新型复合光催化剂的构筑、微结构调控及其降解有机污染物研究
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摘要
近年来,随着人们对环境问题的日益重视,环境污染处理新技术得到快速发展。其中,光催化技术具有能耗低、无污染等优点受到了广泛关注。Ti02半导体因为具有催化活性高、化学和光稳定性好、安全无毒等优点而被作为一种常用的光催化剂。但是,Ti02较宽的禁带宽度使其只能利用太阳光中少部分的紫外光,且存在难以回收利用问题,限制了其在实际中的应用。因此,有必要寻求新型可见光响应的光催化材料并提高其可回收利用性能。Bi2WO6半导体具有高活性、可见光响应、无毒等特点,近年来备受人们关注。但Bi2WO6催化剂仍然存在光生电子空穴容易复合和吸附性不足问题。为解决此问题,本论文主要进行了金属氧化物或粘土复合Bi2WO6研究,并对其可见光催化降解有机污染物进行研究。
本文首先采用简单易行的水热法成功合成具有分等级结构CaWO4/Bi2WO6复合光催化剂。通过XRD、TEM、SEM、UV-vis DRS、BET、XPS等多种现代表征手段,分析CaWO4/Bi2WO6复合光催化剂的微结构、相学组成与表面特征之间的构效关系。探讨CaWO4/Bi2WO6复合光催化剂对有机污染物罗丹明B(RhB)和对硝基苯酚(4-NP)的光催化降解活性。与纯的Bi2WO6比较,复合光催化剂对RhB和4-NP的光催化活性分别提高4.5倍和1.8倍。另外,复合光催化剂在4次光降解循环后仍能保持良好的活性。利用催化剂能带结构的估算,揭示复合光催化材料光催化活性增强的原因是电子空穴对的有效分离。
为了进一步提高Bi2WO6催化剂的光催化活性,本文通过水热法成功合成可见光响应的具有分等级结构α-Fe2O3/Bi2WO6复合光催化剂。采用XRD、SEM、 HRTEM、BET、XPS、UV-vis DRS等多种现代表征手段,分析α-Fe2O3/Bi2WO6复合光催化剂的微结构、相学组成和光吸收等特征。α-Fe2O3/Bi2WO6复合光催化剂对有机污染物罗丹明B(RhB)和酸性红染料呈现出良好的吸附性能和较高的光催化活性。通过各种活性基团的测定结果及催化剂能带结构的估算,发现复合光催化材料具有高活性高吸附性的原因是α-Fe2O3(?)(?)Bi2WO6的协同作用的结果。
为了进一步增强Bi2WO6催化剂的吸附性,提高固液分离效率及重复利用率,本文选用累托石粘土作为载体,通过溶胶凝胶法成功合成可见光响应的Bi2WO6/累托石复合光催化剂。采用XRD、SEM、HRTEM、BET、XPS、UV-vis DRS等多种现代表征手段,分析Bi2WO6/累托石复合光催化剂的层状结构与表面特征之间的关系。Bi2WO6/累托石复合光催化剂对直接大红(4BS)呈现出良好的较高光催化活性和吸附性能。复合光催化剂性能增强的原因主要归因于Bi2WO6半导体的可见光吸收和累托石吸附的协同作用。
最后,本文还对新型等离子体光催化材料进行了探索。以硅酸钠和硝酸银作为原料,采用简单易行的微波法-光诱导还原和离子交换法-光诱导还原两种方法分别合成可见光响应的Ag-Ag6Si207等离子体光催化剂。所制备的等离子体光催化剂对目标污染物亚甲基蓝(MB)有良好的催化降解活性,主要归因于金属Ag等离子体共振效应和Ag6Si207极化场作用。从活性自由基实验结果发现空穴(h+)和过氧(O2·-)自由基在Ag-Ag6Si207光催化剂降解污染物中起了非常重要的作用。最后对Ag-Ag6Si207离子体催化材料的稳定性及相关机理进行了探讨。
Recently, as people pay more attention to the environmental issues, the study on treatment technology of environmental pollution is fastly developed. The photocatalysis has attracted great interest for its low energy consumption and innocuity. TiO2is the most widely used photocatalyst due to its high catalytic activity, good chemical stability and non-toxicity, etc. However, it is activated only under UV light irradiation because of its large band gap, moreover, the TiO2powder in suspended system was difficult to separate from aqueous solution, and these questions hindered its practical applications. Therefore, the development of new visible light-driven photocatalyst is essential to improve recyclable performance. Due to its nontoxicity and visible-light responsiveness, Bi2WO6exhibits excellent photocatalytic properties for the decomposition of a great variety of organic pollutants in environmental purification applications. However, the high recombination of photo-generated carriers and low adsorption capacity cause low photo quantum efficiency, resulting in the low photocatalytic performance of Bi2WO6. To overcome the drawback of low photocatalytic efficiency brought by electron holes recombination and low adsorption capacity, we mainly introduced the synthesis and the enhanced photocatalytic activity of the Bi2WO6composite, the clay composite and the plasma composite.
In this paper, hierarchical structured CaWO4/Bi2WO6composite was successfully synthesized by a facile and low-cost hydrothermal route. The as-prepared composite were characterized by XRD, SEM, TEM, UV-vis DRS, FT-IR, TG-DSC and BET. The relationship between the hierarchical structured, chemical composition and the surface features of the composite was discussed through a various kind's characterization analysis. The photocatalytic activities of the CaWO4Bi2WO6composite were evaluated for the degradation of Rhodamine B (RhB) dye and4-nitrophenol (4-NP) in aqueous solution under visible-light irradiation (>420nm), which were4.5times and2.5times higher than that of the pure Bi2WO6, respectively. The CaWO4/Bi2WO6composite still showed the high photocatalytic activity after four reaction cycles. On the basis of the calculated energy band positions, the mechanism of enhanced photocatalytic activity for the CaWO4/Bi2WO6composite can be attributed to the effective separation of electron-hole pairs.
To further improve the photocatalytic activities of the Bi2WO6, the hierarchically structured a-Fe2O3/Bi2WO6composite was synthesized by a hydrothermal route. The as-prepared samples were characterized by XRD, SEM, TEM, FT-IR, XPS and BET. The a-Fe2O3/Bi2WO6composite exhibited a strong adsorption capability and a higher visible light photocatalytic activity than the pure Bi2WO6for the photocatalytic degradation of acid red G dye or RhB dye. On the basis of the experimental results and calculated energy band positions, the enhanced photocatalytic activity of the composite can be attributed to the hierarchical structure and the coupling effect of a-Fe2O3and Bi2WO6in the composite.
To further improve the adsorption capability of the Bi2WO6, the Bi2WO6/rectorite composites were prepared by a sol-gel method. The relationship between the layer structured and the surface features of the composite was investigated by XRD, SEM, TEM, FT-IR, XPS and BET. The results showed that the composites exhibited a strong adsorption capability and a higher photocatalytic degradation activity for4BS dye, which could be attributed to the synergetic effects of the adsorbability of rectorite and the photocatalytic property of Bi2WO6in it.
The novel, efficient, plasma photocatalytic materials was also exploring at the last part. The visible-light-responsive Ag-Ag6Si2O7photocatalyst was synthesized using sodium silicate and silver nitrate as raw materials by a facile microwave method or ion-exchange method and subsequently light-induced reduction route. The Ag-Ag6Si2O7spherical composite exhibited a higher visible light photocatalytic activity for the photocatalytic degradation of MB dye in aqueous solution, which was attributed to the surface plasmon and the polarized field of the Ag6Si2O7photocatalyst. The results showed that h+and O2·-were involved as the active species in the photocatalytic reaction. A possible photocatalytic mechanism and the photocatalytic stability were discussed.
本文首先采用简单易行的水热法成功合成具有分等级结构CaWO4/Bi2WO6复合光催化剂。通过XRD、TEM、SEM、UV-vis DRS、BET、XPS等多种现代表征手段,分析CaWO4/Bi2WO6复合光催化剂的微结构、相学组成与表面特征之间的构效关系。探讨CaWO4/Bi2WO6复合光催化剂对有机污染物罗丹明B(RhB)和对硝基苯酚(4-NP)的光催化降解活性。与纯的Bi2WO6比较,复合光催化剂对RhB和4-NP的光催化活性分别提高4.5倍和1.8倍。另外,复合光催化剂在4次光降解循环后仍能保持良好的活性。利用催化剂能带结构的估算,揭示复合光催化材料光催化活性增强的原因是电子空穴对的有效分离。
为了进一步提高Bi2WO6催化剂的光催化活性,本文通过水热法成功合成可见光响应的具有分等级结构α-Fe2O3/Bi2WO6复合光催化剂。采用XRD、SEM、 HRTEM、BET、XPS、UV-vis DRS等多种现代表征手段,分析α-Fe2O3/Bi2WO6复合光催化剂的微结构、相学组成和光吸收等特征。α-Fe2O3/Bi2WO6复合光催化剂对有机污染物罗丹明B(RhB)和酸性红染料呈现出良好的吸附性能和较高的光催化活性。通过各种活性基团的测定结果及催化剂能带结构的估算,发现复合光催化材料具有高活性高吸附性的原因是α-Fe2O3(?)(?)Bi2WO6的协同作用的结果。
为了进一步增强Bi2WO6催化剂的吸附性,提高固液分离效率及重复利用率,本文选用累托石粘土作为载体,通过溶胶凝胶法成功合成可见光响应的Bi2WO6/累托石复合光催化剂。采用XRD、SEM、HRTEM、BET、XPS、UV-vis DRS等多种现代表征手段,分析Bi2WO6/累托石复合光催化剂的层状结构与表面特征之间的关系。Bi2WO6/累托石复合光催化剂对直接大红(4BS)呈现出良好的较高光催化活性和吸附性能。复合光催化剂性能增强的原因主要归因于Bi2WO6半导体的可见光吸收和累托石吸附的协同作用。
最后,本文还对新型等离子体光催化材料进行了探索。以硅酸钠和硝酸银作为原料,采用简单易行的微波法-光诱导还原和离子交换法-光诱导还原两种方法分别合成可见光响应的Ag-Ag6Si207等离子体光催化剂。所制备的等离子体光催化剂对目标污染物亚甲基蓝(MB)有良好的催化降解活性,主要归因于金属Ag等离子体共振效应和Ag6Si207极化场作用。从活性自由基实验结果发现空穴(h+)和过氧(O2·-)自由基在Ag-Ag6Si207光催化剂降解污染物中起了非常重要的作用。最后对Ag-Ag6Si207离子体催化材料的稳定性及相关机理进行了探讨。
Recently, as people pay more attention to the environmental issues, the study on treatment technology of environmental pollution is fastly developed. The photocatalysis has attracted great interest for its low energy consumption and innocuity. TiO2is the most widely used photocatalyst due to its high catalytic activity, good chemical stability and non-toxicity, etc. However, it is activated only under UV light irradiation because of its large band gap, moreover, the TiO2powder in suspended system was difficult to separate from aqueous solution, and these questions hindered its practical applications. Therefore, the development of new visible light-driven photocatalyst is essential to improve recyclable performance. Due to its nontoxicity and visible-light responsiveness, Bi2WO6exhibits excellent photocatalytic properties for the decomposition of a great variety of organic pollutants in environmental purification applications. However, the high recombination of photo-generated carriers and low adsorption capacity cause low photo quantum efficiency, resulting in the low photocatalytic performance of Bi2WO6. To overcome the drawback of low photocatalytic efficiency brought by electron holes recombination and low adsorption capacity, we mainly introduced the synthesis and the enhanced photocatalytic activity of the Bi2WO6composite, the clay composite and the plasma composite.
In this paper, hierarchical structured CaWO4/Bi2WO6composite was successfully synthesized by a facile and low-cost hydrothermal route. The as-prepared composite were characterized by XRD, SEM, TEM, UV-vis DRS, FT-IR, TG-DSC and BET. The relationship between the hierarchical structured, chemical composition and the surface features of the composite was discussed through a various kind's characterization analysis. The photocatalytic activities of the CaWO4Bi2WO6composite were evaluated for the degradation of Rhodamine B (RhB) dye and4-nitrophenol (4-NP) in aqueous solution under visible-light irradiation (>420nm), which were4.5times and2.5times higher than that of the pure Bi2WO6, respectively. The CaWO4/Bi2WO6composite still showed the high photocatalytic activity after four reaction cycles. On the basis of the calculated energy band positions, the mechanism of enhanced photocatalytic activity for the CaWO4/Bi2WO6composite can be attributed to the effective separation of electron-hole pairs.
To further improve the photocatalytic activities of the Bi2WO6, the hierarchically structured a-Fe2O3/Bi2WO6composite was synthesized by a hydrothermal route. The as-prepared samples were characterized by XRD, SEM, TEM, FT-IR, XPS and BET. The a-Fe2O3/Bi2WO6composite exhibited a strong adsorption capability and a higher visible light photocatalytic activity than the pure Bi2WO6for the photocatalytic degradation of acid red G dye or RhB dye. On the basis of the experimental results and calculated energy band positions, the enhanced photocatalytic activity of the composite can be attributed to the hierarchical structure and the coupling effect of a-Fe2O3and Bi2WO6in the composite.
To further improve the adsorption capability of the Bi2WO6, the Bi2WO6/rectorite composites were prepared by a sol-gel method. The relationship between the layer structured and the surface features of the composite was investigated by XRD, SEM, TEM, FT-IR, XPS and BET. The results showed that the composites exhibited a strong adsorption capability and a higher photocatalytic degradation activity for4BS dye, which could be attributed to the synergetic effects of the adsorbability of rectorite and the photocatalytic property of Bi2WO6in it.
The novel, efficient, plasma photocatalytic materials was also exploring at the last part. The visible-light-responsive Ag-Ag6Si2O7photocatalyst was synthesized using sodium silicate and silver nitrate as raw materials by a facile microwave method or ion-exchange method and subsequently light-induced reduction route. The Ag-Ag6Si2O7spherical composite exhibited a higher visible light photocatalytic activity for the photocatalytic degradation of MB dye in aqueous solution, which was attributed to the surface plasmon and the polarized field of the Ag6Si2O7photocatalyst. The results showed that h+and O2·-were involved as the active species in the photocatalytic reaction. A possible photocatalytic mechanism and the photocatalytic stability were discussed.
引文
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