不溶性催化电极与电催化反应器的制备及其对废水中有机物、菌藻和纤维素类物质的催化降解作用
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摘要
随着世界各国的经济发展、人口增加,环境污染、能源紧缺成为当前人类面临的严重问题。电催化水处理技术由于具有清洁、无二次污染、氧化彻底等优点而受到科学工作者的关注,成为解决环境污染、能源紧缺的新的途径。电催化技术的核心在于功能电极材料的研制,高性能电极材料的研究成为电化学科学的前沿课题。目前应用最广泛、性能较高的电极材料仍然是钛基形稳阳极,但是由于钛金属较为昂贵,限制了钛基形稳阳极在氯碱工业以外的其它行业的应用。本工作采用不锈钢作为电极的基体金属,制备不锈钢基不溶性催化阳极,并将其应用于废水中有机物和菌藻的去除；并对钛基形稳阳极进行改性研究,将其应用于木质纤维素电催化降解。
用溶胶-热分解的方法制备了不锈钢基SnO2-CeO2阳极,电极制备的优化条件为：涂刷次数20次,烘干温度100℃,热氧化气氛为空气,温度550℃,时间60min。经扫描电镜表征,所制得的电极催化涂层呈现形稳阳极特有的“泥裂”形貌。涂层无纵向贯穿的裂纹,与基体结合紧密。制备的SnO2-CeO2电极的溶胶及其热分解生成的涂层均具有致密的结构,有效阻止空气中的O2到达不锈钢基体,防止制备过程中不锈钢基体氧化腐蚀、保证了SnO2和SnO2-CeO2膜与基体紧密结合。循环伏安测试表明不锈钢基SnO2-CeO2电极具有良好的电化学稳定性,析氧电位高(1.6 V vs.SCE),具有优良的抗氧化能力。采用不锈钢基SnO2-CeO2电极作为阳极,电催化氧化处理常规化学絮凝法处理效果较差的印染工业废水,5 V电压下,电催化2 min,色度去除率达到92.8%, COD去除率达到58.2%,从而证明该电极具有优异的电催化氧化性能。
采用不锈钢基SnO2-CeO2电极极作为阳极,不锈钢电极作为阴极,对模拟抗生素废水进行降解研究,结果表明降解效果显著。在5V电压下电催化氧化5min,COD去除率达到21.3%,氧化20min,去除率达到33.2%；确定最佳的电极间距为10mm。采用水杨酸作为羟基自由基的捕捉剂,验证了电催化过程中有羟基自由基生成,并由此可以证明电催化降解有机物主要是由于产生具有强氧化性的羟基自由基。且不锈钢基SnO2-CeO2电极对青霉素的降解过程遵循表观一级反应动力学规律。针对不锈钢电极以及不锈钢基涂层电极在电催化氧化降解有机物过程中出现的与降解效果密切相关的特征电位,开发了特征电位跟踪系统。该系统能够有效追踪特征电位,并通过信号输出控制电催化电源的工作参数输出,有效保证电催化反应始终处于最佳工作状态。
相同条件下添加三维粒子电极提高电催化降解对模拟抗生素废水COD的去除率3.3至6.8个百分点。对作为三维粒子电极的活性炭进行饱和吸附-电催化氧化再生研究,结果表明电催化氧化对经吸附饱和的活性炭粒子再生效果显著。3V电压下仅电催化氧化3 min,活性炭再生率即达33%,电催化10min,再生率达到50%。而5V电压下仅氧化3分钟,再生率即达53%。而在5V电压下,电催化氧化15 min,对于经12次吸附饱和并电催化再生的活性炭的再生率仍然达到78%。由此得出结论,用于电催化氧化反应的粒子电极,在处理有机废水的过程中,在持续的电场作用下,粒子电极表面及内部孔道能够持续得以氧化再生。
采用不锈钢基SnO2-Ce02电极极作为阳极,不锈钢电极作为阴极,对高浓度含菌废水进行灭菌和去除钙镁离子研究。发现电催化氧化具有优异的灭菌效果,在3V电压下,电催化5min,灭菌率已达89.65%。并且灭菌率随着电压的升高而迅速提高,当电压为5V时,电催化5min,灭菌率即达到99.17%。经过电催化灭菌的模拟循环冷却水放置2天后细菌总数仍保持在较低水平(小于原水1%),放置4天细菌数仍未超过原水细菌数。电催化处理同时具有去除水中钙镁离子的功能,在3V下对总硬度为4mmol／L的模拟废水进行电催化处理30min,总硬度去除率达到50.8%,去除效果显著。
制备钛基SnO2-CeO2电极,并将其作为阳极和阴极材料,首次将电催化引入纤维素水解过程,利用电催化的氧化性能提高纤维素的水解产率,提高降解速率。为了便于木质纤维素的溶解,提高木质纤维素的降解效果,采用两步酸法,即先将木质纤维素进行浓酸水解,之后再稀释进行电催化稀酸水解。木质纸纤维在浓酸水解最佳的反应温度为50℃,反应时间15min,液固比2：1为最佳液固比。稀酸条件下电催化降解纤维素最佳硫酸浓度为3%,电压4V,反应时间为60mmin。在此条件下获得的还原糖得率为51.7%,已超过直接水解2h的得率。木质纤维素在水解前后的SEM和XRD测试表明电催化能够有效破坏木质纤维素的晶体结构,有效提高木质纤维素的水解速度和还原糖得率。
设计并制作单台处理能力为40m3／d的电催化废水处理反应器,并将其应用于电催化降解印染废水中试现场处理研究,对于COD值在200mg/L以下的经过生化处理的印染废水尾水,仅处理5min,废水的COD即可达到国家一级排放标准(<100mg/L),吨水能耗仅为0.9KW·h-1.3KW·h；对于COD值大于2000mg/L的未经生化处理的印染废水原水和化工废水,处理5min,COD去除率达到35%以上,显示了较高的去处效率,能量消耗低、具有良好的经济价值和应用前景。
With economic development, population growth and environmental pollution, energy shortage has become serious problems for humanity to face in the world. Electro-catalytic oxidation technology of wastewater has been concerned by scientists due to its cleaning, no secondary pollution, oxidation and other advantages. And this technology is one of new methods to resolve environmental pollution and energy shortage. The preparation of electro-catalytic function electrode materials is the core and cutting-edge issue of electro-catalytic technology. Currently dimensionally stable anode (DSA) based on Ti is the most widely used and high performance electrode material in the world. But titanium is very expensive, which limits DSA electrode been used in the other fields except chlor-alkali industry. This work involves the preparation of insoluble anode which based on stainless steel (SS), and the modification of DSA electrode based on titanium, and electro-catalytic degradation of organic matter, bacteria,algae,and lignocellulose by using these electrodes.
The SnO2-CeO2 on stainless steel (SS/SnO2-CeO2) was prepared by high temperature thermal decomposition. The experimental results show that the optimum conditions for preparing the electrodes as followed:the coating needs to be brushed 20 times, drying temperature is 100℃, thermal decomposition temperature and time is 550℃and 60 min in air. Characterized by scanning electron microscopy, though the prepared electrodes show the unique "mud crack" look for DSA electrodes, cracks are very shallow and coating closely attaches to the substrate. The structure of sol and coating is very compact and effectively prevents O2 to reach and oxidize stainless steel substrate in the process of thermal decomposition. CV analysis shows that the SS/SnO2-CeO2 electrode behaves high oxygen evolution potential (1.6V vs. SCE), good electrochemical stability, and excellent antioxidant. SS/ SnO2-CeO2 electrodes were used as anodes to oxidize a dying wastewater which was difficult to treat with qualified by conventional chemical flocculation, and the results showed color removal of 92.8% and COD removal of 58.32% with 5V voltage in 2 min, which proved the electrode had excellent performance of electro-catalytic oxidation.
When SS/SnO2-CeO2 electrodes were used as anodes and SS as cathodes to oxidize activated carbon which saturated adsorption by phenol, the results showed the regeneration rate was 33% with only 3V voltage in 3min, and the recycling rate reached 53% with 5V in 3min. The regeneration rate of activated carbon which was saturated adsorption and oxidizing 12 times was activated carbon which was saturated adsorption and oxidizing 12 times was still 78%. At the same time it can be concluded that the surface and internal of particle electrode can continue to be recycled with effect of continuous electric field during electro-catalytic oxidation of organic wastewater.
When SS/SnO2-CeO2 electrodes were used as anodes and SS as cathodes to oxidize simulated antibiotic wastewater, the results showed that COD removal of 24.1% with using particle electrode under 5V in 5min, and the COD removal reached to 38.7% for oxidation 10min. In addition, the optimal electrode spacing was 10mm. It was verified that there were hydroxyl free radicals generated in the electro-catalytic process by using salicylic acid as the capture agent. So organic was degraded mainly by hydroxyl free radicals in the electro-catalytic process.
When SS/SnO2-CeO2 electrodes were used as anodes and SS as cathodes to oxidize high concentrations of bacterial wastewater, the results displayed that sterilization rate reached 89.65% with only 3V in 5min. The sterilization rate increased rapidly with the voltage increase, when the voltage was 5V,the sterilization rate had reached 99.17% for 5 min. The total number of bacteria remained at low levels(less than 1% of the raw water) for 2 days after electro-catalytic sterilization, and the total number of bacteria still was not more than the number of the raw water. Calcium and magnesium can be removed by electro-catalysis, too. The total hardness removal rate reached 50.8% for total hardness 4 mmol/L water with 3V in 30min.
A system of tracking characteristic potential was developed. The characteristic potential can be found in the electro-catalytic process by using SS and coating electrodes on SS. The system can track the characteristic potential effectively, control the operating parameters of electro-catalytic power output, and ensure that catalytic reaction always in the best working condition.
Ti/SnO2-CeO2 electrode was prepared and used as anode and cathode to degrade cellulose and increase the hydrolysis yield. Two-step acid method was used to increase the dissolution and degradation rate of lignocellulose. Lignocellulose was concentrated acid hydrolysis and then diluted to electro-catalytic degaration. The optimum condition of corrugated paper fiber concentrated acid hydrolysis is:50℃,15min, the ratio 2:1 of liquid volume to solid weight. And the optimum condition of electro-catalytic degradation cellulose in dilute acid is:3% sulfuric acid concentration,4V voltage,60min. The reducing sugar yield is 51.7% and more than the yield of direct hydrolysis for 2 hours. SEM and XRD tests of lignocellulose showed that the crystal structure of paper fiber was destroyed seriously, and electro-catalysis can improve the degradation speed of lignocellulose and reducing sugar yield.
A electro-catalytic reactor with a single processing capacity of 40m3/d wastewater was designed and produced. And it was applied to electro-catalytic degradation of dying wastewater. The COD value of dying water with COD <200mg/L decreased to be less than 100 mg/L and meet the national discharge standard. Consumption of a ton of water was only 0.9-1.3 kWh. The COD removal rates of dying water and chemical water with COD>200mg/L were more than 35% in 5min. Consumption of a ton of water was only 1.1-1.7 kWh for electro-catalytic treatment of wastewater, so the method behaved good economic value and application prospect.
用溶胶-热分解的方法制备了不锈钢基SnO2-CeO2阳极,电极制备的优化条件为：涂刷次数20次,烘干温度100℃,热氧化气氛为空气,温度550℃,时间60min。经扫描电镜表征,所制得的电极催化涂层呈现形稳阳极特有的“泥裂”形貌。涂层无纵向贯穿的裂纹,与基体结合紧密。制备的SnO2-CeO2电极的溶胶及其热分解生成的涂层均具有致密的结构,有效阻止空气中的O2到达不锈钢基体,防止制备过程中不锈钢基体氧化腐蚀、保证了SnO2和SnO2-CeO2膜与基体紧密结合。循环伏安测试表明不锈钢基SnO2-CeO2电极具有良好的电化学稳定性,析氧电位高(1.6 V vs.SCE),具有优良的抗氧化能力。采用不锈钢基SnO2-CeO2电极作为阳极,电催化氧化处理常规化学絮凝法处理效果较差的印染工业废水,5 V电压下,电催化2 min,色度去除率达到92.8%, COD去除率达到58.2%,从而证明该电极具有优异的电催化氧化性能。
采用不锈钢基SnO2-CeO2电极极作为阳极,不锈钢电极作为阴极,对模拟抗生素废水进行降解研究,结果表明降解效果显著。在5V电压下电催化氧化5min,COD去除率达到21.3%,氧化20min,去除率达到33.2%；确定最佳的电极间距为10mm。采用水杨酸作为羟基自由基的捕捉剂,验证了电催化过程中有羟基自由基生成,并由此可以证明电催化降解有机物主要是由于产生具有强氧化性的羟基自由基。且不锈钢基SnO2-CeO2电极对青霉素的降解过程遵循表观一级反应动力学规律。针对不锈钢电极以及不锈钢基涂层电极在电催化氧化降解有机物过程中出现的与降解效果密切相关的特征电位,开发了特征电位跟踪系统。该系统能够有效追踪特征电位,并通过信号输出控制电催化电源的工作参数输出,有效保证电催化反应始终处于最佳工作状态。
相同条件下添加三维粒子电极提高电催化降解对模拟抗生素废水COD的去除率3.3至6.8个百分点。对作为三维粒子电极的活性炭进行饱和吸附-电催化氧化再生研究,结果表明电催化氧化对经吸附饱和的活性炭粒子再生效果显著。3V电压下仅电催化氧化3 min,活性炭再生率即达33%,电催化10min,再生率达到50%。而5V电压下仅氧化3分钟,再生率即达53%。而在5V电压下,电催化氧化15 min,对于经12次吸附饱和并电催化再生的活性炭的再生率仍然达到78%。由此得出结论,用于电催化氧化反应的粒子电极,在处理有机废水的过程中,在持续的电场作用下,粒子电极表面及内部孔道能够持续得以氧化再生。
采用不锈钢基SnO2-Ce02电极极作为阳极,不锈钢电极作为阴极,对高浓度含菌废水进行灭菌和去除钙镁离子研究。发现电催化氧化具有优异的灭菌效果,在3V电压下,电催化5min,灭菌率已达89.65%。并且灭菌率随着电压的升高而迅速提高,当电压为5V时,电催化5min,灭菌率即达到99.17%。经过电催化灭菌的模拟循环冷却水放置2天后细菌总数仍保持在较低水平(小于原水1%),放置4天细菌数仍未超过原水细菌数。电催化处理同时具有去除水中钙镁离子的功能,在3V下对总硬度为4mmol／L的模拟废水进行电催化处理30min,总硬度去除率达到50.8%,去除效果显著。
制备钛基SnO2-CeO2电极,并将其作为阳极和阴极材料,首次将电催化引入纤维素水解过程,利用电催化的氧化性能提高纤维素的水解产率,提高降解速率。为了便于木质纤维素的溶解,提高木质纤维素的降解效果,采用两步酸法,即先将木质纤维素进行浓酸水解,之后再稀释进行电催化稀酸水解。木质纸纤维在浓酸水解最佳的反应温度为50℃,反应时间15min,液固比2：1为最佳液固比。稀酸条件下电催化降解纤维素最佳硫酸浓度为3%,电压4V,反应时间为60mmin。在此条件下获得的还原糖得率为51.7%,已超过直接水解2h的得率。木质纤维素在水解前后的SEM和XRD测试表明电催化能够有效破坏木质纤维素的晶体结构,有效提高木质纤维素的水解速度和还原糖得率。
设计并制作单台处理能力为40m3／d的电催化废水处理反应器,并将其应用于电催化降解印染废水中试现场处理研究,对于COD值在200mg/L以下的经过生化处理的印染废水尾水,仅处理5min,废水的COD即可达到国家一级排放标准(<100mg/L),吨水能耗仅为0.9KW·h-1.3KW·h；对于COD值大于2000mg/L的未经生化处理的印染废水原水和化工废水,处理5min,COD去除率达到35%以上,显示了较高的去处效率,能量消耗低、具有良好的经济价值和应用前景。
With economic development, population growth and environmental pollution, energy shortage has become serious problems for humanity to face in the world. Electro-catalytic oxidation technology of wastewater has been concerned by scientists due to its cleaning, no secondary pollution, oxidation and other advantages. And this technology is one of new methods to resolve environmental pollution and energy shortage. The preparation of electro-catalytic function electrode materials is the core and cutting-edge issue of electro-catalytic technology. Currently dimensionally stable anode (DSA) based on Ti is the most widely used and high performance electrode material in the world. But titanium is very expensive, which limits DSA electrode been used in the other fields except chlor-alkali industry. This work involves the preparation of insoluble anode which based on stainless steel (SS), and the modification of DSA electrode based on titanium, and electro-catalytic degradation of organic matter, bacteria,algae,and lignocellulose by using these electrodes.
The SnO2-CeO2 on stainless steel (SS/SnO2-CeO2) was prepared by high temperature thermal decomposition. The experimental results show that the optimum conditions for preparing the electrodes as followed:the coating needs to be brushed 20 times, drying temperature is 100℃, thermal decomposition temperature and time is 550℃and 60 min in air. Characterized by scanning electron microscopy, though the prepared electrodes show the unique "mud crack" look for DSA electrodes, cracks are very shallow and coating closely attaches to the substrate. The structure of sol and coating is very compact and effectively prevents O2 to reach and oxidize stainless steel substrate in the process of thermal decomposition. CV analysis shows that the SS/SnO2-CeO2 electrode behaves high oxygen evolution potential (1.6V vs. SCE), good electrochemical stability, and excellent antioxidant. SS/ SnO2-CeO2 electrodes were used as anodes to oxidize a dying wastewater which was difficult to treat with qualified by conventional chemical flocculation, and the results showed color removal of 92.8% and COD removal of 58.32% with 5V voltage in 2 min, which proved the electrode had excellent performance of electro-catalytic oxidation.
When SS/SnO2-CeO2 electrodes were used as anodes and SS as cathodes to oxidize activated carbon which saturated adsorption by phenol, the results showed the regeneration rate was 33% with only 3V voltage in 3min, and the recycling rate reached 53% with 5V in 3min. The regeneration rate of activated carbon which was saturated adsorption and oxidizing 12 times was activated carbon which was saturated adsorption and oxidizing 12 times was still 78%. At the same time it can be concluded that the surface and internal of particle electrode can continue to be recycled with effect of continuous electric field during electro-catalytic oxidation of organic wastewater.
When SS/SnO2-CeO2 electrodes were used as anodes and SS as cathodes to oxidize simulated antibiotic wastewater, the results showed that COD removal of 24.1% with using particle electrode under 5V in 5min, and the COD removal reached to 38.7% for oxidation 10min. In addition, the optimal electrode spacing was 10mm. It was verified that there were hydroxyl free radicals generated in the electro-catalytic process by using salicylic acid as the capture agent. So organic was degraded mainly by hydroxyl free radicals in the electro-catalytic process.
When SS/SnO2-CeO2 electrodes were used as anodes and SS as cathodes to oxidize high concentrations of bacterial wastewater, the results displayed that sterilization rate reached 89.65% with only 3V in 5min. The sterilization rate increased rapidly with the voltage increase, when the voltage was 5V,the sterilization rate had reached 99.17% for 5 min. The total number of bacteria remained at low levels(less than 1% of the raw water) for 2 days after electro-catalytic sterilization, and the total number of bacteria still was not more than the number of the raw water. Calcium and magnesium can be removed by electro-catalysis, too. The total hardness removal rate reached 50.8% for total hardness 4 mmol/L water with 3V in 30min.
A system of tracking characteristic potential was developed. The characteristic potential can be found in the electro-catalytic process by using SS and coating electrodes on SS. The system can track the characteristic potential effectively, control the operating parameters of electro-catalytic power output, and ensure that catalytic reaction always in the best working condition.
Ti/SnO2-CeO2 electrode was prepared and used as anode and cathode to degrade cellulose and increase the hydrolysis yield. Two-step acid method was used to increase the dissolution and degradation rate of lignocellulose. Lignocellulose was concentrated acid hydrolysis and then diluted to electro-catalytic degaration. The optimum condition of corrugated paper fiber concentrated acid hydrolysis is:50℃,15min, the ratio 2:1 of liquid volume to solid weight. And the optimum condition of electro-catalytic degradation cellulose in dilute acid is:3% sulfuric acid concentration,4V voltage,60min. The reducing sugar yield is 51.7% and more than the yield of direct hydrolysis for 2 hours. SEM and XRD tests of lignocellulose showed that the crystal structure of paper fiber was destroyed seriously, and electro-catalysis can improve the degradation speed of lignocellulose and reducing sugar yield.
A electro-catalytic reactor with a single processing capacity of 40m3/d wastewater was designed and produced. And it was applied to electro-catalytic degradation of dying wastewater. The COD value of dying water with COD <200mg/L decreased to be less than 100 mg/L and meet the national discharge standard. Consumption of a ton of water was only 0.9-1.3 kWh. The COD removal rates of dying water and chemical water with COD>200mg/L were more than 35% in 5min. Consumption of a ton of water was only 1.1-1.7 kWh for electro-catalytic treatment of wastewater, so the method behaved good economic value and application prospect.
引文
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