非均相Fenton反应催化剂的制备及其在难降解有机物处理中的应用
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摘要
随着工业的发展产生了大量有毒有机废水,但是传统的生化工艺无法处理这些污水。高级氧化技术被广泛的应用于处理此类废水,以去除工业废水中和垃圾渗滤液中难降解的有机物。均相Fenton是高级氧化技术中的一种,该技术被认为是处理此类污水最有前景的技术之一。但是该技术存在的明显的缺点限制了其应用：1反应所需pH范围较窄(2-4);2参与反应催化剂的回收比较困难,含重金属的污泥需要再处理,这增加了运行成本。为了克服这些问题,本文制备了一系列的非均相Fenton的催化剂,考查这些催化剂在常温常压下有机物去除情况。
(1)采用不同的浸渍方法制备了2个系列含铁量不同的Fe/SBA15,并使用N2：吸附-脱附和XRD对其进行了表征。考察了该催化剂在非均相Fenton体系下的催化氧化活性。结果表明：用燃烧法制备的催化剂SBA15-acFe(NO3)-2和SBA15-acFe(NO3)-1的催化活性较高,催化剂的稳定性很好。用C10H12FeN2Na08做为铁源制备的催化剂SBA15-iFeEDTA-1和SBA15-iFeEDTA-2的活性虽然高,但是当铁的含量增加后,催化剂的稳定性明显减弱。用传统浸渍法制备的SBA15-iFe(NO3)-1和SBA15-iFe(NO3)-2虽然稳定性较高,但是当铁的含量增加后,铁的氧化物未能均匀的分布在载体上导致催化活性降低。
(2)采用不同的浸渍法和均相共沉淀法制备了一系列含铁量相同的Fe/SBAl5,并使用N：吸附-脱附,TEM/EDX和XRD对其进行了表征,来考查各个催化剂的物理性质。应用传统的浸渍法制备的催化剂上Fe2O3颗粒的直径约为7-8nm,而用燃烧法制备的催化剂上Fe2O3颗粒的直径约为24nm且均匀的分布在载体SBAl5的孔道中。但是用不同均匀共沉淀法制备的催化剂使氧化铁的纳米颗粒物未能分布在载体的孔道内。以苯酚模拟废水为目标降解物,加入双氧水,在常温常压下考察了各个催化剂对苯酚的去除情况。结果表面各个催化剂的活性与铁的稳定性差异比较大。对于浸渍法获得的2个催化剂其活性较高,有一定量的铁滤出。而用均匀共沉淀法制备出的催化剂虽然有大的氧化铁颗粒物,但是还是展示出较高的催化活性和稳定性。
(3)合成具有更大比表面积,孔径和孔体积的新型的γ-Al203,将Fe2O3和LaFeO3负载在γ-Al2O3,通过利用N2吸附-脱附、X射线衍射(XRD), TEM/EDX, TPR等分析方法研究了催化剂的物理和化学结构特性。同时合成已经报道具有良好催化活性的催化剂做为对比催化剂,来考查各个催化剂对苯酚的去除效率,TOC去除率和催化剂的稳定性,研究表明催化剂LaFe-Almeso在众多催化剂中活性最高,且稳定性较高。
(4)制备新型的催化剂Al-Pillared Fe-Smectite,对其进行表征。应用该催化剂于UV-非均相Fenton体系中.在既定的试验条件下,考查该催化剂对橙黄Ⅱ的脱色,TOC去除率,催化剂稳定性和重复使用性等参数。同时通过响应面试验设计来分析各个试验参数对橙黄Ⅱ脱色的各自影响和交互影响。分析表明pH和H2O2浓度对橙黄看Ⅱ的脱色影响最大,同时对比响应面试验设计和析因子实验设计的分析结果。
Due to the inability of biological treatment processes to treat highly contaminated and toxic wastewater with organic pollutants, advanced oxidationprocesses (AOPs) are of great interest for the destruction of toxic and biorefractory organic pollutants found in industrial wastewater and in landfill leachate. Homogeneous Fenton processes are one technology of AOPs, they are considered as a series of most promising technologies for the remediation of wastewaters containing a variety of toxic substances. There are two major drawbacks that limit the industrial application of this technology:(1) the tight range of pH (e.g., pH 2-4) in which the reaction proceeds and (2) the need for recovering the precipitated catalyst after the treatment. The resulted sludge may contain organic substances, as well as heavy metals and has to be further treated, increasing thus the overall costs. However, in order to overcome the major drawbacks of the homogeneous system, heterogeneous Fenton-type systems have been prepared to catalyze the oxidation of various organic compounds in mild reaction conditions.
(1) Two series iron-based mesoporous silica materials were prepared according to different impregnation procedures. Several complementary techniques, including XRD and nitrogen sorption isotherms were used to evaluate the final structural and textural properties of the calcined Fe/SBA-15 materials. Catalytic performances of all the materials were evaluated in the heterogeneous Fenton system. The samples SBA15-acFe (NO3)-2 and SBA15-acFe (NO3)-1, prepared by self-combustion of an iron-glycinic complex within the silica porosity, have showed their good catalytic activity and stability. The sample SBA15-iFeEDTA-1 and SBA15-iFeEDTA-2, using C10H12FeN2NaO8 as iron precursor, have good catalytic activity, but their stability was decreased when the content of iron increased. The sample SBA15-iFe (NO3)-1 and SBA15-iFe (NO3)-2, prepared by classical wet impregnation of the silica support by iron nitrate, have excellent stability, but catalytic activity of these two samples were not good.
(2) Iron-based mesoporous silica materials were prepared according to different impregnation and co-condensation procedures. Several complementary techniques, including XRD, TEM/EDX and nitrogen sorption isotherms were used to evaluate the final structural and textural properties of the calcined Fe/SBA-15 materials. While Fe2O3 isolated particles of which the size is close to the silica pore diameter (～7-8 nm)were obtained using classical wet impregnation procedure, smaller iron oxide particles(-2-4 nm) homogeneously dispersed within the hexagonal pore structure of the SBA15 host support were generated through more sophisticated impregnation route (namely selfcombustionof an impregnated iron glycinic complex). By contrast, the various cocondensation routes used in this work were less efficient to obtain iron oxide nanoparticles inside the silica mesopores. Catalytic performances of all the materials were evaluated in the case of total phenol oxidation by H2O2 in aqueous solution at ambient conditions. Large differences in terms of catalytic activity and iron species stability were observed. While the impregnated solids proved to be the most active catalysts (highest iron oxide nanoparticles dispersion), iron leaching was observed in aqueous solution, accounting for a homogeneous catalytic contribution. In contrast, the co-condensed samples exhibiting larger iron oxide clusters stabilized over the silica surface proved more efficient as active sites in Fenton catalysis.
(3) Novelγ-Al2O3, with a large pore size and a high surface area, was prepared as support. Alumina-supported iron oxide and iron-based perovskite are synthesized. Several complementary techniques, including XRD, TEM/EDX and nitrogen sorption isotherms were used to evaluate the final structural and textural properties of the two samples.Evaluation of the nanocomposite reactivity for the oxidation of phenol indicated an improved catalytic activity for the two novel samples (iron and lanthanum-iron on alumina) than those exhibited by the corresponding bulk perovksite or optimized reference catalysts. Among all the tested samples, the novel LaFe-Almeso composite (an alumina-supported lanthanum iron mixed-oxide) presents the highest activity with excellent stability in reaction.
(4) Al-pillared Fe-Smectite was prepared and used as heterogeneous catalysts for the photo-Fenton decolorization of azo dye C.I. Acid Orange 7 under UV irradiation. UV irradiation is found to enhance the activity of the catalyst in the heterogeneous photo-Fenton process. Catalyst loadings of 0.5 g/L and 13.5 mM of hydrogen peroxide yield a remarkable decolorization, accompanied by excellent catalyst stability. An experimental design based on the response surface methodology is applied to assess the individual and interaction effects of several operating parameters namely hydrogen peroxide concentration, pH and catalyst loadings on the treatment efficiency. It is that the pH and H2O2 are found to be the vital parameters affecting dye degradation. The result of the response surface methodology design and the full factorial design (FFD) were compared.
(1)采用不同的浸渍方法制备了2个系列含铁量不同的Fe/SBA15,并使用N2：吸附-脱附和XRD对其进行了表征。考察了该催化剂在非均相Fenton体系下的催化氧化活性。结果表明：用燃烧法制备的催化剂SBA15-acFe(NO3)-2和SBA15-acFe(NO3)-1的催化活性较高,催化剂的稳定性很好。用C10H12FeN2Na08做为铁源制备的催化剂SBA15-iFeEDTA-1和SBA15-iFeEDTA-2的活性虽然高,但是当铁的含量增加后,催化剂的稳定性明显减弱。用传统浸渍法制备的SBA15-iFe(NO3)-1和SBA15-iFe(NO3)-2虽然稳定性较高,但是当铁的含量增加后,铁的氧化物未能均匀的分布在载体上导致催化活性降低。
(2)采用不同的浸渍法和均相共沉淀法制备了一系列含铁量相同的Fe/SBAl5,并使用N：吸附-脱附,TEM/EDX和XRD对其进行了表征,来考查各个催化剂的物理性质。应用传统的浸渍法制备的催化剂上Fe2O3颗粒的直径约为7-8nm,而用燃烧法制备的催化剂上Fe2O3颗粒的直径约为24nm且均匀的分布在载体SBAl5的孔道中。但是用不同均匀共沉淀法制备的催化剂使氧化铁的纳米颗粒物未能分布在载体的孔道内。以苯酚模拟废水为目标降解物,加入双氧水,在常温常压下考察了各个催化剂对苯酚的去除情况。结果表面各个催化剂的活性与铁的稳定性差异比较大。对于浸渍法获得的2个催化剂其活性较高,有一定量的铁滤出。而用均匀共沉淀法制备出的催化剂虽然有大的氧化铁颗粒物,但是还是展示出较高的催化活性和稳定性。
(3)合成具有更大比表面积,孔径和孔体积的新型的γ-Al203,将Fe2O3和LaFeO3负载在γ-Al2O3,通过利用N2吸附-脱附、X射线衍射(XRD), TEM/EDX, TPR等分析方法研究了催化剂的物理和化学结构特性。同时合成已经报道具有良好催化活性的催化剂做为对比催化剂,来考查各个催化剂对苯酚的去除效率,TOC去除率和催化剂的稳定性,研究表明催化剂LaFe-Almeso在众多催化剂中活性最高,且稳定性较高。
(4)制备新型的催化剂Al-Pillared Fe-Smectite,对其进行表征。应用该催化剂于UV-非均相Fenton体系中.在既定的试验条件下,考查该催化剂对橙黄Ⅱ的脱色,TOC去除率,催化剂稳定性和重复使用性等参数。同时通过响应面试验设计来分析各个试验参数对橙黄Ⅱ脱色的各自影响和交互影响。分析表明pH和H2O2浓度对橙黄看Ⅱ的脱色影响最大,同时对比响应面试验设计和析因子实验设计的分析结果。
Due to the inability of biological treatment processes to treat highly contaminated and toxic wastewater with organic pollutants, advanced oxidationprocesses (AOPs) are of great interest for the destruction of toxic and biorefractory organic pollutants found in industrial wastewater and in landfill leachate. Homogeneous Fenton processes are one technology of AOPs, they are considered as a series of most promising technologies for the remediation of wastewaters containing a variety of toxic substances. There are two major drawbacks that limit the industrial application of this technology:(1) the tight range of pH (e.g., pH 2-4) in which the reaction proceeds and (2) the need for recovering the precipitated catalyst after the treatment. The resulted sludge may contain organic substances, as well as heavy metals and has to be further treated, increasing thus the overall costs. However, in order to overcome the major drawbacks of the homogeneous system, heterogeneous Fenton-type systems have been prepared to catalyze the oxidation of various organic compounds in mild reaction conditions.
(1) Two series iron-based mesoporous silica materials were prepared according to different impregnation procedures. Several complementary techniques, including XRD and nitrogen sorption isotherms were used to evaluate the final structural and textural properties of the calcined Fe/SBA-15 materials. Catalytic performances of all the materials were evaluated in the heterogeneous Fenton system. The samples SBA15-acFe (NO3)-2 and SBA15-acFe (NO3)-1, prepared by self-combustion of an iron-glycinic complex within the silica porosity, have showed their good catalytic activity and stability. The sample SBA15-iFeEDTA-1 and SBA15-iFeEDTA-2, using C10H12FeN2NaO8 as iron precursor, have good catalytic activity, but their stability was decreased when the content of iron increased. The sample SBA15-iFe (NO3)-1 and SBA15-iFe (NO3)-2, prepared by classical wet impregnation of the silica support by iron nitrate, have excellent stability, but catalytic activity of these two samples were not good.
(2) Iron-based mesoporous silica materials were prepared according to different impregnation and co-condensation procedures. Several complementary techniques, including XRD, TEM/EDX and nitrogen sorption isotherms were used to evaluate the final structural and textural properties of the calcined Fe/SBA-15 materials. While Fe2O3 isolated particles of which the size is close to the silica pore diameter (～7-8 nm)were obtained using classical wet impregnation procedure, smaller iron oxide particles(-2-4 nm) homogeneously dispersed within the hexagonal pore structure of the SBA15 host support were generated through more sophisticated impregnation route (namely selfcombustionof an impregnated iron glycinic complex). By contrast, the various cocondensation routes used in this work were less efficient to obtain iron oxide nanoparticles inside the silica mesopores. Catalytic performances of all the materials were evaluated in the case of total phenol oxidation by H2O2 in aqueous solution at ambient conditions. Large differences in terms of catalytic activity and iron species stability were observed. While the impregnated solids proved to be the most active catalysts (highest iron oxide nanoparticles dispersion), iron leaching was observed in aqueous solution, accounting for a homogeneous catalytic contribution. In contrast, the co-condensed samples exhibiting larger iron oxide clusters stabilized over the silica surface proved more efficient as active sites in Fenton catalysis.
(3) Novelγ-Al2O3, with a large pore size and a high surface area, was prepared as support. Alumina-supported iron oxide and iron-based perovskite are synthesized. Several complementary techniques, including XRD, TEM/EDX and nitrogen sorption isotherms were used to evaluate the final structural and textural properties of the two samples.Evaluation of the nanocomposite reactivity for the oxidation of phenol indicated an improved catalytic activity for the two novel samples (iron and lanthanum-iron on alumina) than those exhibited by the corresponding bulk perovksite or optimized reference catalysts. Among all the tested samples, the novel LaFe-Almeso composite (an alumina-supported lanthanum iron mixed-oxide) presents the highest activity with excellent stability in reaction.
(4) Al-pillared Fe-Smectite was prepared and used as heterogeneous catalysts for the photo-Fenton decolorization of azo dye C.I. Acid Orange 7 under UV irradiation. UV irradiation is found to enhance the activity of the catalyst in the heterogeneous photo-Fenton process. Catalyst loadings of 0.5 g/L and 13.5 mM of hydrogen peroxide yield a remarkable decolorization, accompanied by excellent catalyst stability. An experimental design based on the response surface methodology is applied to assess the individual and interaction effects of several operating parameters namely hydrogen peroxide concentration, pH and catalyst loadings on the treatment efficiency. It is that the pH and H2O2 are found to be the vital parameters affecting dye degradation. The result of the response surface methodology design and the full factorial design (FFD) were compared.
引文
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