有序介观结构TiO_2及复合体的控制合成与性能研究
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摘要
属于纳米材料范畴的介孔材料由于其特殊的结构性质在催化、分离、离子交换等领域具有很多潜在的应用。但是，传统的介孔材料由于具有较小的介孔孔径(＜7nm)，从而制约了介孔材料在催化、大分子吸附、分离等领域的进一步应用。为拓展介孔材料的应用领域，合成具有大孔径(＞7nm)的介孔材料具有重要意义。
本文对有序介观结构TiO_2及复合体的控制合成与性能进行了研究，首次设计合成出大孔径的介孔TiO_2材料，研究发现通过改变合成参数可实现介孔TiO_2的孔径在一定范围内可调控。在制备孔径为14nm介孔TiO_2的基础上，加入锆源后，采用一步合成的方法设计合成了一系列介孔TiO_2-ZrO_2复合体材料。研究了介孔TiO_2和介孔TiO_2-ZrO_2复合体材料的光催化和亲水性能，并对其合成机理、光催化机理、亲水性机理作了深入探讨。
以Ti(OBu~n)_4水解原位释放的丁醇为助表面活性剂，以三嵌段聚合物P123为结构导向剂，在非水介质中采用溶剂蒸发诱导自组装的方法首次设计合成了大孔径的介孔TiO_2并对其进行了表征，结果表明所得材料具有大孔径(14nm)、窄孔径分布、二维六方结构，其晶型为锐钛矿相，BET比表面积为115m~2g~(-1)，孔容为0.219cm~3g~(-1)。这是迄今文献报道的孔径最大的介孔TiO_2材料。
在嵌段聚合物P123-Ti(OBu~n)_4-EtOH-HCl非水体系中，通过调控无机前驱体Ti(OBu~n)_4的量，即可改变原位生成Bu~nOH的量并实现材料孔径在一定范围内的可调控，本文设计合成了孔径可控(8.3-14nm)的一系列透明介孔TiO_2薄膜材料，其合成机理可归纳为以下几点：(ⅰ)原位生成的丁醇起到助表面活性剂的作用；(ⅱ)非水体系的合成条件提供了较大的表面活性剂有效堆积参数；(ⅲ)Ti(OBu~n)_4具有较长的线性和较大的立体构型；(ⅳ)大的水解速率／抑制速率(H／p)比。
Mesoporous materials which belong to the category of nanomaterials have opened some interesting applications in the field of catalysis, separation, ion-exchange, and others due to their unique structural character. However, the conventional mesoporous materials possess small mesopore diameter (<7 run), which limit their potential applications for catalysis, sorption and separation of large molecules. In order to extend the utility of mesoporous materials, it is essential to be able to synthesize large-pore (>7 ran) mesoporous materials.
The current dissertation concerns study on the controlled synthesis and properties of TiO_2 and its composite with ordered mesostructures. Large-pore meso-nc-TiO2 has been successfully designed and synthesized in our laboratory. Furthermore, the mesopore size can be easily controlled through adjusting the synthetic parameters. In this dissertation, on the basis of the synthetic strategy for the preparation of large-pore meso-nc-TiO_2 with 14 nm mesopore diameter, we also design and synthesize a series of mesoporous TiO_2-ZrO_2 composites using one-step synthesis strategy through introducing different amount of zirconia source. The photocatalytic activity and hydrophilicity of our obtained meso-nc-TiO_2 and mesoporous TiO_2-ZrO_2 composites were investigated in this thesis. The formation mechanism, photocatalysis mechanism and hydrophilicity mechanism of meso-nc-TiO_2 and mesoporous TiO_2-ZrO_2 composites were also presented in this dissertation.
A novel and facile synthesis strategy was demonstrated for the design and synthesis of large-pore meso-nc-TiO_2 thin films using butanol released in situ as the cosurfactant and triblock copolymer P123 as the template in the non-aqueous
本文对有序介观结构TiO_2及复合体的控制合成与性能进行了研究，首次设计合成出大孔径的介孔TiO_2材料，研究发现通过改变合成参数可实现介孔TiO_2的孔径在一定范围内可调控。在制备孔径为14nm介孔TiO_2的基础上，加入锆源后，采用一步合成的方法设计合成了一系列介孔TiO_2-ZrO_2复合体材料。研究了介孔TiO_2和介孔TiO_2-ZrO_2复合体材料的光催化和亲水性能，并对其合成机理、光催化机理、亲水性机理作了深入探讨。
以Ti(OBu~n)_4水解原位释放的丁醇为助表面活性剂，以三嵌段聚合物P123为结构导向剂，在非水介质中采用溶剂蒸发诱导自组装的方法首次设计合成了大孔径的介孔TiO_2并对其进行了表征，结果表明所得材料具有大孔径(14nm)、窄孔径分布、二维六方结构，其晶型为锐钛矿相，BET比表面积为115m~2g~(-1)，孔容为0.219cm~3g~(-1)。这是迄今文献报道的孔径最大的介孔TiO_2材料。
在嵌段聚合物P123-Ti(OBu~n)_4-EtOH-HCl非水体系中，通过调控无机前驱体Ti(OBu~n)_4的量，即可改变原位生成Bu~nOH的量并实现材料孔径在一定范围内的可调控，本文设计合成了孔径可控(8.3-14nm)的一系列透明介孔TiO_2薄膜材料，其合成机理可归纳为以下几点：(ⅰ)原位生成的丁醇起到助表面活性剂的作用；(ⅱ)非水体系的合成条件提供了较大的表面活性剂有效堆积参数；(ⅲ)Ti(OBu~n)_4具有较长的线性和较大的立体构型；(ⅳ)大的水解速率／抑制速率(H／p)比。
Mesoporous materials which belong to the category of nanomaterials have opened some interesting applications in the field of catalysis, separation, ion-exchange, and others due to their unique structural character. However, the conventional mesoporous materials possess small mesopore diameter (<7 run), which limit their potential applications for catalysis, sorption and separation of large molecules. In order to extend the utility of mesoporous materials, it is essential to be able to synthesize large-pore (>7 ran) mesoporous materials.
The current dissertation concerns study on the controlled synthesis and properties of TiO_2 and its composite with ordered mesostructures. Large-pore meso-nc-TiO2 has been successfully designed and synthesized in our laboratory. Furthermore, the mesopore size can be easily controlled through adjusting the synthetic parameters. In this dissertation, on the basis of the synthetic strategy for the preparation of large-pore meso-nc-TiO_2 with 14 nm mesopore diameter, we also design and synthesize a series of mesoporous TiO_2-ZrO_2 composites using one-step synthesis strategy through introducing different amount of zirconia source. The photocatalytic activity and hydrophilicity of our obtained meso-nc-TiO_2 and mesoporous TiO_2-ZrO_2 composites were investigated in this thesis. The formation mechanism, photocatalysis mechanism and hydrophilicity mechanism of meso-nc-TiO_2 and mesoporous TiO_2-ZrO_2 composites were also presented in this dissertation.
A novel and facile synthesis strategy was demonstrated for the design and synthesis of large-pore meso-nc-TiO_2 thin films using butanol released in situ as the cosurfactant and triblock copolymer P123 as the template in the non-aqueous
引文
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