炭质光催化复合材料制备及液相有机物去除性能的研究
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摘要
在环境保护领域中,采用半导体光催化材料降解溶液中有机物的反应探索已经进行了几十年。而单纯半导体金属氧化物由于其不易回收、稳定性低、可见光响应性弱、反应效率低等缺点,始终制约着该项技术向工业领域的推广。炭材料具有良好的稳定性与较强的吸附性能,同时作为催化剂载体有着广泛的应用,因此将新型炭材料与传统半导体金属氧化物进行结合,可以有效避免单纯半导体催化剂所产生的各种问题,从而为光催化材料在环境保护领域的发展提供了全新的途径,传统的以活性炭颗粒为代表的一系列炭材料为载体的复合光催化材料的产生已经证明了炭材料在此方向的优越性能。因此,本文旨在采用多种制备方法构建了一系列新型炭质光催化复合材料,并对其液相有机物去除性能进行探索。
1.以微孔型沥青基球状活性炭(PSAC)为载体,钛酸四正丁酯为钛源,采用溶胶-凝胶法和浸渍-烧结法分别制备了TiO2/PSAC复合材料。考察了两种方法制备的复合材料对于探针有机物的光催化降解性能以及循环反应性能。结果表明,两种方法制备所得样品均为微孔材料,且具备了光催化降解有机物的活性。其中,溶胶-凝胶法所制备的TiO2/PSAC复合光催化剂在高纯氮气环境下于450℃煅烧后,TiO2晶型为锐钛矿型,并以薄膜形式涂覆在PSAC表层,其在紫外光照射下反应420min对探针有机物的去除率可达96.7%,第三次循环反应结束后去除率仍能保持在84.0%,分别高于浸渍-烧结法制备样品的90.1%和69.1%,而纯PSAC吸附对于探针有机物的吸附去除率为55.0%。
2.以7nm的SiO2为模板剂,采用硬模板法制备的中孔炭(MC)为载体,通过溶胶-凝胶法制备了TiO2/MC复合光催化剂,并考察了其对有机物大分子液相光催化去除能力。复合材料TiO2含量及其晶型结构分别通过改变前驱体组成及煅烧温度进行调节。结果表明,由于中孔炭的纳米孔限域作用,锐钛矿型的TiO2以纳米颗粒形式均匀分散在炭的网络骨架界面上,从而形成了高度分散的TiO2/MC内米复合材料。另外,复合系统中中孔吸附作用的存在,与纳米TiO2的高效光催化产生协同作用,增强了复合材料在紫外光照射下对于水溶液中有机物的去除能力。在紫外光照射下反应75min时样品对探针有机物的去除率可达89%,而最终可达93%。此外,光降解反应遵循一级反应动力学,其最大反应速率常数为0.0147min-1。
3.分别以粒径为7nm与12nm的SiO2为模板剂,采用硬模板法制备孔结构不同的中孔炭MC-7以及MC-12,并通过水热法制备非金属氮元素掺杂二氧化钛中孔炭复合光催化剂。氮气吸附测试结果表明样品负载前后孔结构参数有较大程度变化,电镜结果表明氮元素掺杂并未改变样品晶体结构同时有效促进了颗粒尺寸的减小。氮元素的掺杂促使样品产生可见光区激发反应,而MC-7与MC-12相比更适合作为复合催化剂载体,其样品在吸附-光催化协同作用下75液相有机物除率可达68%。
4.采用三种结构不同的经过酸性氧化预处理的碳纳米纤维(CNFs)作为载体,以钛酸异丙酯为前驱体,通过水热法制备TiO2/CNFs复合催化剂,通过改变前驱体组成控制复合催化剂中TiO2含量。在材料复合过程中,纤维表面可以均匀负载锐钛矿型TiO2纳米颗粒,使样品在紫外光照条件下具有较好的液相有机物分子降解性能。CNFs促进了二氧化钛颗粒在其表面的分散,同时在复合材料系统中CNF所具有的吸附性能可与光催化降解作用形成协同效应。在不同CNF作为载体的复合材料中,TiO2/PCNF复合催化剂去除有机物性能高于其它。不同TiO2含量TiO2/PCNF复合催化剂中,TiO2含量80%时复合催化剂120min去除探针有机物效率最高,达到80.1%,不同煅烧温度复合催化剂中,煅烧温度500℃时复合催化剂120min内探针有机物去除效率最高,达到79.2%。在三次循环反应后,TiO2/PCNF复合催化剂对于液相有机物去除率仍能保持80%以上
5.以三嵌段共聚物F127作为模板剂,钛酸四正丁酯为钛源,使用溶剂蒸发诱导自组装法制备了非金属元素掺杂的中孔TiO2体系。研究了样品制备过程中热处理温度、前驱体配比、氧气后处理等条件对于样品去除水溶液有机物性能的影响。结果表明,样品液相吸附性能由其孔结构决定,光催化降解性能受到晶体结构、元素掺杂含量等因素影响,当样品前驱体配比为1/1,煅烧温度700℃时具有最强的紫外光激发催化活性；当前驱体配比为3/1与4/1且经过氧气后处理时,样品表现出可见光激发响应性,同时紫外光激发响应性也有大幅提高,其对于探针有机物总去除率可分别达89.6%和89.5%。样品具有较高的稳定性,其暗反应、紫外光激发与可见光激发反应对探针有机物去除率均能在多次循环反应后保持稳定。
In the environmental protection field, the reactions of photocatalytic materials degradation organic molecule in solutions have been researched for decades, but pure semiconductor metal oxide powders have some disadvantages such as hardly to be recovered, low stability, weak visible light responsiveness, low reaction efficiency and so on, which always restrict the promotion of this technology to civil industry. Carbon materials exhibt good stability, strong adsorption performance, and a wide range of applications as catalyst supports, thus combining the novel carbon materials and traditional semiconductor metal oxide, can avoid various problems of pure powder catalysts, and provide a new way for photocatalytic materials in the field of environmental protection. Therefore, this thesis was aimed to use a variety of preparation method to construct a series of new type of carbonaceous photocatalytic composite materials, and to investigate the removing performance for organics in liquid solution.
1. The TiO2/PSAC composites were prepared through sol-gel method and impregnation-calcination method, respectively, with tetrabuty tinanate as titanium source and pitch-based spherical activated carbon (PSAC) as support. The photocatalytic degradation activity and cyclic reaction of samples were studied using organic solution as a probe. The results indicated that the samples synthesized from the two methods exhibit microporous structure and show high photocatalytic activity. The composite prepared by sol-gel method sintered at450℃dunder N2atmosphere has an anatase crystal model coating on the surface of carrier, and its photocatalytic activities for probe organic can reach96.7%after the first cycle reaction, and84.0%after the third cycle, while the activities of composite sample prepared by impregnation-calcination method can just reach90.1%and69.1%, respectively, superior to pure PSAC just about55.0%.
2. Mesopous carbons (MC) from colloid silica templates were employed as supports to prepare TiO2/MC nanocomposites through a sol-gel process. TiO2content and crystalline structure of photocatalysts were turned by changing the precursor composition and calcination temperature, respectively. The experiment results showed that anatase TiO2nanoparticles could be highly dispersed on the surface of carbon framework, leading to the formation of high performance photocatalysts for degradation of probe organic under UV irradiation. The MC promoted the dispersion of TiO2in composite system and induced synergistic effects of adsorption and phtocatalytic degradation on the removal of probe organic. The organic removing rate could reach as high as89%in75min and93%at last under UV irradiation. The kinetics of organic degradation fitted well the first-order reaction kinetic and the largest rate constant was about0.015min-1.
3. Different pore structure mesoporous carbon were prepared with7nm and12nm SiO2particle as templates, then nitrogen element doped titanium dioxide mesoporous composites were prepared through hydrothermal process, results of nitrogen adsorption and electron microscope showed that pore structure parameters of MCs changed a lot after TiO2loading, and nitrogen doped did not change the crystal structure of TiO2loading on support, nitrogen doping prompted sample visible light excitation response and MC-7was more suitable than MC-12as a composite suppot, the removing rate of30%N-TiO2/MC-7for orgnic could reach68%in75min reaction.
4. Three kinds of carbon nanofibers (CNFs) pretreated by acidity oxidation treatment were employed as supports to prepare TiO2/CNFs nanocomposites by a hydrothermal process with titanium (IV) isopropoxide as the precursor, their photocatalysis activity and recycle property were investigated. The TiO2content of photocatalysts was turned by changing the precursor composition. Anatase TiO2nanoparticles could be highly dispersed on the surface of fibers, leading to the formation of high performance photocatalysts for degradation of probe organic under UV irradiation. The CNFs promoted the dispersion of TiO2in composite system and induced synergistic effects of adsorption and phtocatalytic degradation on the removal of organic. The TiO2/PCNF showed better performance than other composite, and the highest organic removing rate of TiO2/PCNF could reach as high as80.1%in120min for different TiO2content samples and79.2%for different temperature under UV irradiation. After three cycle reaction, the organic removing rate of TiO2/PCNF could still reach80%.
5. Block copolymers F127as template agent, titanium acid butyl acetate as titanium source, using solvent evaporation induced self-assembly process to prepare nonmetallic element doped mesopore TiO2system. The effect on removing properties for organic compound of sample preparation process conditions like heat treatment temperature, ratio of precursors, and oxygen post-treatment were investigated. The results showed that the liquid adsorption performance of samples was determined by its pore structure and the photocatalytic degradation performance was determined by the crystal structure, element doping content and so on. When precursor ratio1/1, calcining temperature700℃, the sample had strongest ultraviolet excitation catalytic activity, when the ratio of precursor were3/1,4/1and after oxygen post-processing, the samples showed visible light excitation response, at the same time ultraviolet excitation response also have greatly improved, and total removing rate for probe organic can reach up to89.6%and89.5%, respectively. The removing rate under dark reaction, ultraviolet and visible light excitation response to probe organic can remain stable for multiple cycle reaction that proved the high stability of the samples.
1.以微孔型沥青基球状活性炭(PSAC)为载体,钛酸四正丁酯为钛源,采用溶胶-凝胶法和浸渍-烧结法分别制备了TiO2/PSAC复合材料。考察了两种方法制备的复合材料对于探针有机物的光催化降解性能以及循环反应性能。结果表明,两种方法制备所得样品均为微孔材料,且具备了光催化降解有机物的活性。其中,溶胶-凝胶法所制备的TiO2/PSAC复合光催化剂在高纯氮气环境下于450℃煅烧后,TiO2晶型为锐钛矿型,并以薄膜形式涂覆在PSAC表层,其在紫外光照射下反应420min对探针有机物的去除率可达96.7%,第三次循环反应结束后去除率仍能保持在84.0%,分别高于浸渍-烧结法制备样品的90.1%和69.1%,而纯PSAC吸附对于探针有机物的吸附去除率为55.0%。
2.以7nm的SiO2为模板剂,采用硬模板法制备的中孔炭(MC)为载体,通过溶胶-凝胶法制备了TiO2/MC复合光催化剂,并考察了其对有机物大分子液相光催化去除能力。复合材料TiO2含量及其晶型结构分别通过改变前驱体组成及煅烧温度进行调节。结果表明,由于中孔炭的纳米孔限域作用,锐钛矿型的TiO2以纳米颗粒形式均匀分散在炭的网络骨架界面上,从而形成了高度分散的TiO2/MC内米复合材料。另外,复合系统中中孔吸附作用的存在,与纳米TiO2的高效光催化产生协同作用,增强了复合材料在紫外光照射下对于水溶液中有机物的去除能力。在紫外光照射下反应75min时样品对探针有机物的去除率可达89%,而最终可达93%。此外,光降解反应遵循一级反应动力学,其最大反应速率常数为0.0147min-1。
3.分别以粒径为7nm与12nm的SiO2为模板剂,采用硬模板法制备孔结构不同的中孔炭MC-7以及MC-12,并通过水热法制备非金属氮元素掺杂二氧化钛中孔炭复合光催化剂。氮气吸附测试结果表明样品负载前后孔结构参数有较大程度变化,电镜结果表明氮元素掺杂并未改变样品晶体结构同时有效促进了颗粒尺寸的减小。氮元素的掺杂促使样品产生可见光区激发反应,而MC-7与MC-12相比更适合作为复合催化剂载体,其样品在吸附-光催化协同作用下75液相有机物除率可达68%。
4.采用三种结构不同的经过酸性氧化预处理的碳纳米纤维(CNFs)作为载体,以钛酸异丙酯为前驱体,通过水热法制备TiO2/CNFs复合催化剂,通过改变前驱体组成控制复合催化剂中TiO2含量。在材料复合过程中,纤维表面可以均匀负载锐钛矿型TiO2纳米颗粒,使样品在紫外光照条件下具有较好的液相有机物分子降解性能。CNFs促进了二氧化钛颗粒在其表面的分散,同时在复合材料系统中CNF所具有的吸附性能可与光催化降解作用形成协同效应。在不同CNF作为载体的复合材料中,TiO2/PCNF复合催化剂去除有机物性能高于其它。不同TiO2含量TiO2/PCNF复合催化剂中,TiO2含量80%时复合催化剂120min去除探针有机物效率最高,达到80.1%,不同煅烧温度复合催化剂中,煅烧温度500℃时复合催化剂120min内探针有机物去除效率最高,达到79.2%。在三次循环反应后,TiO2/PCNF复合催化剂对于液相有机物去除率仍能保持80%以上
5.以三嵌段共聚物F127作为模板剂,钛酸四正丁酯为钛源,使用溶剂蒸发诱导自组装法制备了非金属元素掺杂的中孔TiO2体系。研究了样品制备过程中热处理温度、前驱体配比、氧气后处理等条件对于样品去除水溶液有机物性能的影响。结果表明,样品液相吸附性能由其孔结构决定,光催化降解性能受到晶体结构、元素掺杂含量等因素影响,当样品前驱体配比为1/1,煅烧温度700℃时具有最强的紫外光激发催化活性；当前驱体配比为3/1与4/1且经过氧气后处理时,样品表现出可见光激发响应性,同时紫外光激发响应性也有大幅提高,其对于探针有机物总去除率可分别达89.6%和89.5%。样品具有较高的稳定性,其暗反应、紫外光激发与可见光激发反应对探针有机物去除率均能在多次循环反应后保持稳定。
In the environmental protection field, the reactions of photocatalytic materials degradation organic molecule in solutions have been researched for decades, but pure semiconductor metal oxide powders have some disadvantages such as hardly to be recovered, low stability, weak visible light responsiveness, low reaction efficiency and so on, which always restrict the promotion of this technology to civil industry. Carbon materials exhibt good stability, strong adsorption performance, and a wide range of applications as catalyst supports, thus combining the novel carbon materials and traditional semiconductor metal oxide, can avoid various problems of pure powder catalysts, and provide a new way for photocatalytic materials in the field of environmental protection. Therefore, this thesis was aimed to use a variety of preparation method to construct a series of new type of carbonaceous photocatalytic composite materials, and to investigate the removing performance for organics in liquid solution.
1. The TiO2/PSAC composites were prepared through sol-gel method and impregnation-calcination method, respectively, with tetrabuty tinanate as titanium source and pitch-based spherical activated carbon (PSAC) as support. The photocatalytic degradation activity and cyclic reaction of samples were studied using organic solution as a probe. The results indicated that the samples synthesized from the two methods exhibit microporous structure and show high photocatalytic activity. The composite prepared by sol-gel method sintered at450℃dunder N2atmosphere has an anatase crystal model coating on the surface of carrier, and its photocatalytic activities for probe organic can reach96.7%after the first cycle reaction, and84.0%after the third cycle, while the activities of composite sample prepared by impregnation-calcination method can just reach90.1%and69.1%, respectively, superior to pure PSAC just about55.0%.
2. Mesopous carbons (MC) from colloid silica templates were employed as supports to prepare TiO2/MC nanocomposites through a sol-gel process. TiO2content and crystalline structure of photocatalysts were turned by changing the precursor composition and calcination temperature, respectively. The experiment results showed that anatase TiO2nanoparticles could be highly dispersed on the surface of carbon framework, leading to the formation of high performance photocatalysts for degradation of probe organic under UV irradiation. The MC promoted the dispersion of TiO2in composite system and induced synergistic effects of adsorption and phtocatalytic degradation on the removal of probe organic. The organic removing rate could reach as high as89%in75min and93%at last under UV irradiation. The kinetics of organic degradation fitted well the first-order reaction kinetic and the largest rate constant was about0.015min-1.
3. Different pore structure mesoporous carbon were prepared with7nm and12nm SiO2particle as templates, then nitrogen element doped titanium dioxide mesoporous composites were prepared through hydrothermal process, results of nitrogen adsorption and electron microscope showed that pore structure parameters of MCs changed a lot after TiO2loading, and nitrogen doped did not change the crystal structure of TiO2loading on support, nitrogen doping prompted sample visible light excitation response and MC-7was more suitable than MC-12as a composite suppot, the removing rate of30%N-TiO2/MC-7for orgnic could reach68%in75min reaction.
4. Three kinds of carbon nanofibers (CNFs) pretreated by acidity oxidation treatment were employed as supports to prepare TiO2/CNFs nanocomposites by a hydrothermal process with titanium (IV) isopropoxide as the precursor, their photocatalysis activity and recycle property were investigated. The TiO2content of photocatalysts was turned by changing the precursor composition. Anatase TiO2nanoparticles could be highly dispersed on the surface of fibers, leading to the formation of high performance photocatalysts for degradation of probe organic under UV irradiation. The CNFs promoted the dispersion of TiO2in composite system and induced synergistic effects of adsorption and phtocatalytic degradation on the removal of organic. The TiO2/PCNF showed better performance than other composite, and the highest organic removing rate of TiO2/PCNF could reach as high as80.1%in120min for different TiO2content samples and79.2%for different temperature under UV irradiation. After three cycle reaction, the organic removing rate of TiO2/PCNF could still reach80%.
5. Block copolymers F127as template agent, titanium acid butyl acetate as titanium source, using solvent evaporation induced self-assembly process to prepare nonmetallic element doped mesopore TiO2system. The effect on removing properties for organic compound of sample preparation process conditions like heat treatment temperature, ratio of precursors, and oxygen post-treatment were investigated. The results showed that the liquid adsorption performance of samples was determined by its pore structure and the photocatalytic degradation performance was determined by the crystal structure, element doping content and so on. When precursor ratio1/1, calcining temperature700℃, the sample had strongest ultraviolet excitation catalytic activity, when the ratio of precursor were3/1,4/1and after oxygen post-processing, the samples showed visible light excitation response, at the same time ultraviolet excitation response also have greatly improved, and total removing rate for probe organic can reach up to89.6%and89.5%, respectively. The removing rate under dark reaction, ultraviolet and visible light excitation response to probe organic can remain stable for multiple cycle reaction that proved the high stability of the samples.
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