废水中难降解有机物在不锈钢不溶性电极上电化学行为研究
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摘要
对难生物降解的有机废水处理,电催化法是一种很有发展前景的高级氧化法。本课题组研发的不锈钢不溶性电极及其电催化反应器可大大降低设备成本和提高电催化效率,已在制药废水等难降解废水处理和回用中成功应用。为扩大电催化法的应用范围和进一步提高效能,有必要从理论上更深入地研究废水中的难降解有机物在不锈钢不溶性电极上的电化学行为。
以不锈钢不溶性电极为工作电极,采用动电位扫描法研究了电解质溶液中抗生素等有机物在电极上的电化学行为,发现在析氧电位以下会出现一个电流峰及相应的特征电位；特征电位值几乎与有机物浓度无关,对于所选用多种有机物,特征电位值保持稳定,仅随着扫描速度的加快和温度的下降而正移。在28℃,扫描速度2 mV/s的条件下,该特征电位从起始至终止的范围为600-1050 mV,出现电流峰值的电位为920 mV左右。有机物浓度越大,特征电位所对应的电流峰越高；当电解质溶液中不含有机物时,电流峰及相应的特征电位消失。当用多种有机物进行试验时,也发现了类似规律。根据电位值不因所选用有机物种类而改变等现象推测,该电位值可能与羟基自由基的生成有关。该特征电位对电解质溶液中的有机物定量、羟基自由基的跟踪及抑制电化学副反应有重大意义。
然而,当以不锈钢基不溶性电极为阳极处理苯酚废水时,发现在电极表面形成黄褐色薄膜。通过阳极极化,循环伏安,恒电流电解氧化等手段,对成膜行为进行了研究,表明阳极电极电位为1.45 V时反应效率最高,此时阴阳极板间电压为2.5 V。通过红外光谱分析,证明了成膜产物为聚苯酚,产物中包含有大量羟基。聚苯酚分子的长链结构不仅有对位取代形成长链,而且会发生邻位取代形成侧链。利用聚苯酚产物部分溶于四氢呋喃的特性,对聚苯酚薄膜在使用四氢呋喃进行溶解清洗前后的结构进行SEM分析对比,提出苯酚聚合生长的线性与平面模型。中性水溶液条件下,聚苯酚主要按照平面生长模型,平行于电极表面逐层生长；每层聚苯酚中,以某些活性中心为聚合引发点,形成直径为50纳米的不规则薄片单元,薄片单元之间通过低聚物与未聚合单体相互连接。
研究了聚合物膜生成后对电极过程的作用,发现聚苯酚成膜对于不锈钢在3.5%氯化钠介质中耐点蚀能力有显著提升。在相同反应条件下将部分苯酚换作苯胺,共同电聚合成膜,当溶液成分为0.09 mol/L苯酚和0.01mol/L苯胺时,电聚合成膜的抗点蚀能力最强,其点蚀电位上升至0.382 V,具有最佳耐氯离子腐蚀能力。通过红外光谱对苯酚聚合物与苯酚苯胺共聚物进行分析比较,证明苯酚苯胺共聚产物中存在聚苯胺结构,并解释耐蚀能力增强的原因。与聚苯酚相比,共聚产物中存在更多芳环的1,2,4取代现象,说明其中生成了更多侧链,使得产物成膜的结合更紧密。利用聚苯酚和聚苯胺在四氢呋喃中的部分溶解特性,使用SEM分析比较聚苯酚膜和苯酚苯胺共聚合膜表面形貌。0.09 mol/L苯酚和0.01 mol/L苯胺溶液下生成的苯酚苯胺共聚膜,由网状聚苯胺构成空间骨架,其间填充聚苯酚,形成不易开裂且结构紧密的聚合物膜,提升成膜耐氯离子腐蚀能力。
对电聚合处理苯酚废水的进一步研究发现,苯酚浓度越高电聚合速率越快,但更高浓度的苯酚导致处理效果的下降,选用0.002 mol/L作为待处理苯酚废水的浓度。槽电压在2.9-3.1 V范围内处理效果较好,为尽可能减少副反应,选取2.9 V为处理槽电压。经过电化学处理12h后,苯酚电聚合成膜产物整体脱落,意味着苯酚基本从水中被除去。苯酚浓度由0.002 mol/L变为0.087 mmol/L,去除率95.6%,化学需氧量由500 mg/L变为COD为68 mg/L,去除率86.5%。在12h的处理过程中的平均电流效率为60.36%,处理每吨0.002 mol/L苯酚废水耗能6.96 kwh,能耗和处理成本较电催化氧化法有较大下降。
As one of advanced oxidation processes, electrocatalysis treatment was developing quickly in refractory organic wastewater treatment. Our reaearch team developed stainless steel insoluble electrodes and electrocatalysis reactors, which had been applied successfully in pharmaceutical wastewater treatment and reuse. For expanding the application range of electrocatalysis in wastewater treatment and improving the current efficiency, it was necessary to further study electrochemical behavior of refractory organics on stainless steel insoluble electrodes.
Using stainless steel as the working electrode, the electro-catalysis process of organic compound in electrolyte solution was studied through the potentiodynamic scanning, and a characteristic electrode potential and current maximum was observed below oxygen evolution. The concentration and the choosed species of the organic compound, the scanning speed and the temperature did not affect the form of the characteristic electrode potential, which moved towards positive with the raising of the scanning speed and the falling of the temperature. At 28℃and the scanning speed of 2 mV/s, the characteristic electrode potential exists between 600 to 1050 mV, the maximum of the current appears at the electrode potential of 920 mV. The current maximum at the characteristic electrode potential became higher with the concentration of the organic compound, and the current maximum disappeared when the solution did not contain organics. Since the characteristic electrode potential was independent to the concentration and the choosed species of the organic compound in the wastewater, the characteristic electrode potential should be the synthesis of the hydroxyl radical. The characteristic electrode potential had great significance for the rapid detection of organics in wastewater, real time trace of the hydroxyl radical, and the reduction of electrochemical side reactions in wastewater treatment.
However, a yellow brown polyphenol coating was generated on stainless steel electrode surface, when anodic oxidation treatment of phenol wastewater was carried out using stainless steel based insoluble electrode. The coating formation was discussed by linear scanning, cyclic voltammetry and constant current process. The anodic electrode potential of 1.45V was the best condition for good reaction efficiency, while the bath voltage between anode and cathode was about 2.5V. Coating product was analyzed by IR, and the chemical structure was proved to be polyphenol. Polyphenol film contained linear chain and side chain, in which large number of substitutine hydroxyl existed. Making use of part solubility of polyphenol in tetrahydrofuran, the micro structure of polyphenol film was analyzed and compared between original and tetrahydrofuran cleaned polymer coating by SEM micrograph, by which linear mode and plane mode of polyphenol growth was summarized. In neutral media major part of polyphenol grew following the flake-layer mode, layer by layer, parallel to the electrode surface. Polyphenol growth began at some active sites on electrode or polymer, and formed nearly round flakes with 50nm diameter parallel to the anode plane. Flakes connected each other through low polymer and unpolymerized phenol, and formed a layer.
The electrochemical process of coating covered electrode was studied, and the polyphenol coating notablely enhanced the pit corrosion resistance of 304 stainless steel in 3.5% sodium chloride solution. Keeping the sum of phenol and aniline concentration, the phenol-aniline copolymer coating was synthesized at the same electrochemical condition on 304 stainless steel anodes. When the solution contained 0.09 mol/L phenol and 0.01 mol/L aniline, the copolymer coating achieved the best pit corrosion resistance, while the pit corrosion potential in 3.5% sodium chloride increased to 0.382 V. Through the infrared spectrum comparison of phenol polymer and phenol-aniline copolymer coatings, the polyaniline structure was proved in the copolymer, and the reasons of the corrosion resistance enhancement were discussed. There was more 1,2,4-ring substitution occurring in phenol-aniline copolymer than polyphenol, which caused more side chains generated during the electropolymerization and a much more compact coating product. Taking advantage of the part solubility of polyphenol and polyaniline in THF, SEM was used to analyze the microstructure of phenol-aniline copolymer coating, with the comparison of polyphenol coating. In the copolymer synthesized in the solution contained 0.09 mol/L phenol and 0.01 mol/L aniline, the bifurcate network structure was observed, which was mainly composed from polyaniline, with other copolymer, mainly polyphenol, filling the interspaces. The network structure in copolymer coating restrained the growth of cracks, enhanced the connection between layers, synthesied the copolymer coating, which raised the pit corrosion resistance against chloride ions.
In further research, rapid electropolymerization rate was observed in higher phenol concentration. However, the phenol removel effect became lower in much higher phenol concentration, so the concentration of phenol wastewater in electropolymerization treatment was fixed at 0.002 mol/L. The COD removal efficiency was better between the bath voltages of 2.9 V and 3.1 V,2.9 V was chosen for the less oxygen evolution and energy consumption. After the 12-hour electropolymerization treatment, the polymer coating cracked and wholly dropped from the stainless steel base, which meant the exhausting of phenol in wastewater. The phenol concentration became 0.087mmol/L from 0.002 mol/L, with the removal efficiency of 95.6%, and the COD became 68 mg/L from 500 mg/L, with the removal efficiency of 86.5%. During the treatment the average current efficiency was 60.36% and power consumption was 6.96 kwh/t, which showed a great decline in power consumption and treatment cost comparing with electrocatalysis treatment.
以不锈钢不溶性电极为工作电极,采用动电位扫描法研究了电解质溶液中抗生素等有机物在电极上的电化学行为,发现在析氧电位以下会出现一个电流峰及相应的特征电位；特征电位值几乎与有机物浓度无关,对于所选用多种有机物,特征电位值保持稳定,仅随着扫描速度的加快和温度的下降而正移。在28℃,扫描速度2 mV/s的条件下,该特征电位从起始至终止的范围为600-1050 mV,出现电流峰值的电位为920 mV左右。有机物浓度越大,特征电位所对应的电流峰越高；当电解质溶液中不含有机物时,电流峰及相应的特征电位消失。当用多种有机物进行试验时,也发现了类似规律。根据电位值不因所选用有机物种类而改变等现象推测,该电位值可能与羟基自由基的生成有关。该特征电位对电解质溶液中的有机物定量、羟基自由基的跟踪及抑制电化学副反应有重大意义。
然而,当以不锈钢基不溶性电极为阳极处理苯酚废水时,发现在电极表面形成黄褐色薄膜。通过阳极极化,循环伏安,恒电流电解氧化等手段,对成膜行为进行了研究,表明阳极电极电位为1.45 V时反应效率最高,此时阴阳极板间电压为2.5 V。通过红外光谱分析,证明了成膜产物为聚苯酚,产物中包含有大量羟基。聚苯酚分子的长链结构不仅有对位取代形成长链,而且会发生邻位取代形成侧链。利用聚苯酚产物部分溶于四氢呋喃的特性,对聚苯酚薄膜在使用四氢呋喃进行溶解清洗前后的结构进行SEM分析对比,提出苯酚聚合生长的线性与平面模型。中性水溶液条件下,聚苯酚主要按照平面生长模型,平行于电极表面逐层生长；每层聚苯酚中,以某些活性中心为聚合引发点,形成直径为50纳米的不规则薄片单元,薄片单元之间通过低聚物与未聚合单体相互连接。
研究了聚合物膜生成后对电极过程的作用,发现聚苯酚成膜对于不锈钢在3.5%氯化钠介质中耐点蚀能力有显著提升。在相同反应条件下将部分苯酚换作苯胺,共同电聚合成膜,当溶液成分为0.09 mol/L苯酚和0.01mol/L苯胺时,电聚合成膜的抗点蚀能力最强,其点蚀电位上升至0.382 V,具有最佳耐氯离子腐蚀能力。通过红外光谱对苯酚聚合物与苯酚苯胺共聚物进行分析比较,证明苯酚苯胺共聚产物中存在聚苯胺结构,并解释耐蚀能力增强的原因。与聚苯酚相比,共聚产物中存在更多芳环的1,2,4取代现象,说明其中生成了更多侧链,使得产物成膜的结合更紧密。利用聚苯酚和聚苯胺在四氢呋喃中的部分溶解特性,使用SEM分析比较聚苯酚膜和苯酚苯胺共聚合膜表面形貌。0.09 mol/L苯酚和0.01 mol/L苯胺溶液下生成的苯酚苯胺共聚膜,由网状聚苯胺构成空间骨架,其间填充聚苯酚,形成不易开裂且结构紧密的聚合物膜,提升成膜耐氯离子腐蚀能力。
对电聚合处理苯酚废水的进一步研究发现,苯酚浓度越高电聚合速率越快,但更高浓度的苯酚导致处理效果的下降,选用0.002 mol/L作为待处理苯酚废水的浓度。槽电压在2.9-3.1 V范围内处理效果较好,为尽可能减少副反应,选取2.9 V为处理槽电压。经过电化学处理12h后,苯酚电聚合成膜产物整体脱落,意味着苯酚基本从水中被除去。苯酚浓度由0.002 mol/L变为0.087 mmol/L,去除率95.6%,化学需氧量由500 mg/L变为COD为68 mg/L,去除率86.5%。在12h的处理过程中的平均电流效率为60.36%,处理每吨0.002 mol/L苯酚废水耗能6.96 kwh,能耗和处理成本较电催化氧化法有较大下降。
As one of advanced oxidation processes, electrocatalysis treatment was developing quickly in refractory organic wastewater treatment. Our reaearch team developed stainless steel insoluble electrodes and electrocatalysis reactors, which had been applied successfully in pharmaceutical wastewater treatment and reuse. For expanding the application range of electrocatalysis in wastewater treatment and improving the current efficiency, it was necessary to further study electrochemical behavior of refractory organics on stainless steel insoluble electrodes.
Using stainless steel as the working electrode, the electro-catalysis process of organic compound in electrolyte solution was studied through the potentiodynamic scanning, and a characteristic electrode potential and current maximum was observed below oxygen evolution. The concentration and the choosed species of the organic compound, the scanning speed and the temperature did not affect the form of the characteristic electrode potential, which moved towards positive with the raising of the scanning speed and the falling of the temperature. At 28℃and the scanning speed of 2 mV/s, the characteristic electrode potential exists between 600 to 1050 mV, the maximum of the current appears at the electrode potential of 920 mV. The current maximum at the characteristic electrode potential became higher with the concentration of the organic compound, and the current maximum disappeared when the solution did not contain organics. Since the characteristic electrode potential was independent to the concentration and the choosed species of the organic compound in the wastewater, the characteristic electrode potential should be the synthesis of the hydroxyl radical. The characteristic electrode potential had great significance for the rapid detection of organics in wastewater, real time trace of the hydroxyl radical, and the reduction of electrochemical side reactions in wastewater treatment.
However, a yellow brown polyphenol coating was generated on stainless steel electrode surface, when anodic oxidation treatment of phenol wastewater was carried out using stainless steel based insoluble electrode. The coating formation was discussed by linear scanning, cyclic voltammetry and constant current process. The anodic electrode potential of 1.45V was the best condition for good reaction efficiency, while the bath voltage between anode and cathode was about 2.5V. Coating product was analyzed by IR, and the chemical structure was proved to be polyphenol. Polyphenol film contained linear chain and side chain, in which large number of substitutine hydroxyl existed. Making use of part solubility of polyphenol in tetrahydrofuran, the micro structure of polyphenol film was analyzed and compared between original and tetrahydrofuran cleaned polymer coating by SEM micrograph, by which linear mode and plane mode of polyphenol growth was summarized. In neutral media major part of polyphenol grew following the flake-layer mode, layer by layer, parallel to the electrode surface. Polyphenol growth began at some active sites on electrode or polymer, and formed nearly round flakes with 50nm diameter parallel to the anode plane. Flakes connected each other through low polymer and unpolymerized phenol, and formed a layer.
The electrochemical process of coating covered electrode was studied, and the polyphenol coating notablely enhanced the pit corrosion resistance of 304 stainless steel in 3.5% sodium chloride solution. Keeping the sum of phenol and aniline concentration, the phenol-aniline copolymer coating was synthesized at the same electrochemical condition on 304 stainless steel anodes. When the solution contained 0.09 mol/L phenol and 0.01 mol/L aniline, the copolymer coating achieved the best pit corrosion resistance, while the pit corrosion potential in 3.5% sodium chloride increased to 0.382 V. Through the infrared spectrum comparison of phenol polymer and phenol-aniline copolymer coatings, the polyaniline structure was proved in the copolymer, and the reasons of the corrosion resistance enhancement were discussed. There was more 1,2,4-ring substitution occurring in phenol-aniline copolymer than polyphenol, which caused more side chains generated during the electropolymerization and a much more compact coating product. Taking advantage of the part solubility of polyphenol and polyaniline in THF, SEM was used to analyze the microstructure of phenol-aniline copolymer coating, with the comparison of polyphenol coating. In the copolymer synthesized in the solution contained 0.09 mol/L phenol and 0.01 mol/L aniline, the bifurcate network structure was observed, which was mainly composed from polyaniline, with other copolymer, mainly polyphenol, filling the interspaces. The network structure in copolymer coating restrained the growth of cracks, enhanced the connection between layers, synthesied the copolymer coating, which raised the pit corrosion resistance against chloride ions.
In further research, rapid electropolymerization rate was observed in higher phenol concentration. However, the phenol removel effect became lower in much higher phenol concentration, so the concentration of phenol wastewater in electropolymerization treatment was fixed at 0.002 mol/L. The COD removal efficiency was better between the bath voltages of 2.9 V and 3.1 V,2.9 V was chosen for the less oxygen evolution and energy consumption. After the 12-hour electropolymerization treatment, the polymer coating cracked and wholly dropped from the stainless steel base, which meant the exhausting of phenol in wastewater. The phenol concentration became 0.087mmol/L from 0.002 mol/L, with the removal efficiency of 95.6%, and the COD became 68 mg/L from 500 mg/L, with the removal efficiency of 86.5%. During the treatment the average current efficiency was 60.36% and power consumption was 6.96 kwh/t, which showed a great decline in power consumption and treatment cost comparing with electrocatalysis treatment.
引文
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