与具有较大平均停留时间的路径2有关的模型参数受流速的影响较大,这是由于反应器中的流体流动起强化对流和减小水力边界层厚度的作用,而电极结构对流动性能的影响体现在路径1上。
用极限电流法对竖直放置的管式电极反应器的平均传质系数的测定结果表明,反应器的平均传质系数随着入口扩大系数的减小而增大,但与入口流道的数量和分布无关。CFD模拟结果解释了传质提高的原因：当入口扩大系数减小时,反应器入口的下游出现了射流,并且由于射流的卷吸和扩展,电解液的湍流程度加剧,起到了强化传质的作用。
网状电极对管式平行电极反应器传质强化的研究表明,使用网状电极后,电解液的流动模式由平板电极的层流变为湍流,电极表面的水力边界层厚度减小网状电极通过强化对流提高了管式平行电极反应器的传质性能。
CFD数值模拟结果与实验结果的比较表明,CFD模拟过程中所做出的关于Nernst扩散层的假设是正确的。CFD数值模拟方法可以弥补实验条件的不足,对电化学反应器单相流动的数值模拟能够较好的反映和预测反应器的传质性能。
本论文基于有机污染物电化学降解机理,克服了已有文献中按照反应控制步骤分段讨论的缺点,建立了能描述整个降解过程的数学模型；并针对电催化氧化技术对反应器的特殊要求,提出了研究电极附近液层特征的新方法,完善了相关的电化学工程基础理论,为用于有机废水处理的电化学反应器的的设计和优化提供了有效的信息。
Electrochemical oxidation means conversion or destruction of organic substrates in wastewater under the influence of the electric field. It can take place through two different oxidation mechanisms:(1) direct anodic oxidation, where the pollutants are destroyed at the anode surface;(2) indirect oxidation where a mediator is electrochemically generated to carry out the oxidation. Electrochemical oxidation method is a perspective technology for organic wastewater treatment because its advantages such as free secondary pollution, environmental compatibility, mild reaction conditions, easy automation, etc. However, the practical application of this technology still faces some urgent problems such as low current efficiency and weak mass transfer performance. The purpose of this thesis is accelerating the industrialization of the "green" electrochemical wastewater treatment technology. Aiming to the above existing problems, we make a series of fundamental engineering researches on the electrochemical reaction kinetics for organic pollutant degradation, flow characteristic and mass transport process in the electrochemical reactor.
(1) Application of electrochemical oxidation technology for practical chemical produce wastewater treatment
Good effect was achieved by the treatment of reverse osmosis concentrated wastewater from refinery and saponification wastewater from propylene oxide production using two-dimension or three-dimension electrochemical reactor. Type of electrochemical reactor, current density, electrolysis time, electrolyte flow rate, electrode materials and their opposite area were important factors that effects the organic pollutant degradation results. However, some problem such as high energy consumption, block of three-dimension electrode, mechanism and kinetic of organic degradation was appeared. The solution of these problems needs our theoretical study about electrochemical engineering.
(2) Kinetic of organic electrochemical oxidation
The whole degradation process of oxalic acid in a cylindrical electrochemical reactor with active Ti/IrO2-Ta2O5 anode was studied. The relation between instantaneous current efficiency and organic concentration was established base on the two paths for direct electrochemical oxidation, and the kinetic model was verified by experiments. The experimental results are consistent with the established kinetic model. Furthermore, the competition between the two paths was explored with model parameter analysis.
The indirect electrochemical oxidation process of oxalic acid under the condition of chloride ion existence was studies. Organic degradation in this system is a typical series electrochemical-chemical process. When the amount of chloride ion is too little, the current efficiency is very low, that is because the reaction system occurs mainly direct electrochemical oxidation or oxygen generation. Only the indirect electro-oxidation reflects significant degradation effect when organic wastewater containing some amount of chloride ions. The variety of pH showed that, electrolyte maintains strong acid until the removal percentage of oxalic acid larger than 80%.
The indirect electrochemical degradation of oxalic acid is agreed with the role of first order reaction kinetics. The value of the Hatta number, which approximated to 0.1 indicates that, most of the reactions between the organic and the active chlorine take place both in the bulk solution and in the reaction zone near the anode.
(3) Flow characteristics and mass transfer performance of electrochemical reactor
The residence time distribution in a laboratory scale filter-press type electrochemical reactor was determined using common impulse-response technique. The phenomenon of tailing indicated the existence of "dead zone" in the reactor. This phenomenon reduces and even disappears at high flow rate. The two peaks for RTD curves can be well expressed by the composite flow model about two paths. And path-1 is the flow moves through the holes of the electrode; path-2 is the fluid flows along the internal walls of the filter-press type electrochemical reactor. The effect of flow rate and electrode configuration on the flow model parameters was investigated. Because of the enhancement of convection and the decrease of boundary layer thickness, the parameters for path-2 are significantly influenced by flow rate. And the model parameters of path-1 reflected the effect of electrode configuration on the total flow characteristics.
Determination of mass transfer coefficient for vertical tubular electrochemical reactor with parallel electrodes has shown that mass transfer coefficient increased with the decrease of expansion ratio, but it is little related to distribution and amount of circular arranged holes in baffles. The CFD simulation result showed the appearance of jet flow downstream the sudden expansion entrance. In effect, the high rates of shear induce the rotation of the solution and small eddies are formed, the level of electrolyte turbulence enhances and plays a role in improving mass transfer performance.
The study of mass transfer enhancement for mesh electrode in a tubular electrochemical reactor indicated that, the insert of mesh electrode has changed the flow pattern from laminar to turbulence, and the thickness of boundary layer gets smaller. This leads to the improvement of force convection and enhancement of mass transfer performance.
The comparison of CFD simulation and experimental results showed that the assumption related to Nernst diffusion layer is correct. The single-phase CFD simulation method is a useful tool to describe the flow characteristic and predict the local mass transfer performance in such an electrochemical reactor.
In this thesis, a kinetic model described the whole degradation process of organic pollutants was established based on the mechanism of electrochemical oxidation. And this model overcomes the shortage of former literatures discussed by control steps. Furthermore, according to the special requirements for electrochemical oxidation reactor, we have raised a novel method investigating the electrolyte layer near the electrode. These studies have provided some useful information on the selection, design and optimization of electrochemical oxidation reactor for organic pollutants.
引文
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