微波强化ClO_2催化氧化工艺及应用研究
摘要
针对目前水中难降解有机污染物处理中存在的技术问题,本文研究开发出一种新型物理化学水处理技术-微波强化高级氧化工艺(Microwave-enhanced Advanced Oxidation Process,简称为MAOP)。微波强化高级氧化技术具有反应速度快、占地面积小、设备简单、操作方便等优点,在水处理领域内有着广阔的应用前景。本文围绕微波强化ClO_2催化氧化工艺中催化剂的研制这一技术关键,制备了CuO/γ-Al_2O_3和La_2O_3-CuO/γ-Al_2O_3催化剂,并以La_2O_3-CuO/γ-Al_2O_3为催化剂,以活性艳黄染料和苯酚模拟废水为处理对象,建立微波强化ClO_2催化氧化处理难降解有机物工艺;研究苯酚和活性艳黄染料在微波强化ClO_2催化氧化工艺中的动力学和体系中羟基自由基的产生以及作用机制;并分析催化剂La_2O_3-CuO/γ-Al_2O_3在使用过程中的失活原因,确定最优的再生方法,均取得了理想的结果。
本文首先以γ-Al_2O_3为载体,以铜盐为活性组分,采用浸渍沉淀法制备了CuO/γ-Al_2O_3催化剂,对其在微波强化ClO_2催化氧化工艺中的催化活性和稳定性进行研究,并进一步选取稀土镧为助剂,采用分层浸渍沉淀法制备出La_2O_3-CuO/γ-Al_2O_3催化剂。催化剂的结构分析表明,La_2O_3-CuO/γ-Al_2O_3中铜以CuO和Cu2O的形式存在,镧以La_2O_3的形式存在,其中铜的含量为6.748%,镧的含量为0.257%。同时,镧的掺杂可以与载体结合,提高载体γ-Al_2O_3的热稳定性,增大催化剂的比表面积,提高活性组分的负载量,并使得催化剂表面的活性组分CuO的粒径更小、分散更加均匀,增加了催化剂表面的活性点,提高其催化活性和稳定性。
以自制La_2O_3-CuO/γ-Al_2O_3为催化剂,ClO_2为氧化剂,研究建立微波强化ClO_2催化氧化工艺。对于100mL初始浓度为200mg/L的模拟染料废水,最佳的处理工艺条件为:微波辐照功率400W,辐照时间1.5min,pH值为7, ClO_2投加量80mg/L,催化剂加入量70g/L。在此工艺条件下,对活性艳黄染料的脱色率达到94.03%,TOC去除率为67.92%;对于100mL初始浓度为100mg/L的模拟苯酚废水,最佳的处理工艺条件为:微波辐照功率50W,辐照时间5min,pH值为7,ClO_2投加量80mg/L,催化剂加入量50g/L。在此工艺条件下,对苯酚的去除率达91.66%,TOC去除率为50.35%;
本文系统研究了微波强化ClO_2催化氧化、微波强化ClO_2氧化、水浴条件下ClO_2催化氧化和水浴条件下ClO_2氧化四种工艺中ClO_2与苯酚的反应动力学。结果表明,四种处理工艺条件下,ClO_2催化氧化苯酚的反应对于苯酚反应级数为1,对ClO_2反应级数为1,总反应级数为2。对比四种不同工艺中的反应速率常数可知,微波辐照与La_2O_3-CuO/γ-Al_2O_3催化剂联合使用可明显提高ClO_2降解有机物的反应速率。
采用分子荧光光谱法,本文对微波强化ClO_2催化氧化体系中的羟基自由基的生成规律进行了研究探讨。结果表明,常温下ClO_2氧化体系未检测到·OH自由基;常温下ClO_2催化氧化体系和微波强化ClO_2氧化体系可产生少量的·OH自由基;当微波辐照、La_2O_3-CuO/γ-Al_2O_3催化剂和ClO_2联合使用时,体系中有大量的·OH自由基生成,说明微波辐照与催化剂具有协同作用,可明显提高ClO_2氧化体系产生·OH自由基的能力。基于此,本文提出微波强化ClO_2催化氧化处理水中有机污染物的可能机制为:废水中的有机污染物首先被吸附于催化剂表面,由于催化剂能够强烈地吸收微波,催化剂表面在微波场中生成“热点”,同时微波诱导ClO_2产生羟基自由基,由于“热点”的高温作用和羟基自由基氧化反应使吸附于催化剂表面的有机污染物被迅速氧化分解。
本文还对系统处理活性艳黄染料废水过程中催化剂的失活原因和再生方法进行了深入研究。结果表明,催化剂在使用过程中的失活主要是由废水降解所产生的含碳的中间产物吸附在催化剂表面,掩盖了催化剂的活性中心而引起的。微波辐射再生是一种非常有效的再生方法,其最优工艺条件是微波功率500W,辐照时间30min,SiC与催化剂比值2:1,在此条件下再生的催化剂活性可恢复到新鲜催化剂的91.67%。再生催化剂的结构表征分析表明,催化剂再生之后,其各项结构参数均可基本恢复至新鲜催化剂的状态。
本文将微波技术和改性γ-Al_2O_3催化剂结合,对传统的ClO_2氧化法进行改进,该方法具有ClO_2用量少、pH值适用范围广、处理速度快、处理效率高、出水温度适宜、投加方式简单、设备简单、操作方便等优点,为水中难降解有机污染物的处理提供了一种新型的有潜力的处理工艺。
Aim to problems of nonbiodegradable wastewater treatment, micirowave-enhanced advanced oxidation process (MAOP) is founded. Compared with other advanced oxidation processes, microwave enhanced oxidation process has many advantages such as the oxidation speed and the mineralization efficiency are higher, the set-up is simpler, and the operation conditions are more convenient. So it promises to have a wide application in the wastewater treatment. The preparing of heterogeneous catalysts with high activity and stability is one of key techniques in MAOP. In this paper, CuO/γ-Al_2O_3 catalyst and La_2O_3-CuO/γ-Al_2O_3 catalyst were prepared. The catalytic activity of La_2O_3-CuO/γ-Al_2O_3 catalyst was investigated in microwave enhanced ClO_2 catatlytic oxidation process by using phenol and remazol golden yellow dye as as model pollutants.
The kinetic and degradation mechanism of remazol golden yellow dye and phenol in MAOP were studied. The formation of hydroxide radical group (·OH) in MAOP was also investigated. The reason of deactivated catalyst La_2O_3-CuO/γ-Al_2O_3 was analyzed and several different regeneration methods were compared. Firstly, CuO/γ-Al_2O_3 was prepared by impregnation-deposition method. The catalytic activity and stability were investigated in MAOP. Because the catalytic activity of CuO/γ-Al_2O_3 decreased fast in the successive runs, La_2O_3-CuO/γ-Al_2O_3 catalyst was prepared by selecting La as doping agent to improve the catalytic activity of CuO/γ-Al_2O_3. According to the structure analysis, Cu exists as CuO and Cu2O in La_2O_3-CuO/γ-Al_2O_3 with the loading amount of 6.748%; La exists as La_2O_3 in La_2O_3-CuO/γ-Al_2O_3 with the loading amount of 0.257%. It proved the surface modification of the carrierγ-Al_2O_3 by the addition of La_2O_3 could reinforce the thermal ability of the support within a certain extent. La_2O_3 could promote the structure of supports and intensify the interaction between active component and support, so that the loading of Cu in the catalyst was improved. Better dispersion and smaller size of CuO crystals could be obtained by La_2O_3, which made the number of active site increased.
The process of microwave enhanced chlorine dioxide oxidation treating phenol or remazol golden yellow dye wastewater was investigated by adding La_2O_3-CuO/γ-Al_2O_3 as a catalyst. 100mL synthetic wastewater containing 100 mg/L phenol was treated in MAOP and 91.66% of phenol and 50.35% of total organic carbon (TOC) could be removed under the optimum process conditions: ClO_2 concentration 80 mg/L, microwave power 50 W, contact time 5 min, catalyst dosage 50 g/L, pH 9. Under an optimal condition (ClO_2 concentration 80 mg/L, microwave power 400 W, contact time 1.5 min, catalyst dosage 70 g/L, pH 7), remazol golden yellow dye removal percentage approached 94.03%, corresponding to 67.92% of TOC removal.
The reaction kinetics in microwave enhanced ClO_2 catatlytic oxidation process, microwave enhanced ClO_2 oxidation process, traditional waterbath ClO_2 catatlytic oxidation process and traditional waterbath ClO_2 oxidation process were studied. Results suggested that the process between phenol and ClO_2 oxidation reaction accord to first-order reaction for phenol and first-order for chlorine dioxide, the total reaction order was 2. Comparesion of reaction constant in different treatments, it could be concluded in microwave enhanced ClO_2 catatlytic oxidation process microwave irradiation and catalyst work together to improve the reaction rate.
The fluorescence technology was applied to detect the regulation of hydroxyl radicals (·OH) created in microwave enhanced ClO_2 catatlytic oxidation process. The results showed that there was no·OH created in ClO_2 oxidation process under room temperature; there were a few hydroxyl radicals created in ClO_2 catatlytic oxidation process under room temperature and microwave enhanced ClO_2 oxidation process; a lot of hydroxyl radicals were created in microwave enhanced ClO_2 catatlytic oxidation process. The mechanisms of organic pollutant degraded in microwave enhanced ClO_2 catatlytic oxidation process could be conluded: organic pollutant were absorbed on the surface of the catalyst, at the same time; microwave was focused on the surface of the catalyst which can absorb microwave. And microwave was transferred heat energy. So the catalyst was heated to very high temperature, which is called hot spot. Then organic pollutant were degraded by·OH which produced by microwave induced ClO_2 under high temperature of the hot spot formed on the surfaced of catalyst in the microwave field.
The deactivation reason and regeneration methods of prepared catalysts were also studied in this dissertation. The deactivation was caused by the degradation products of pllutions contained C elements remained on the surface of catalyst and covered the active sites. Microwave radiation regeneration technology was an effective regeneration method; the regenerated catalyst could restore the 91.67% activity of the fresh catalyst with the following working conditions: power of microwave, 500W; exposure time, 30 min; SiC catalyst ratio, 2:1. Studies showed the catalytic activity of regenerated catalyst was very close to initial activity.
The improvement of traditional chlorine dioxide oxidation has been realized by combining microwave technology and modifiedγ-Al_2O_3 catalytic oxidation. Compared with traditional ClO_2 oxidation, microwave-assisted ClO_2 catalytic oxidation process can degrade contaminants in short reaction time and with low oxidant dosage, extensive pH range. As a developing process, the microwave enhanced ClO_2 catalytic oxidation process would provide a novel treatment method for the refractory wastewater and would have a broad prospect.
本文首先以γ-Al_2O_3为载体,以铜盐为活性组分,采用浸渍沉淀法制备了CuO/γ-Al_2O_3催化剂,对其在微波强化ClO_2催化氧化工艺中的催化活性和稳定性进行研究,并进一步选取稀土镧为助剂,采用分层浸渍沉淀法制备出La_2O_3-CuO/γ-Al_2O_3催化剂。催化剂的结构分析表明,La_2O_3-CuO/γ-Al_2O_3中铜以CuO和Cu2O的形式存在,镧以La_2O_3的形式存在,其中铜的含量为6.748%,镧的含量为0.257%。同时,镧的掺杂可以与载体结合,提高载体γ-Al_2O_3的热稳定性,增大催化剂的比表面积,提高活性组分的负载量,并使得催化剂表面的活性组分CuO的粒径更小、分散更加均匀,增加了催化剂表面的活性点,提高其催化活性和稳定性。
以自制La_2O_3-CuO/γ-Al_2O_3为催化剂,ClO_2为氧化剂,研究建立微波强化ClO_2催化氧化工艺。对于100mL初始浓度为200mg/L的模拟染料废水,最佳的处理工艺条件为:微波辐照功率400W,辐照时间1.5min,pH值为7, ClO_2投加量80mg/L,催化剂加入量70g/L。在此工艺条件下,对活性艳黄染料的脱色率达到94.03%,TOC去除率为67.92%;对于100mL初始浓度为100mg/L的模拟苯酚废水,最佳的处理工艺条件为:微波辐照功率50W,辐照时间5min,pH值为7,ClO_2投加量80mg/L,催化剂加入量50g/L。在此工艺条件下,对苯酚的去除率达91.66%,TOC去除率为50.35%;
本文系统研究了微波强化ClO_2催化氧化、微波强化ClO_2氧化、水浴条件下ClO_2催化氧化和水浴条件下ClO_2氧化四种工艺中ClO_2与苯酚的反应动力学。结果表明,四种处理工艺条件下,ClO_2催化氧化苯酚的反应对于苯酚反应级数为1,对ClO_2反应级数为1,总反应级数为2。对比四种不同工艺中的反应速率常数可知,微波辐照与La_2O_3-CuO/γ-Al_2O_3催化剂联合使用可明显提高ClO_2降解有机物的反应速率。
采用分子荧光光谱法,本文对微波强化ClO_2催化氧化体系中的羟基自由基的生成规律进行了研究探讨。结果表明,常温下ClO_2氧化体系未检测到·OH自由基;常温下ClO_2催化氧化体系和微波强化ClO_2氧化体系可产生少量的·OH自由基;当微波辐照、La_2O_3-CuO/γ-Al_2O_3催化剂和ClO_2联合使用时,体系中有大量的·OH自由基生成,说明微波辐照与催化剂具有协同作用,可明显提高ClO_2氧化体系产生·OH自由基的能力。基于此,本文提出微波强化ClO_2催化氧化处理水中有机污染物的可能机制为:废水中的有机污染物首先被吸附于催化剂表面,由于催化剂能够强烈地吸收微波,催化剂表面在微波场中生成“热点”,同时微波诱导ClO_2产生羟基自由基,由于“热点”的高温作用和羟基自由基氧化反应使吸附于催化剂表面的有机污染物被迅速氧化分解。
本文还对系统处理活性艳黄染料废水过程中催化剂的失活原因和再生方法进行了深入研究。结果表明,催化剂在使用过程中的失活主要是由废水降解所产生的含碳的中间产物吸附在催化剂表面,掩盖了催化剂的活性中心而引起的。微波辐射再生是一种非常有效的再生方法,其最优工艺条件是微波功率500W,辐照时间30min,SiC与催化剂比值2:1,在此条件下再生的催化剂活性可恢复到新鲜催化剂的91.67%。再生催化剂的结构表征分析表明,催化剂再生之后,其各项结构参数均可基本恢复至新鲜催化剂的状态。
本文将微波技术和改性γ-Al_2O_3催化剂结合,对传统的ClO_2氧化法进行改进,该方法具有ClO_2用量少、pH值适用范围广、处理速度快、处理效率高、出水温度适宜、投加方式简单、设备简单、操作方便等优点,为水中难降解有机污染物的处理提供了一种新型的有潜力的处理工艺。
Aim to problems of nonbiodegradable wastewater treatment, micirowave-enhanced advanced oxidation process (MAOP) is founded. Compared with other advanced oxidation processes, microwave enhanced oxidation process has many advantages such as the oxidation speed and the mineralization efficiency are higher, the set-up is simpler, and the operation conditions are more convenient. So it promises to have a wide application in the wastewater treatment. The preparing of heterogeneous catalysts with high activity and stability is one of key techniques in MAOP. In this paper, CuO/γ-Al_2O_3 catalyst and La_2O_3-CuO/γ-Al_2O_3 catalyst were prepared. The catalytic activity of La_2O_3-CuO/γ-Al_2O_3 catalyst was investigated in microwave enhanced ClO_2 catatlytic oxidation process by using phenol and remazol golden yellow dye as as model pollutants.
The kinetic and degradation mechanism of remazol golden yellow dye and phenol in MAOP were studied. The formation of hydroxide radical group (·OH) in MAOP was also investigated. The reason of deactivated catalyst La_2O_3-CuO/γ-Al_2O_3 was analyzed and several different regeneration methods were compared. Firstly, CuO/γ-Al_2O_3 was prepared by impregnation-deposition method. The catalytic activity and stability were investigated in MAOP. Because the catalytic activity of CuO/γ-Al_2O_3 decreased fast in the successive runs, La_2O_3-CuO/γ-Al_2O_3 catalyst was prepared by selecting La as doping agent to improve the catalytic activity of CuO/γ-Al_2O_3. According to the structure analysis, Cu exists as CuO and Cu2O in La_2O_3-CuO/γ-Al_2O_3 with the loading amount of 6.748%; La exists as La_2O_3 in La_2O_3-CuO/γ-Al_2O_3 with the loading amount of 0.257%. It proved the surface modification of the carrierγ-Al_2O_3 by the addition of La_2O_3 could reinforce the thermal ability of the support within a certain extent. La_2O_3 could promote the structure of supports and intensify the interaction between active component and support, so that the loading of Cu in the catalyst was improved. Better dispersion and smaller size of CuO crystals could be obtained by La_2O_3, which made the number of active site increased.
The process of microwave enhanced chlorine dioxide oxidation treating phenol or remazol golden yellow dye wastewater was investigated by adding La_2O_3-CuO/γ-Al_2O_3 as a catalyst. 100mL synthetic wastewater containing 100 mg/L phenol was treated in MAOP and 91.66% of phenol and 50.35% of total organic carbon (TOC) could be removed under the optimum process conditions: ClO_2 concentration 80 mg/L, microwave power 50 W, contact time 5 min, catalyst dosage 50 g/L, pH 9. Under an optimal condition (ClO_2 concentration 80 mg/L, microwave power 400 W, contact time 1.5 min, catalyst dosage 70 g/L, pH 7), remazol golden yellow dye removal percentage approached 94.03%, corresponding to 67.92% of TOC removal.
The reaction kinetics in microwave enhanced ClO_2 catatlytic oxidation process, microwave enhanced ClO_2 oxidation process, traditional waterbath ClO_2 catatlytic oxidation process and traditional waterbath ClO_2 oxidation process were studied. Results suggested that the process between phenol and ClO_2 oxidation reaction accord to first-order reaction for phenol and first-order for chlorine dioxide, the total reaction order was 2. Comparesion of reaction constant in different treatments, it could be concluded in microwave enhanced ClO_2 catatlytic oxidation process microwave irradiation and catalyst work together to improve the reaction rate.
The fluorescence technology was applied to detect the regulation of hydroxyl radicals (·OH) created in microwave enhanced ClO_2 catatlytic oxidation process. The results showed that there was no·OH created in ClO_2 oxidation process under room temperature; there were a few hydroxyl radicals created in ClO_2 catatlytic oxidation process under room temperature and microwave enhanced ClO_2 oxidation process; a lot of hydroxyl radicals were created in microwave enhanced ClO_2 catatlytic oxidation process. The mechanisms of organic pollutant degraded in microwave enhanced ClO_2 catatlytic oxidation process could be conluded: organic pollutant were absorbed on the surface of the catalyst, at the same time; microwave was focused on the surface of the catalyst which can absorb microwave. And microwave was transferred heat energy. So the catalyst was heated to very high temperature, which is called hot spot. Then organic pollutant were degraded by·OH which produced by microwave induced ClO_2 under high temperature of the hot spot formed on the surfaced of catalyst in the microwave field.
The deactivation reason and regeneration methods of prepared catalysts were also studied in this dissertation. The deactivation was caused by the degradation products of pllutions contained C elements remained on the surface of catalyst and covered the active sites. Microwave radiation regeneration technology was an effective regeneration method; the regenerated catalyst could restore the 91.67% activity of the fresh catalyst with the following working conditions: power of microwave, 500W; exposure time, 30 min; SiC catalyst ratio, 2:1. Studies showed the catalytic activity of regenerated catalyst was very close to initial activity.
The improvement of traditional chlorine dioxide oxidation has been realized by combining microwave technology and modifiedγ-Al_2O_3 catalytic oxidation. Compared with traditional ClO_2 oxidation, microwave-assisted ClO_2 catalytic oxidation process can degrade contaminants in short reaction time and with low oxidant dosage, extensive pH range. As a developing process, the microwave enhanced ClO_2 catalytic oxidation process would provide a novel treatment method for the refractory wastewater and would have a broad prospect.
引文
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