介孔氧化钛磁负载光催化剂的制备及应用基础研究
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摘要
介孔氧化钛因其具有丰富的孔道结构、较高的比表面积、更多的催化活性位和更高的光催化活性而倍受关注。然而,纳米级介孔氧化钛光催化剂的固液分离是实际应用过程中面临的难题之一。通常,将纳米氧化钛负载于载体表面,以解决固液分离和活性组分易流失的问题。但是,由于载体对光源的遮蔽和色散效应,会降低光源能量的利用效率。将纳米级磁性颗粒作为光催化剂的载体,不仅可以减少载体对光源的遮蔽和色散效应,而且还可以使光催化剂保持较高的光催化活性,同时磁负载后的光催化剂在外加磁场条件下易于固液分离、实现光催化剂的快速高效回收和再利用。然而,磁负载光催化剂研究过程中也出现了两类问题,其一：在光催化剂内引入磁性材料,极易导致光降解过程中“photodissolution"的发生,从而影响磁负载光催化剂的稳定性；其二：磁负载光催化剂相对于纯组分的氧化钛光催化剂的光催化活性偏低。针对这些问题的研究一直在进行中,已证实前者可以在磁性核和活性组分之间引入惰性中间层(如氧化硅或氧化铝)阻止“photodissolution"的发生。针对后者,有不少学者尝试采用磁负载光催化剂的壳层中掺杂贵金属(如银或铂)或者增加比表面积(如引入活性炭或制成中空球)的方式提高光催化效率。目前,如何提高磁负载光催化剂的催化活性仍是该领域研究的热点问题。
本论文提出制备具有介孔壳结构的磁负载光催化剂,其介孔壳结构可以提高比表面积,增加光催化反应物在孔道内的吸附和扩散,从而提高磁负载光催化剂的催化活性。
本论文首先采用水热法制备了具有超顺磁特征的尖晶石铁酸镍纳米颗粒,其次应用溶胶-凝胶法对铁酸镍颗粒包覆氧化硅惰性层,再经过溶剂热合成路线制备了氧化钛／氧化硅／铁酸镍复合光催化剂。最后,以硝基苯为模拟污染物,对制备的介孔结构磁负载光催化剂的光催化活性和稳定性进行评价。
采用湿化学法制备了Ti02/Si02/NiFe204磁负载光催化剂,样品采用X-电子衍射(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)、N2吸附-脱附、振动样品磁场计(VSM)等手段进行了表征。结果表明制备得Ti02/Si02/NiFe2O4磁负载光催化剂具有明显的壳／核型结构,颗粒分布均匀,呈超顺磁性。颗粒大小约50nm,壳层氧化钛为结晶度高的锐钛型,最佳实验条件下,其BET比表面积达145m2/g,平均孔径为5.28nm,孔容约为0.16 cm3/g。
以硝基苯为模拟污染物,对TiO2/SiO2/NiFe2O4磁负载光催化剂进行了光催化性能评价。结果表明在UV/H2O2光降解条件下,18.8%包覆量的磁负载光催化剂性能最优,具有良好的光催化活性,300min时TOC去除率达90%,其拟一级反应速率常数是P25光催化剂的1.75倍。在外加磁场条件下,该介孔磁载光催化剂在30s可全部聚集回收。重复性实验表明制备的磁负载光催化剂具有良好的磁回收性能和稳定性。
采用色质联用技术对UV/H2O2光降解硝基苯过程中间产物和离子碎片进行检测,对UV/H2O2与硝基苯反应途径进行探讨。认为硝基苯的光催化降解分为两种途径,即羟基自由基进攻使苯环羟基化,然后是羟基化的苯环发生开裂而逐步降解,或者先发生脱硝基反应再使苯环羟基化,最终均转化成各种脂肪族化合物或进一步矿化成二氧化碳和水。提出的硝基苯光催化降解的可能途径为：
通过对TiO2/SiO2/NiFe2O4磁负载光催化剂的形成过程进行系统分析,探讨了TiO2/SiO2/NiFe2O4的介孔结构壳／核结构光催化剂的可能的形成机制如下：
Mesoporous TiO2 has been drawn more attention because of its abundant porous structure, large specific surface area and more cataystic active sites. However, the separation and recovery of suspended small nanostructure TiO2 particles from treated water is very difficult to operate in the practical application process. Usually, small TiO2 particles are immobilized onto a carrier to solve the problem of TiO2 particles separation from liquid phase and avoiding the loss of active component. Unfortunately, a significant loss of photocatalytic activity was generally reported due to greatly reducing surface area after immobilization, shadowing and the dispersion effect. The incorporation of magnetic carrier into nanostructure TiO2 provides an alternative way to solve this problem because of its small diameter. Compared to conventional supported TiO2 photocatalysts, the submicron sizes of the magnetic photocatalyst provide a larger surface area, which subsequently enables higher efficiency in photocatalytic degradations. However, there are two major problems in employing TiO2 coated magnetic materials as a photocatalyst. The first obstacle is a photo-dissolution phenomenon, which may affect the stabilization of magnetic photocatalyst due to the electronic interaction happening between TiO2 coating and the magnetic core. To overcome this problem, an inertial layer (SiO2 or Al2O3) between the TiO2 and magnetic materials was proposed. The second obstacle is the low photocatalystic activity due to low specific area arising from heat treatment of sintering, which is to increase the crystallinity of TiO2 particles. Many researches have tried to enhance the photocatalystic activity by loading the noble metal such as Ag and Pt, and the specific area of shell layer of magnic catalyst and so on. To improve the activity of magnetic photocatalyst is still a hot problem.
In the dissertation, Mesoporous magnetic photocatalyst was proposed to enhance the specific surface area and more cataystic active sites, which can increase the reactant adsorption and disperse in the porous structure.
The spinel structure nickel ferrete with superparamagnetism nature was firstly prepared by using hydrothermal method, and then its surface was coated with the silica inert layer via the sol-gel method. Finally, TiO2/SiO2/NiFe2O4 composite photocatalysts was prepared by using solvothermal method. Taking nitrobenzene as a simulating pollutant, the photocatalysis avtivities and stabilization of the prepaired mesoporous magnetic photocatalyst has been appreciated.
The preparied magnetic TiO2/SiO2/NiFe2O4 composite photocatalysts by wet-chamical method was characterized by N2 adsorption-desorption, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). TiO2/SiO2/NiFe2O4 composite photocatalysts is spherical partical with shell/core structure, well distribution and superparamagnetism. The sample had an average size of about 50 nm in diameter with abundant mesopore structured anatase TiO2. Under the optimum experimental condition, the BET value is about 145m2/g, average pore size is 5.28 nm, and pore volume is 0.16 cm3/g.
The photocatalytic activity of TiO2/SiO2/NiFe2O4 particles was also investigated by the photocatalytic degradation coupled with H2O2 oxidation of nitrobenzene in aqueous solution. Experimental results showed that the sample with 18.8% TiO2 coating amount has the best photocatalytic performance.The TOC removal could amount to 90% during 300 min, the rate of degradation of TiO2/SiO2/NiFe2O4 composite catalyst was 1.75 times of the P25. The TiO2/SiO2/NiFe2O4 composite catalyst could be recovered completely within 30s. The repetitive experiments have been also carried out in the photodegradation solution, which indicated the photocatalyst has good recovered ability and stabilization.
Based on the analyzing of the degradation products including fragment ions and intermediate products with GC-MS, the possible degradation pathways of nitrobenzene were also suggested. The possible reaction routes could be divided into two pathways:One is hydroxyl radical attacked phenyl ring to form phenolic compounds, then the ring was opened, forming into various aliphatic compounds; Another is hydroxyl radical attacked directly the nitro-proup and phenol and its derivatives were generated while the nitro-proup was released by the radical addition-elimination. In the subsequent degradation processes, the two pathways have experimenced similar reaction being mineralized to inorganic compounds such as carbon dioxide and water. The probable photodegradation pathways were proposed and discussed as follows.
The possible formation mechanism of mesopore shell/core structured photocatalyst TiO2/SiO2/NiFe2O4 has also been discussued as follows.
本论文提出制备具有介孔壳结构的磁负载光催化剂,其介孔壳结构可以提高比表面积,增加光催化反应物在孔道内的吸附和扩散,从而提高磁负载光催化剂的催化活性。
本论文首先采用水热法制备了具有超顺磁特征的尖晶石铁酸镍纳米颗粒,其次应用溶胶-凝胶法对铁酸镍颗粒包覆氧化硅惰性层,再经过溶剂热合成路线制备了氧化钛／氧化硅／铁酸镍复合光催化剂。最后,以硝基苯为模拟污染物,对制备的介孔结构磁负载光催化剂的光催化活性和稳定性进行评价。
采用湿化学法制备了Ti02/Si02/NiFe204磁负载光催化剂,样品采用X-电子衍射(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)、N2吸附-脱附、振动样品磁场计(VSM)等手段进行了表征。结果表明制备得Ti02/Si02/NiFe2O4磁负载光催化剂具有明显的壳／核型结构,颗粒分布均匀,呈超顺磁性。颗粒大小约50nm,壳层氧化钛为结晶度高的锐钛型,最佳实验条件下,其BET比表面积达145m2/g,平均孔径为5.28nm,孔容约为0.16 cm3/g。
以硝基苯为模拟污染物,对TiO2/SiO2/NiFe2O4磁负载光催化剂进行了光催化性能评价。结果表明在UV/H2O2光降解条件下,18.8%包覆量的磁负载光催化剂性能最优,具有良好的光催化活性,300min时TOC去除率达90%,其拟一级反应速率常数是P25光催化剂的1.75倍。在外加磁场条件下,该介孔磁载光催化剂在30s可全部聚集回收。重复性实验表明制备的磁负载光催化剂具有良好的磁回收性能和稳定性。
采用色质联用技术对UV/H2O2光降解硝基苯过程中间产物和离子碎片进行检测,对UV/H2O2与硝基苯反应途径进行探讨。认为硝基苯的光催化降解分为两种途径,即羟基自由基进攻使苯环羟基化,然后是羟基化的苯环发生开裂而逐步降解,或者先发生脱硝基反应再使苯环羟基化,最终均转化成各种脂肪族化合物或进一步矿化成二氧化碳和水。提出的硝基苯光催化降解的可能途径为：
通过对TiO2/SiO2/NiFe2O4磁负载光催化剂的形成过程进行系统分析,探讨了TiO2/SiO2/NiFe2O4的介孔结构壳／核结构光催化剂的可能的形成机制如下：
Mesoporous TiO2 has been drawn more attention because of its abundant porous structure, large specific surface area and more cataystic active sites. However, the separation and recovery of suspended small nanostructure TiO2 particles from treated water is very difficult to operate in the practical application process. Usually, small TiO2 particles are immobilized onto a carrier to solve the problem of TiO2 particles separation from liquid phase and avoiding the loss of active component. Unfortunately, a significant loss of photocatalytic activity was generally reported due to greatly reducing surface area after immobilization, shadowing and the dispersion effect. The incorporation of magnetic carrier into nanostructure TiO2 provides an alternative way to solve this problem because of its small diameter. Compared to conventional supported TiO2 photocatalysts, the submicron sizes of the magnetic photocatalyst provide a larger surface area, which subsequently enables higher efficiency in photocatalytic degradations. However, there are two major problems in employing TiO2 coated magnetic materials as a photocatalyst. The first obstacle is a photo-dissolution phenomenon, which may affect the stabilization of magnetic photocatalyst due to the electronic interaction happening between TiO2 coating and the magnetic core. To overcome this problem, an inertial layer (SiO2 or Al2O3) between the TiO2 and magnetic materials was proposed. The second obstacle is the low photocatalystic activity due to low specific area arising from heat treatment of sintering, which is to increase the crystallinity of TiO2 particles. Many researches have tried to enhance the photocatalystic activity by loading the noble metal such as Ag and Pt, and the specific area of shell layer of magnic catalyst and so on. To improve the activity of magnetic photocatalyst is still a hot problem.
In the dissertation, Mesoporous magnetic photocatalyst was proposed to enhance the specific surface area and more cataystic active sites, which can increase the reactant adsorption and disperse in the porous structure.
The spinel structure nickel ferrete with superparamagnetism nature was firstly prepared by using hydrothermal method, and then its surface was coated with the silica inert layer via the sol-gel method. Finally, TiO2/SiO2/NiFe2O4 composite photocatalysts was prepared by using solvothermal method. Taking nitrobenzene as a simulating pollutant, the photocatalysis avtivities and stabilization of the prepaired mesoporous magnetic photocatalyst has been appreciated.
The preparied magnetic TiO2/SiO2/NiFe2O4 composite photocatalysts by wet-chamical method was characterized by N2 adsorption-desorption, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). TiO2/SiO2/NiFe2O4 composite photocatalysts is spherical partical with shell/core structure, well distribution and superparamagnetism. The sample had an average size of about 50 nm in diameter with abundant mesopore structured anatase TiO2. Under the optimum experimental condition, the BET value is about 145m2/g, average pore size is 5.28 nm, and pore volume is 0.16 cm3/g.
The photocatalytic activity of TiO2/SiO2/NiFe2O4 particles was also investigated by the photocatalytic degradation coupled with H2O2 oxidation of nitrobenzene in aqueous solution. Experimental results showed that the sample with 18.8% TiO2 coating amount has the best photocatalytic performance.The TOC removal could amount to 90% during 300 min, the rate of degradation of TiO2/SiO2/NiFe2O4 composite catalyst was 1.75 times of the P25. The TiO2/SiO2/NiFe2O4 composite catalyst could be recovered completely within 30s. The repetitive experiments have been also carried out in the photodegradation solution, which indicated the photocatalyst has good recovered ability and stabilization.
Based on the analyzing of the degradation products including fragment ions and intermediate products with GC-MS, the possible degradation pathways of nitrobenzene were also suggested. The possible reaction routes could be divided into two pathways:One is hydroxyl radical attacked phenyl ring to form phenolic compounds, then the ring was opened, forming into various aliphatic compounds; Another is hydroxyl radical attacked directly the nitro-proup and phenol and its derivatives were generated while the nitro-proup was released by the radical addition-elimination. In the subsequent degradation processes, the two pathways have experimenced similar reaction being mineralized to inorganic compounds such as carbon dioxide and water. The probable photodegradation pathways were proposed and discussed as follows.
The possible formation mechanism of mesopore shell/core structured photocatalyst TiO2/SiO2/NiFe2O4 has also been discussued as follows.
引文
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