太阳能光催化剂的制备及其光催化性能的研究
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摘要
近几年,光催化已经成为光化学反应的一个前沿领域,在处理各种生物难降解有机废水方面有很广阔的应用前景。如何制备能响应于太阳光的光催化剂和如何推广其实际应用成为了当今光催化研究的主攻方向。当前研究主要集中在以下两个方面:一、探索高比表面积光催化材料的合成方法,提高光催化剂对废水中污染物的吸附能力,从而提高光催化材料对废水中污染物的光催化降解能力。二、选择合适的且能响应于太阳光的光催化材料,为光催化氧化的实际应用化提供可能。
以下是每一部分的具体内容:
第一章概述了光催化氧化对废水污染物的降解机理、特点以及应用范围,并介绍了TiO_2作为光催化材料的研究现状及其弊端,以及响应于太阳光的光催化剂作为潜在光催化剂的优势。最后提出了自己对光催化氧化技术的实际应用化的设想和方法。
第二章在聚乙二醇/环己烷/水的水包油(O/W)乳浊液体系中,成功地合成了80 - 120 nm的CdS纳米空心球,通过XRD, SEM,TEM和UV-Vis等测试手段对该光催化剂进行了表征。本文还对其形成机理进行了初步探讨。并以亚甲基兰溶液为模拟染料废水,以太阳光为光源,研究了其光催化活性。结果表明,仅60 min亚甲基兰就几乎完全被光催化降解。
第三章是利用柠檬酸络合法和固相法来制备光催化剂SrCoO_x。通过XRD分析,确定合成的SrCoO_x粉体具有六方晶体结构。根据样品SrCoO_x的紫外漫反射分析,确定其具有良好的光吸收特性。并以碱性臧花红溶液为模拟染料废水,以太阳为光源,研究了其光催化活性。结果表明发现柠檬酸络合法比固相研磨法所制备的SrCoO_x光催化活性好,光照仅4.5 h,染料降解率就达95.2%。
第四章分为三部分:
1.本节采用高温固相煅烧的方法制备了Bi_(38)ZnO_(58)光催化纳米材料。用紫外-可见分光光度计对该光催化剂的光吸收特性进行测定,发现Bi_(38)ZnO_(58)光催化剂在紫外光区和可见光区均有较强的光吸收特性。本实验以亚甲基兰溶液作为被降解物质,以太阳光为光源来研究该催化剂的光催化活性。测试结果表明,Bi_(38)ZnO_(58)光催化剂对亚甲基兰溶液具有较强的光催化降解性能,4 h就可将亚甲基兰近乎完全催化降解。而且此光催化剂也可被循环使用,循环使用5次后,Bi_(38)ZnO_(58)样品的晶体结构基本没变,其光催化效率仍保持在98%以上,显示出该催化剂具有良好的稳定性。
2.本节在聚乙二醇/环己烷/水的乳液体系中,在超声条件下制备了砖形BiVO_4微米棒光催化材料,并通过XRD、SEM、TEM和UV-Vis等测试手段对该光催化剂进行了表征。结果表明,用该法制备的由BiVO_4纳米粒子构成的砖形微米棒光催化材料,在紫外和可见光区均有较强的光吸收性能。并对其形成机理进行了初步探讨。以亚甲基兰作为被降解物质,在太阳光照射下来研究其光催化活性,发现BiVO_4对亚甲基兰有较强的降解作用,60 min就可将亚甲基兰近乎完全的光催化降解,这使得该光催化剂具有了广阔的应用前景。
3.本节采用固相法制备了Bi_(20)MoO_(33)光催化材料,并通过XRD,SEM和UV-Vis等测试手段对该光催化剂进行了表征。结果表明,用该法制备的Bi_(20)MoO_(33)光催化剂在紫外和可见光区均有较强的光吸收性能。以亚甲基兰作为被降解物质,在太阳光照射下来研究其光催化活性,发现Bi_(20)MoO_(33)对亚甲基兰有较强的降解作用,8 h亚甲基兰降解率达到84%。
In recent years, photocatalysis has been a one-up field in photochemistry, and has widely applied foreground in disposing organic waste water. Now, it is the major research direction how to synthesize the sunlight-driven photocatalysts and further apply the photocatalysts to the wastewater treatment. The current reseach is focused on the following two aspects: one is the exploring synthesis methods of photocatalysts with high specific surface areas, and promoting the adsorption properties of the synthesized phtocatalysts, and consequently promoting photocatalytic degradation activities of the photocatalysts on the pollutants; and the other is how to selecte the sunlight-driven photocatalysts and make it applicable to use photocatalytic oxidation technique in real waste water treatment.
The thesis can be divided into four parts: the first chapter is the research grounds of photocatalysis; The second is the study on the synthesis of CdS hollow spheres and their photocatalytic properties; The third is the study of effects of different synthesis methods on the photocatlytic properties of SrCoO_x; And the forth is the study of the preparation of compound metal oxidation containing bismuth and their photocatalytic properties.
The following is the concrete contents of every chapter:
The purpose of the first chapter is to summarize the fundamental principles, characterizations and applied ranges of photocatalysis, further to investigate the research actuality of TiO_2 as photocatalyst and its defects,and the advantages of sunlight-driven photocatalysts as potential photocatalysts. Based on the above overviews, I put forth my tentative plans and some ideas to apply photocatalytic oxidation techniques to real application.
In the second chapter, CdS hollow spheres with the diameter of 80-120 nm were successfully synthesized in the system of oil in water emulsion and characterized by the XRD, SEM, TEM and UV-Vis technologies. The formation mechanism of CdS hollow spheres was also discussed. The photocatalytic activity of CdS hollow spheres has been tested on the decomposable substrate methylene blue under sunlight illumination. Test results showed that methylene blue was completely decomposed within just 60 min.
In the third chapter, SrCoO_x photocatalysts were successfully synthesized by using the different synthesis methods of citric acid complex method and the solid-phase method. SrCoO_x powders have hexagonal crystal system structure through XRD analysis. Through UV-Vis reflectance spectra, it can be seen that the synthesized products have good photo absorption properties. Using sun as light source, the decomposition experiments of water soluble dye safranine T were carried out in the suspension liquid with SrCoO_x to investigate the photocatalytic properties of SrCoO_x. The results showed showed that SrCoO_x showed stronger photocatalytic activity by using citric acid complex method than that of SrCoO_x by using solid-phase method, and the dye decolorization ratio is up to 95.2% through 4.5 h under sunlight irradiation, which demonstrated that SrCoO_x phtocatalysts have good photocatalytic property.
The forth chapter was divided into three parts:
1. Bi_(38)ZnO_(58) was successfully synthesized by means of solid state reaction method. The photo-absorption property was determined by UV-Vis diffuse reflectance spectrum, from which it could be seen that Bi_(38)ZnO_(58) owned much strong photo-absorption property both in the ultraviolet and visible light regions. The photocatalytic activity of Bi_(38)ZnO_(58) was tested on methylene blue solution under sunlight illumination. The test results showed that methylene blue was nearly completely degraded after 4 h, which confirmed the high photocatalytic activity of the photocatalyst. Moreover, the crystal structure of Bi_(38)ZnO_(58) was still unvaried and its photocatalytic efficiency was still above 98% even after being reused for five times, which demonstrated the high stability of the photocatalyst.
2. In this chapter, BiVO_4 micro-rods with brick shape were successfully synthesized in the system of polyglycol/cyclohexane/water emulsion and under ultrasonic condition, and characterized by the XRD、SEM、TEM and UV-Vis technologies. BiVO_4 micro-rods with brick shape, which were composed of nano-particles, have strong photo-absorption property both in the UV region and the visible light region. The formation mechanism of BiVO_4 micro-rods was also discussed tentatively. The photocatalytic activity of BiVO_4 micro-rods had been tested on the decomposable substrate methylene blue under sunlight illumination. Test results revealed that methylene blue was completely decomposed within just 60 min, which made the catalyst have greatly potential applications.
3. In this chapter, Bi_(20)MoO_(33) photocatalysts were successfully synthesized by the solid-state reaction method, and characterized by the XRD、SEM and UV-Vis technologies. Test results showed that Bi_(20)MoO_(33) photocatalyst has strong photo-absorption property both in the UV region and the visible light region. The photocatalytic activity of Bi_(20)MoO_(33) photocatalyst had been tested on the decomposable substrate methylene blue under sunlight illumination. Test results revealed that the degradation ratio of methylene blue was up to 84% through 8 h under sunlight irradiation, which made photocatalyst have greatly potential applications.
以下是每一部分的具体内容:
第一章概述了光催化氧化对废水污染物的降解机理、特点以及应用范围,并介绍了TiO_2作为光催化材料的研究现状及其弊端,以及响应于太阳光的光催化剂作为潜在光催化剂的优势。最后提出了自己对光催化氧化技术的实际应用化的设想和方法。
第二章在聚乙二醇/环己烷/水的水包油(O/W)乳浊液体系中,成功地合成了80 - 120 nm的CdS纳米空心球,通过XRD, SEM,TEM和UV-Vis等测试手段对该光催化剂进行了表征。本文还对其形成机理进行了初步探讨。并以亚甲基兰溶液为模拟染料废水,以太阳光为光源,研究了其光催化活性。结果表明,仅60 min亚甲基兰就几乎完全被光催化降解。
第三章是利用柠檬酸络合法和固相法来制备光催化剂SrCoO_x。通过XRD分析,确定合成的SrCoO_x粉体具有六方晶体结构。根据样品SrCoO_x的紫外漫反射分析,确定其具有良好的光吸收特性。并以碱性臧花红溶液为模拟染料废水,以太阳为光源,研究了其光催化活性。结果表明发现柠檬酸络合法比固相研磨法所制备的SrCoO_x光催化活性好,光照仅4.5 h,染料降解率就达95.2%。
第四章分为三部分:
1.本节采用高温固相煅烧的方法制备了Bi_(38)ZnO_(58)光催化纳米材料。用紫外-可见分光光度计对该光催化剂的光吸收特性进行测定,发现Bi_(38)ZnO_(58)光催化剂在紫外光区和可见光区均有较强的光吸收特性。本实验以亚甲基兰溶液作为被降解物质,以太阳光为光源来研究该催化剂的光催化活性。测试结果表明,Bi_(38)ZnO_(58)光催化剂对亚甲基兰溶液具有较强的光催化降解性能,4 h就可将亚甲基兰近乎完全催化降解。而且此光催化剂也可被循环使用,循环使用5次后,Bi_(38)ZnO_(58)样品的晶体结构基本没变,其光催化效率仍保持在98%以上,显示出该催化剂具有良好的稳定性。
2.本节在聚乙二醇/环己烷/水的乳液体系中,在超声条件下制备了砖形BiVO_4微米棒光催化材料,并通过XRD、SEM、TEM和UV-Vis等测试手段对该光催化剂进行了表征。结果表明,用该法制备的由BiVO_4纳米粒子构成的砖形微米棒光催化材料,在紫外和可见光区均有较强的光吸收性能。并对其形成机理进行了初步探讨。以亚甲基兰作为被降解物质,在太阳光照射下来研究其光催化活性,发现BiVO_4对亚甲基兰有较强的降解作用,60 min就可将亚甲基兰近乎完全的光催化降解,这使得该光催化剂具有了广阔的应用前景。
3.本节采用固相法制备了Bi_(20)MoO_(33)光催化材料,并通过XRD,SEM和UV-Vis等测试手段对该光催化剂进行了表征。结果表明,用该法制备的Bi_(20)MoO_(33)光催化剂在紫外和可见光区均有较强的光吸收性能。以亚甲基兰作为被降解物质,在太阳光照射下来研究其光催化活性,发现Bi_(20)MoO_(33)对亚甲基兰有较强的降解作用,8 h亚甲基兰降解率达到84%。
In recent years, photocatalysis has been a one-up field in photochemistry, and has widely applied foreground in disposing organic waste water. Now, it is the major research direction how to synthesize the sunlight-driven photocatalysts and further apply the photocatalysts to the wastewater treatment. The current reseach is focused on the following two aspects: one is the exploring synthesis methods of photocatalysts with high specific surface areas, and promoting the adsorption properties of the synthesized phtocatalysts, and consequently promoting photocatalytic degradation activities of the photocatalysts on the pollutants; and the other is how to selecte the sunlight-driven photocatalysts and make it applicable to use photocatalytic oxidation technique in real waste water treatment.
The thesis can be divided into four parts: the first chapter is the research grounds of photocatalysis; The second is the study on the synthesis of CdS hollow spheres and their photocatalytic properties; The third is the study of effects of different synthesis methods on the photocatlytic properties of SrCoO_x; And the forth is the study of the preparation of compound metal oxidation containing bismuth and their photocatalytic properties.
The following is the concrete contents of every chapter:
The purpose of the first chapter is to summarize the fundamental principles, characterizations and applied ranges of photocatalysis, further to investigate the research actuality of TiO_2 as photocatalyst and its defects,and the advantages of sunlight-driven photocatalysts as potential photocatalysts. Based on the above overviews, I put forth my tentative plans and some ideas to apply photocatalytic oxidation techniques to real application.
In the second chapter, CdS hollow spheres with the diameter of 80-120 nm were successfully synthesized in the system of oil in water emulsion and characterized by the XRD, SEM, TEM and UV-Vis technologies. The formation mechanism of CdS hollow spheres was also discussed. The photocatalytic activity of CdS hollow spheres has been tested on the decomposable substrate methylene blue under sunlight illumination. Test results showed that methylene blue was completely decomposed within just 60 min.
In the third chapter, SrCoO_x photocatalysts were successfully synthesized by using the different synthesis methods of citric acid complex method and the solid-phase method. SrCoO_x powders have hexagonal crystal system structure through XRD analysis. Through UV-Vis reflectance spectra, it can be seen that the synthesized products have good photo absorption properties. Using sun as light source, the decomposition experiments of water soluble dye safranine T were carried out in the suspension liquid with SrCoO_x to investigate the photocatalytic properties of SrCoO_x. The results showed showed that SrCoO_x showed stronger photocatalytic activity by using citric acid complex method than that of SrCoO_x by using solid-phase method, and the dye decolorization ratio is up to 95.2% through 4.5 h under sunlight irradiation, which demonstrated that SrCoO_x phtocatalysts have good photocatalytic property.
The forth chapter was divided into three parts:
1. Bi_(38)ZnO_(58) was successfully synthesized by means of solid state reaction method. The photo-absorption property was determined by UV-Vis diffuse reflectance spectrum, from which it could be seen that Bi_(38)ZnO_(58) owned much strong photo-absorption property both in the ultraviolet and visible light regions. The photocatalytic activity of Bi_(38)ZnO_(58) was tested on methylene blue solution under sunlight illumination. The test results showed that methylene blue was nearly completely degraded after 4 h, which confirmed the high photocatalytic activity of the photocatalyst. Moreover, the crystal structure of Bi_(38)ZnO_(58) was still unvaried and its photocatalytic efficiency was still above 98% even after being reused for five times, which demonstrated the high stability of the photocatalyst.
2. In this chapter, BiVO_4 micro-rods with brick shape were successfully synthesized in the system of polyglycol/cyclohexane/water emulsion and under ultrasonic condition, and characterized by the XRD、SEM、TEM and UV-Vis technologies. BiVO_4 micro-rods with brick shape, which were composed of nano-particles, have strong photo-absorption property both in the UV region and the visible light region. The formation mechanism of BiVO_4 micro-rods was also discussed tentatively. The photocatalytic activity of BiVO_4 micro-rods had been tested on the decomposable substrate methylene blue under sunlight illumination. Test results revealed that methylene blue was completely decomposed within just 60 min, which made the catalyst have greatly potential applications.
3. In this chapter, Bi_(20)MoO_(33) photocatalysts were successfully synthesized by the solid-state reaction method, and characterized by the XRD、SEM and UV-Vis technologies. Test results showed that Bi_(20)MoO_(33) photocatalyst has strong photo-absorption property both in the UV region and the visible light region. The photocatalytic activity of Bi_(20)MoO_(33) photocatalyst had been tested on the decomposable substrate methylene blue under sunlight illumination. Test results revealed that the degradation ratio of methylene blue was up to 84% through 8 h under sunlight irradiation, which made photocatalyst have greatly potential applications.
引文
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