光催化—催化湿式氧化处理有机染料废水的研究
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摘要
随着现代工业的不断发展，同时产生大量有机废水，成分较为复杂，许多难降解有机污染物存在于水体中，它们毒性大，很难用常规的物化和生化方法进行处理达标排放，造成极严重的环境污染，治理水污染已成为当前我国城镇社会经济发展中迫切需要解决的重要问题，因此，寻求高效的水污染处理技术已成为当前国内外研究工作者的研究热点，高级氧化技术是当前难降解有机废水治理方向重要技术手段。本论文分别以甲基橙、酸性大红GR为模拟污染物，考察了光催化氧化技术和催化湿式氧化技术的处理效果，在此基础上构建了光催化-催化湿式氧化技术体系，以活性艳红X-3B为模拟污染物，考察了各因素的影响，得出动力学方程，同时探讨该技术协同机理，并对工业有机废水处理进行了研究。
本文首先研究了光催化氧化技术处理甲基橙溶液的效果。采用水热法制备出了不同形貌的ZnO纳米阵列，以甲基橙溶液为模拟有机废水考察了它们各自在紫外光下的催化性能。并对不同形貌的ZnO形貌的生长机理进行了分析，结果发现通过控制pH、添加不同活性剂等反应条件可以调控纳米ZnO样品的形貌，得到比表面积大、催化活性高的催化剂。为了提高单一半导体在催化过程中对污染物的降解效率，分别将TiO2、CuO等与ZnO复合，可控制备纳米TiO2/ZnO，CuO/ZnO等复合催化剂，结果表明两种半导体在降解过程中发挥了协同作用，共同促进了催化剂的降解效率，其中纳米CuO/ZnO复合催化剂的催化活性最高，有效地提高了光催化氧化技术处理有机废水效果。
其次，研究了催化湿式氧化技术对模拟酸性大红GR有机废水的处理效果。通过对各过渡金属催化性能的比较、复合及稀土Ce改性催化活性和催化剂稳定性研究，制备工艺的改进，采用浸渍法以γ-Al2O3为载体制备了高催化性能CuO-ZnO-CeO2/γ-Al2O3催化剂，并在常压下以该催化剂处理酸性大红GR模拟染料难降解有机废水，通过单因素及正交优化实验研究，得出处理模拟该废水最佳处理工艺条件：处理600mg/L的酸性大红GR模拟难降解有机废水（其CODCr值为396.85mg/L），反应温度70℃、反应时间2.5h、催化剂加入量为2.5g、30%H2O2加入量为0.5mL、进水pH值为4，废水CODCr去除率和脱色率分别达到86.13%和99.91%，降解效果显著。
在集合光催化氧化技术和催化湿式氧化技术研究基础上，构建了光催化-催化湿式氧化新工艺体系。考察了以CuO-ZnO-CeO2/γ-Al_2O_3为催化剂对活性艳红X-3B模拟有机染料废水处理工艺条件，并通过响应曲面法优化工艺，得出最佳工艺条件为：反应温度54℃，反应时间2.7h，催化剂投加量2.6g，H_2O_2投加量0.62mL，pH值3.4。此时脱色率可达99.33%。
采用ELKM动力学模型进行分析，结合实验分析结果，对光催化-催化湿式氧化降解活性艳红X-3B进行了动力学研究，发现符合伪一级动力学模型；反应动力学表观速率常数随温度升高有所增加，且与反应温度关系符合Arrhenius方程，表观活化能为32.79kJ/mol，表观动力学方程为：
利用UV-Vis、IR和GC-MS等检测手段分析光催化-催化湿式氧化工艺处理染料活性艳红X-3B中间产物进行分析，推测其降解路径，并由此推断光催化-催化湿式氧化工艺处理有机染料废水降解机理和协同效应，符合自由基机理，羟基自由基起主要作用。
最后，比较光催化-催化湿式氧化工艺和催化湿式氧化工艺处理实际工业有机废水处理效果，结果表明，光催化-催化湿式氧化工艺所要求温度更低和双氧水投加量更少，处理效率更佳，降低了能耗、物耗，为环境友好的处理工艺。
With development of modern industry, a large number of organic wastewaterwas produced, the compositions of wastewater were complicated and existed as thedifficult degradable organic pollutants in water. As we all known, the wastewater wastoxic and difficult to reach to standard emission using conventional physicochemicaland biochemical methods, which caused very serious environmental pollution, andthe control of water pollution had become the current urgent problems. Therefore,many domestic and foreign research workers focused on seeking effective waterpollution treatment methods. Advanced oxidation technology was an importanttechnical method to the current direction of refractory organic wastewater treatment.This paper respectively used methyl orange and acid red GR as simulate pollutants, toexamine the treatment effect of the photocatalytic oxidation technology and catalyticwet oxidation technology. The photocatalytic-catalytic wet oxidation technologysystem was built, and active brilliant red X-3B as simulate pollutants was used, theeffect of various factors, finally fabricating kinetics equation was studied, and thenthe technology synergy mechanism and the industrial organic wastewater werestudied.
Firstly,This paper studied the effect of the methyl orange solution’s degradationwhich used the technique of photocatalytic oxidation. Different morphology ZnOnanoparticle arrays was prepared by using hydrothermal method and their catalyticproperties were investigated under UV light with methyl orange solution as simulateorganic wastewater. And the growth mechanism of different morphology of ZnO wasanalyzed. These results showed that controlling the pH and adding different surfactantcould control the size of nanometer ZnO, and could get the nanometer ZnO of largespecific surface area and high catalytic activity of the catalyst. In order to overcomedefect of the single semiconductor of catalytic degradation efficiency of pollutants inthe process, TiO2, CuO were respectively composited with ZnO, the preparation ofnanometer TiO2/ZnO and CuO/ZnO composite catalyst, the results showed that thetwo kinds of semiconductor played a synergy in the degradation process, promoted the efficiency of the degradation of catalyst, the composite of nanometer CuO/ZnOcatalyst had the highest catalytic activity, effectively improved the effect of thetreatment of photocatalytic oxidation to deal with organic wastewater.
Secondly,The treatment effect of acid red GR and industrial refractory organicwastewater were studied by catalytic wet air oxidation technology. The high catalyticperformanceCuO-ZnO-CeO2/γ-Al2O3was prepared with impregnation methodon the carrier of γ-Al2O3. And the catalyst was used to deal with simulated acid redGR dye biodegradable organic wastewater at atmospheric pressure. On the basic ofexperimental studies by single factor and orthogonal optimization, the optimaltreatment conditions of the wastewater treatment process were:600mg/L ofsimulated acid red GR refractory organic wastewater (COD value was396.85mg/L),reaction temperature was70℃, reaction time was2.5h, catalyst dosage was2.5g,30%H2O2dosage was0.5mL, pH was4.COD removal and decolonization ratereached86.13%and99.91%, respectively. The degradation effect was remarkable.
Based on study of photocatalytic oxidation technology and catalytic wetoxidation technology research, the photocatalytic-wet catalytic oxidation process wasconstructed. Treatment process conditions of red X-3B dye analog refractory organicwastewater were studied by using the catalystCuO-ZnO-CeO2/γ-Al2O3and thisprocess. And optimization conditions by response surface methodology: the reactiontemperature was54℃, reaction time was2.7h, catalyst dosage was2.6g, dosagewas0.62mL, pH was3.4. At this point, the decolonization rate reached to99.33%.
Kinetic studies of degradation of reactive brilliant red X-3B by thephotocatalytic-catalytic wet oxidation were carried out by applying ELKM kineticmodels and combining with experimental results. The results showed that the processcompliance with the pseudo-first-order kinetic model. And apparent reaction kineticrate constants increased with temperature increasing, and fitted the Arrheniusequation relationship with the reaction temperature, and the apparent activationenergy was32.79kJ/mol. The apparent kinetic equation was:
The degradation path of simulation dye reactive brilliant red X-3B by the photocatalytic-wet catalytic oxidation process was analyzed by using UV-Vis, IR andGC-MS detection means. And the degradation mechanism of organic wastewatertreated by the process was inferred.
Finally, the effect of refractory industrial organic wastewater treatment wascomprised the photocatalytic-wet catalytic oxidation process and wet catalyticoxidation process. And the results showed that the photocatalytic-wet catalyticoxidation process required lower temperature and less hydrogen peroxide dosingwhile it attained better processing efficiency, and reduced the energy consumption. Itwas an environmental friendly process.
本文首先研究了光催化氧化技术处理甲基橙溶液的效果。采用水热法制备出了不同形貌的ZnO纳米阵列，以甲基橙溶液为模拟有机废水考察了它们各自在紫外光下的催化性能。并对不同形貌的ZnO形貌的生长机理进行了分析，结果发现通过控制pH、添加不同活性剂等反应条件可以调控纳米ZnO样品的形貌，得到比表面积大、催化活性高的催化剂。为了提高单一半导体在催化过程中对污染物的降解效率，分别将TiO2、CuO等与ZnO复合，可控制备纳米TiO2/ZnO，CuO/ZnO等复合催化剂，结果表明两种半导体在降解过程中发挥了协同作用，共同促进了催化剂的降解效率，其中纳米CuO/ZnO复合催化剂的催化活性最高，有效地提高了光催化氧化技术处理有机废水效果。
其次，研究了催化湿式氧化技术对模拟酸性大红GR有机废水的处理效果。通过对各过渡金属催化性能的比较、复合及稀土Ce改性催化活性和催化剂稳定性研究，制备工艺的改进，采用浸渍法以γ-Al2O3为载体制备了高催化性能CuO-ZnO-CeO2/γ-Al2O3催化剂，并在常压下以该催化剂处理酸性大红GR模拟染料难降解有机废水，通过单因素及正交优化实验研究，得出处理模拟该废水最佳处理工艺条件：处理600mg/L的酸性大红GR模拟难降解有机废水（其CODCr值为396.85mg/L），反应温度70℃、反应时间2.5h、催化剂加入量为2.5g、30%H2O2加入量为0.5mL、进水pH值为4，废水CODCr去除率和脱色率分别达到86.13%和99.91%，降解效果显著。
在集合光催化氧化技术和催化湿式氧化技术研究基础上，构建了光催化-催化湿式氧化新工艺体系。考察了以CuO-ZnO-CeO2/γ-Al_2O_3为催化剂对活性艳红X-3B模拟有机染料废水处理工艺条件，并通过响应曲面法优化工艺，得出最佳工艺条件为：反应温度54℃，反应时间2.7h，催化剂投加量2.6g，H_2O_2投加量0.62mL，pH值3.4。此时脱色率可达99.33%。
采用ELKM动力学模型进行分析，结合实验分析结果，对光催化-催化湿式氧化降解活性艳红X-3B进行了动力学研究，发现符合伪一级动力学模型；反应动力学表观速率常数随温度升高有所增加，且与反应温度关系符合Arrhenius方程，表观活化能为32.79kJ/mol，表观动力学方程为：
利用UV-Vis、IR和GC-MS等检测手段分析光催化-催化湿式氧化工艺处理染料活性艳红X-3B中间产物进行分析，推测其降解路径，并由此推断光催化-催化湿式氧化工艺处理有机染料废水降解机理和协同效应，符合自由基机理，羟基自由基起主要作用。
最后，比较光催化-催化湿式氧化工艺和催化湿式氧化工艺处理实际工业有机废水处理效果，结果表明，光催化-催化湿式氧化工艺所要求温度更低和双氧水投加量更少，处理效率更佳，降低了能耗、物耗，为环境友好的处理工艺。
With development of modern industry, a large number of organic wastewaterwas produced, the compositions of wastewater were complicated and existed as thedifficult degradable organic pollutants in water. As we all known, the wastewater wastoxic and difficult to reach to standard emission using conventional physicochemicaland biochemical methods, which caused very serious environmental pollution, andthe control of water pollution had become the current urgent problems. Therefore,many domestic and foreign research workers focused on seeking effective waterpollution treatment methods. Advanced oxidation technology was an importanttechnical method to the current direction of refractory organic wastewater treatment.This paper respectively used methyl orange and acid red GR as simulate pollutants, toexamine the treatment effect of the photocatalytic oxidation technology and catalyticwet oxidation technology. The photocatalytic-catalytic wet oxidation technologysystem was built, and active brilliant red X-3B as simulate pollutants was used, theeffect of various factors, finally fabricating kinetics equation was studied, and thenthe technology synergy mechanism and the industrial organic wastewater werestudied.
Firstly,This paper studied the effect of the methyl orange solution’s degradationwhich used the technique of photocatalytic oxidation. Different morphology ZnOnanoparticle arrays was prepared by using hydrothermal method and their catalyticproperties were investigated under UV light with methyl orange solution as simulateorganic wastewater. And the growth mechanism of different morphology of ZnO wasanalyzed. These results showed that controlling the pH and adding different surfactantcould control the size of nanometer ZnO, and could get the nanometer ZnO of largespecific surface area and high catalytic activity of the catalyst. In order to overcomedefect of the single semiconductor of catalytic degradation efficiency of pollutants inthe process, TiO2, CuO were respectively composited with ZnO, the preparation ofnanometer TiO2/ZnO and CuO/ZnO composite catalyst, the results showed that thetwo kinds of semiconductor played a synergy in the degradation process, promoted the efficiency of the degradation of catalyst, the composite of nanometer CuO/ZnOcatalyst had the highest catalytic activity, effectively improved the effect of thetreatment of photocatalytic oxidation to deal with organic wastewater.
Secondly,The treatment effect of acid red GR and industrial refractory organicwastewater were studied by catalytic wet air oxidation technology. The high catalyticperformanceCuO-ZnO-CeO2/γ-Al2O3was prepared with impregnation methodon the carrier of γ-Al2O3. And the catalyst was used to deal with simulated acid redGR dye biodegradable organic wastewater at atmospheric pressure. On the basic ofexperimental studies by single factor and orthogonal optimization, the optimaltreatment conditions of the wastewater treatment process were:600mg/L ofsimulated acid red GR refractory organic wastewater (COD value was396.85mg/L),reaction temperature was70℃, reaction time was2.5h, catalyst dosage was2.5g,30%H2O2dosage was0.5mL, pH was4.COD removal and decolonization ratereached86.13%and99.91%, respectively. The degradation effect was remarkable.
Based on study of photocatalytic oxidation technology and catalytic wetoxidation technology research, the photocatalytic-wet catalytic oxidation process wasconstructed. Treatment process conditions of red X-3B dye analog refractory organicwastewater were studied by using the catalystCuO-ZnO-CeO2/γ-Al2O3and thisprocess. And optimization conditions by response surface methodology: the reactiontemperature was54℃, reaction time was2.7h, catalyst dosage was2.6g, dosagewas0.62mL, pH was3.4. At this point, the decolonization rate reached to99.33%.
Kinetic studies of degradation of reactive brilliant red X-3B by thephotocatalytic-catalytic wet oxidation were carried out by applying ELKM kineticmodels and combining with experimental results. The results showed that the processcompliance with the pseudo-first-order kinetic model. And apparent reaction kineticrate constants increased with temperature increasing, and fitted the Arrheniusequation relationship with the reaction temperature, and the apparent activationenergy was32.79kJ/mol. The apparent kinetic equation was:
The degradation path of simulation dye reactive brilliant red X-3B by the photocatalytic-wet catalytic oxidation process was analyzed by using UV-Vis, IR andGC-MS detection means. And the degradation mechanism of organic wastewatertreated by the process was inferred.
Finally, the effect of refractory industrial organic wastewater treatment wascomprised the photocatalytic-wet catalytic oxidation process and wet catalyticoxidation process. And the results showed that the photocatalytic-wet catalyticoxidation process required lower temperature and less hydrogen peroxide dosingwhile it attained better processing efficiency, and reduced the energy consumption. Itwas an environmental friendly process.
引文
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