介孔烷基有机钛杂化材料的制备及光催化性能研究

发布时间：2018-02-01 19:21

本文关键词： 介孔材料烷基功能化二氧化钛 CH_3-TiO_2 C_6H_5CH_2-TiO_2　出处：《长春工业大学》2017年硕士论文　论文类型：学位论文

【摘要】：近几年来大规模的雾霾空气等环境污染不时爆发,保护环境也越加紧迫、治理环境污染刻不容缓。印染工业生产过程造成的染料污染,是水体污染的重要原因之一。水中的污染物能够吸收光线,降低水的可见度,并且消耗水中的氧气,造成水中缺少氧气。本文选取染料罗丹明B(RhB)作为代表性的染料目标化合物,以进行光催化降解测试。(1)以乙醚(Et_2O)为溶剂,以卤代烃CH_3I与镁屑(Mg)反应,制备格式试剂CH3MgI。在低温条件下,控制格氏试剂CH3MgI与无机钛试剂(TiCl4)反应,得到有机钛前驱体(CH3TiCl3)溶液;利用水解共缩合技术,得到基于甲基基团的介孔有机钛CH3-TiO2杂化材料。通过傅里叶红外FT-IR表征介孔有机钛CH3-TiO2杂化材料中甲基官能团的存在;利用氮气吸附-脱附技术、X射线粉末衍射(XRD)、透射电镜(TEM)、扫描电镜(SEM)、紫外可见漫反射光谱(UV/Vis-NIR)等技术,表征介孔甲基有机钛CH3-TiO2杂化材料的表面物理化学性质、形貌、光吸收性能等。结果表明:所制备的CH3-TiO2是一种介孔材料。以染料罗丹明B(RhB)为目标降解底物,介孔甲基有机钛CH3-TiO2杂化材料为降解催化剂,在模拟太阳光的条件下来探究介孔甲基有机钛CH3-TiO2杂化材料的光催化活性。与无机TiO2材料相比,介孔有机钛CH3-TiO2杂化材料的光催化活性更好。(2)以四氢呋喃(THF)为溶剂,以卤代烃C_6H_5CH_2Cl与镁屑(Mg)反应,制备格式试剂C6H5CH2MgCl。在低温条件下,按照格氏试剂C6H5CH2MgCl与无机钛试剂TiCl4与Ti(iO-Pr)4的摩尔比为4:1:3来控制反应,得到有机钛前驱体(C6H5CH2Ti(iO-Pr)3);利用水解共缩合结合溶剂挥发诱导自组装技术(EISA),制备基于苄基基团的介孔有机钛BnTiO杂化材料。通过各种表征手段,如核磁共振技术确定苄基有机钛前驱体(C6H5CH2Ti(iO-Pr)3),傅里叶红外FT-IR表征介孔有机钛BnTiO杂化材料中有机基团苄基的引入。利用氮气吸附-脱附技术、X射线粉末衍射(XRD)、透射电镜(TEM)、扫描电镜(SEM)、紫外可见漫反射光谱(UV/Vis-NIR)等技术,表征介孔材料有机钛BnTiO杂化材料的外貌物理化学性质、形貌、光吸收性能等。结果表明:经过水解缩合得到的BnTiO(C6H5CH2-TiO2)是一种介孔材料。并且引入苄基后紫外可见漫反射光谱吸收范围拓展到可见光区。以染料罗丹明B(RhB)为目标降解底物,介孔苄基有机钛BnTiO杂化材料为降解催化剂,在模拟太阳光的条件下来探究介孔苄基有机钛BnTiO杂化材料的光催化活性。与无机TiO2材料相比,介孔苄基有机钛BnTiO杂化材料的光催化活性更好。
[Abstract]:In recent years large-scale environmental pollution such as haze air and other environmental pollution erupts from time to time and the protection of the environment is more and more urgent so it is urgent to control the environmental pollution. The dye pollution caused by printing and dyeing industry production process is urgent. Pollutants in water can absorb light, reduce the visibility of water, and consume oxygen in water. In this paper, the dye Rhodamine Bhh Rh B) was selected as the representative dye target compound for photocatalytic degradation test. The standard reagent Ch _ 3MgI was prepared by the reaction of halogenated hydrocarbon CH_3I with magnesium chip Mg.The reaction of Grignard reagent CH3MgI with inorganic titanium reagent (TiCl _ 4) was controlled at low temperature. The organic titanium precursor (Ch _ 3TiCl _ 3) solution was obtained. The hydrolysis co-condensation technique was used. The mesoporous organic titanium CH3-TiO2 hybrid material based on methyl group was obtained. The existence of methyl functional group in mesoporous organic titanium CH3-TiO2 hybrid material was characterized by Fourier transform infrared FT-IR. Nitrogen adsorption-desorption techniques such as X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and UV-Vis diffuse reflectance spectroscopy (UV / Vis-NIRs) were used. The surface physicochemical properties and morphology of mesoporous organic titanium (CH3-TiO2) hybrid materials were characterized. The results showed that the prepared CH3-TiO2 was a mesoporous material and the dye Rhodamine was used as the target substrate for degradation. Mesoporous organotitanium CH3-TiO2 hybrid material was used as the degradation catalyst. The photocatalytic activity of mesoporous organotitanium (CH3-TiO2) hybrid materials was investigated under simulated solar light. Compared with inorganic TiO2 materials. The mesoporous organic titanium (CH3-TiO2) hybrid material has better photocatalytic activity. The tetrahydrofuran (THF) is used as the solvent, and the halide C _ 6H _ 5CH2Cl is used to react with mg / mg. The standard reagent C6H5CH2MgCl. was prepared at low temperature. The reaction was controlled by the molar ratio of Grignard reagent C6H5CH2MgCl and inorganic titanium reagent TiCl4 to Ti(iO-Pr)4 of 4: 1: 3. The organic titanium precursor, C6H5CH2TiTiOPRO3, was obtained. The mesoporous organic titanium (BnTiO) hybrid materials based on benzyl group were prepared by hydrolysis co-condensation and solvent volatilization induced self-assembly technique. For example, the benzyl organic titanium precursor, C6H5CH2TiTiO-Pr3, was determined by NMR. Fourier transform infrared (FTIR) FT-IR was used to characterize the introduction of organic benzyl groups in mesoporous BnTiO hybrid materials. X-ray powder diffraction (XRD) was performed by nitrogen adsorption-desorption technique. Transmission electron microscopy (TEM), scanning electron microscopy (SEM) and diffuse reflectance spectroscopy (UV / Vis-NIR). The physical and chemical properties and morphology of mesoporous organic titanium BnTiO hybrid materials were characterized. The results show that the BnTiON C6H5CH2-TiO2 was obtained by hydrolysis and condensation. It is a kind of mesoporous material, and the absorption range of UV-Vis diffuse reflectance spectrum is extended to the visible region after the introduction of benzyl. Mesoporous benzyl organic titanium (BnTiO) hybrid material was used as the degradation catalyst. The photocatalytic activity of mesoporous benzyl organic titanium (BnTiO) hybrid materials was investigated under simulated solar light. Compared with inorganic TiO2 materials. Mesoporous benzyl organic titanium (BnTiO) hybrid materials have better photocatalytic activity.
【学位授予单位】：长春工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O643.36

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