摘要
随着人类社会的发展,环境污染日益严重,因此环境污染问题,特别是室内污染问题日益引起人们的关注。众所周知,人生大约70%是在室内度过的,而室内的污染相对于室外高出很多倍。挥发性有机物(VOCs)被广泛的应用于工业和室内装修,其广泛的应用必然导致了水和空气的污染,特别是对室内污染更大。光催化剂在去除环境污染有很多优点,因此近年来采用光催化剂去除环境污染受到人们极大的重视。
二氧化钛是一种比较常用的光催化剂,其具有稳定性高,催化活性高,无毒和便宜的优点,因此在环境污染处理中受到极大的关注。然而二氧化钛亦有很多缺点,太阳光利用率低,粒子回收困难,容易失活,而且当污染物浓度比较低的时候,光催化仅发生在催化剂附近等。因此需要研究新的催化剂和催化剂复合材料,以提高催化剂的性能。
本文的主要研究内容和结果如下：
(1)采用水热合成法,以Cu(NO3)2为原料,乙二醇为溶剂和还原剂,聚乙烯吡咯烷酮k30(PVP)为表面活性剂,一步合成具有可见光响应的Cu-Cu2+1O金属半导体复合材料。表征结果显示产物由两种不同尺寸粒子构成,其中大的粒了为Cu,直径为50nm,小的粒子为Cu2+10,直径为20nm。表面活性剂PVP的加入降低Cu2+1O的结晶度,提高了铜的含量,并影响两种粒子的尺寸分布和界面结合情况,因而影响产物的催化性能。催化活性测试结果表明,Cu-Cu2+1O金属半导体复合材料具有可见光催化活性,其对苯酚降解符合一级反应动力学。并采用Cu(NO3)2为原料,明胶为分散剂,Na2SO3为还原剂,活性炭为负载剂,采用原位沉淀法实现活性炭负载复合型Cu2O/AC光催化剂的制备,测试结果显示活性炭的加入影响了产物的相结构,而禁带宽度没有受到影响。以苯酚为模型,光催化测试结果显示,复合型Cu2O/AC光催化剂的催化活性高于Cu2O,原因可能是活性炭和Cu2O存在吸附催化协同作用,其导致了产物催化活性的提高。
(2)合成两类不同的介孔氧化镍。以硝酸镍为原料,氢氧化钠为沉淀剂,十二烷基苯磺酸钠(SDBS)为表面活性剂,采用水热合成法制备具有介孔结构的纳米片状p型氢氧化镍,将介孔结构的纳米片状β型氢氧化镍焙烧即可以获得相同形貌的纳米氧化镍。XRD测试结果显示纳米片状氧化镍是体心立方结构,电子衍射显示其为单晶结构,而且氢氧化镍也是单晶结构,氧化镍的比表面积为85.98m2/g,具有介孔结构。以苯酚为模型,光催化测试结果显示,片状氧化镍具有一定的催化活性,但很容易失活。花状氧化镍的合成。在不添加任何模板和表面活性剂条件下,采用均匀沉淀法制备出具有自组装结构的花状α型Ni(OH)2,并以其为前驱体,通过焙烧即可获得同样具有花状结构的氧化镍。测试结果显示,所制备的氧化镍比表面积是125.2m2/g.其禁带宽度为4.43eV。光催化测试结果显示花状氧化镍对甲基橙的有较高的光催化降解性能。
(3)控制合成氢氧化钢并制备氢氧化铟—活性炭复合材料。首先,以硝酸钢为原料,尿素为沉淀剂,十六烷基溴化铵(CTAB)为软模板剂,采用一步一点法制备具有介孔结构的纳米棒状氢氧化钢。测试结果显示：样品都是长度为300nm宽度为90nm的棒状有孔结构,低温液氮吸附技术证实了样品是具有介孔结构的材料,其平均孔径为3.1nm。光学测试显示,其禁带宽度为5.15eV,其具有较强的荧光性能,在紫外激发下具有两个比较强的光谱带。并且还探讨了纳米棒状成因和CTAB对形成氢氧化铟板状结构的作用。而后继工作发现通过控制反应条件,不使用CTAB作为模板,在低温条件下(70℃)也可获得形貌和尺、J‘可控的纳米氢氧化钢。例如时间、浓度以及沉淀剂种类,即可控制反应产物的形貌和粒了尺寸的大小。氢氧化铟可能的形貌控制机理也被讨论。催化测试显示：其对气态苯的光催化降解与二氧化钛相比,所制备的样品也显示出更高的催化活性。以In(NO3)3·4.5H2O和六亚甲基四胺(HMT)为原料,采用水热合成出具有介孔结构的块状氢氧化铟。其具有较高的比表面积,其比表面积为97.04m2/g。对甲苯的光催化测试结果显示,其具有较高的催化活性而且催化活性很稳定。最后,以In(NO3)3·4.5H2O和六亚甲基四胺为原料,采用水热合成法制备了氢氧化铟—活性炭复合材料。测试结果显示,活性炭的加入影响了晶体结构和粒径大小。活性炭的加入没有影响氢氧化钢粒子形貌。氢氧化钢是以化学键的形式负载在活性炭上而且多孔活性炭并没有影响氢氧化铟的禁带宽度。对甲苯的催化测试显示含量3%的氢氧化铟—活性炭复合材料具有最高的催化活性。
(4)采用丝网印刷技术制备了二氧化钛/活性炭纤维复合光催化剂。通过XRD和SEM测试显示,复合催化剂内的二氧化钛的相是锐钛矿结构,活性炭纤维的存在没有影响二氧化钛的相结构。SEM显示二氧化钛在活性炭纤维表面形成薄膜。对苯的光催化测试显示复合材料的光催化性能要高于二氧化钛的催化活性。
The environmental pollution is increasingly serious with the development of human society so that the pollution of the environment, especially in door, caused the attention of people increasingly. It has been well known that majority of people spend approximately70%of their time in the indoor environments, such as residences, public buildings and offices. The levels of indoor air pollutants can be several hundred times higher than that of outdoor ones. The volatile organic compounds (VOCs) are widely used in industrial process and domestic activities. These extensive uses lead to water and air pollution, particularly in indoor pollution. The photocatalytic oxidation technology has increasingly been paid great attention to in recent years because photocatalysts in the removal of environmental pollution have a lot of advantages.
Titanium dioxide(TiO2) have been extensively studied for environmental purification applications, due to its good characteristics of powerful oxidation strength, chemicalstability, nontoxicity and inexpensiveness. However, there are certain shortcomings associated with conventional TiO2powders catalysts, including an inefficient use of light, difficulty experienced during both stirring and separation of the catalyst from the reaction medium, rapidly losed activation, and the occurrence of low-concentration contamination near TiO2during the photocatalytic process. It may be a good strategy to extend the research using other classes of photocatalysts for improvement of the system efficiency or using the new composite materials.
The main research contents and results were summarized as follows:
1.Visible-light response Cu-Cu2+1O metal-semiconductor nanocrystals composites were successfully synthesized by using hydrothermal synthesis methods with Cu(NO3)2as starting materials, ethylene glycol (EG) as the solvent and reducing agent, and polyvinypyrrolidone k30(PVP) as surfactant. The photocatalytic performance was tested through the degradation of phenol under xenon lamp irradiation. The characterization results showed that the products were composed of two different sizes of particles. The larger particle with the diameter of50nm was Cu and the smaller particle with the diameter of20nm was Cu2+1O. The content of Cu2+1O was decreased and that of Cu was improverd when PVP was added. The distribution and integration of Cu and CU2+1O particles were also affected so that the photocatalytic activity was affected. Activity results showed that Cu-Cu2+1O particles could degrade phenol and the kinetics fits a first-order reaction. Cu2O/AC (porous activated carbon) composite photocatalysts were also prepared by an insitu method with Cu(NO3)2as starting materials, glutin as dispersant, and AC as a carrier of Cu2O. The crystal structure, spectra characteristics, and surface properties of the obtained catalysts were characterize in order to study the influence of AC on the composite photocatalysts. The results showed that the adding of actived carbon can affect the phase structure of composite photocatalysts. The energy band of Cu2O was had no effect on when actived carbon was added. The photocatalytic activity of the prepare Cu2O/AC and Cu2O for phenol degradation were investigated under visible light irradiation. The results showed the photocatalytic activity of the prepare Cu2O/AC was higher than that of the prepare CU2O/AC under visible light irradiation. It was attributed to the synergistic effect between porous activated carbon and Cu2O.
2. The single-crystalline nickel oxide (NiO) mesoporous nanosheets and the flowerlike nickel oxide (NiO) were prepared, respectively. At first, the mesoporous nanosheets of single-crystalline β-nickel hydroxide (β-Ni(OH)2) were successfully synthesized via a facile hydrothermal method using Ni(NO3)2·6H2O as precursor in a mixed solution of sodium hydroxide (NaOH) and sodium dodecylbenzenesulfonate (SDBS). Then, single-crystalline nickel oxide (NiO) mesoporous nanosheets could be obtained through a thermal decomposition method using β-Ni(OH)2mesoporous nanosheets as precursor. The prepared NiO was body centred cubic structure.The prepared NiO was single-crystalline and its specific surface area was85.98m2/g. The photocatalytic degradation of phenol showed that the prepared NiO has the photocatalytic activity but it lose catalytic activity soon. The flowerlike nickel oxide (NiO) was also synthesized. The flowerlike a-nickel hydroxide (Ni(OH)2), being used as the precursor of the nickel oxide, was successfully synthesized by homogeneous precipitation method without using any templates or surfactants. Flowerlike nickel oxide (NiO) with the similar flowerlike structure can be obtained by further calcination of the prepared Ni(OH)2at400℃for2h. The results showed that the specific surface area of flowerlike NiO was125.2m2/g and the band gap energy of it was4.43eV. The flowerlike NiO have higher photocatalytic property to decompose Methyl orange pollutant.
3. The morphology-and size-controlled ln(OH)3and ln(OH)3/AC (porous activated carbon) composite photocatalysts were successfully prepared. First, Mesoporous indium hydroxide nanorods were successfully synthesized by a mild one-step one-pot method.There are some pores in the samples, which are mainly composed of rod-like shapes with length of300nm and diameter of90nm. N2adsorption/desorption measurements confirmed that the prepared powder is mesoporous with average pore diameter of3.1nm. The ultraviolet-visible absorption spectroscopy analysis indicated that the band gap energy of the samples is5.15eV. Photoluminescence spectrum showed that there are two stronger emissions under ultraviolet light irradiation. The growth mechanism of indium hydroxide nanorods and the role of cetyltrimethyl ammonium bromide were also discussed. Then, the morphology-and size-controlled In(OH)3nanocrystals have been synthesized via a novel, low-cost and low-temperature(70℃) route without using CTAB as surfactant. The morphology and size of In(OH)3nanostructures can be controlled by adjusting the reaction conditions, such as the reaction time, concentration of the alkali and the alkaline source. A possible mechanism for the evolution of the morphology-and size-controlled In(OH)3was proposed. The photocatalytic degradation of phene showed that the ln(OH)3have higher photocatalytic activity than TiO2(p-25). Mesoporous nanosheets of ln(OH)3with high specific surface area were also successfully synthesized via a facile hydrothermal method using In(NO3)3and hexamethylene tetramine(HMT) as raw materials. The photocatalyst sample is highly photoactive and stable for gas-phase removal of toluene under UV irradiation.In the end, In(OH)3/AC (porous activated carbon) composite photocatalysts were prepared via a facile hydrothermal method using In(NO3)3and hexamethylene tetramine(HMT) as raw materials and AC as a carrier. The results showed that the doped of actived carbon can affect the crystal structure and the size of In(OH)3. TEM results showed that the morphology of In(OH)3were not affected when actived carbon was added.The DRS results showed that the energy band of In(OH)3was had no effect on when actived carbon was added. Results of FT-IR showed that the AC and In(OH)3were connected by chemical bond. The photocatalytic degradation of toluene showed that In(OH)3/AC catalysts with optimal AC content3%exhibited higher activity than other In(OH)3/AC catalysts,
4. The TiO2/ACF composite photocatalyst was prepared by using the screen printed technology. The results of XRD showed the TiO2/ACF composite photocatalyst is confirmed anatase as the only phase present and ACF has no effects on the phase structures of TiO2. The results of SEM showed that TiO2can form thin film on ACF surface. Benzene was chosen as the model of the volatile organic compounds (VOCs) to investigate the capability of TiO2/ACF composite photocatalyst. The results showed that the TiO2/ACF composite photocatalyst have higher activity for benzene removal than only TiO2photocatalyst.
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