氧化铁改性及氧化钛固有光催化活性研究
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摘要
作为高级氧化技术的一员,半导体光催化技术成为当今环境与能源领域的研究热点。通过利用清洁、可再生的太阳能,光催化技术可在较为温和的反应条件下,将有机物彻底矿化分解,不会造成二次污染,且常见的光催化剂通常无毒,价格低廉,在环境领域中有巨大的应用前景。自20世纪80年代以来,光催化在污染物的处理方面(水相和气相)取得了十足的发展,逐渐成为研究的热点与重点。以Ti02和Fe203等为代表的半导体光催化剂具有高活性、低成本,环境友好及稳定性好的优势,其原理及应用的相关研究日益受到广泛的重视。
围绕这个主题,我们从光催化的基本原理入手,将Fe203分散于氧化铝载体上,制备了活性及稳定性较高的光催化剂。而通过对Ti02固有光催化活性的研究,首次发现高温处理得到的Ti02具有更强的光吸收,更多的表面缺陷,更高的空穴-电子分离效率,进而导致更高的“固有”光催化活性,强调了高温煅烧对于提高TiO2光催化活性的重要性。进一步,通过研究板钛矿TiO2的光催化活性,证实TiO2的固有光催化活性仅与煅烧温度有关,而与其晶型无直接联系。还通过使用氧化铈修饰金红石TiO2提高了其光催化活性。本论文分为七章,主要研究内容与成果如下：
(1)通过溶胶-凝胶法将Fe203分散于氧化铝载体上,有效地减小氧化铁的粒子大小,增加了有机物的吸附量,进而有效提高了氧化铁的光催化活性。氧化铁的含量为25wt%,且煅烧温度为400℃的负载样品具有最高的反应活性。此种活性不仅明显高于氧化铁本身,也高于氧化硅负载的氧化铁样品。通过循环试验,发现氧化铁/氧化铝负载催化剂的光稳定性明显强于氧化铁/氧化硅负载催化剂。
(2)通过水热法合成了三组具有不同粒径大小的锐钛矿Ti02：不同水热时间、不同煅烧温度及不同煅烧时间的TiO2。通过使用O2和Ag+作为电子捕获剂,考察了TiO2的煅烧温度和粒径对其降解苯酚速率的影响。研究结果清晰地表明：随着Ti02颗粒的增大,其“固有”光催化活性逐渐增大。然而,粒子大小并不是高温煅烧提高光催化活性的主要原因。在相同的粒子大小条件下,与低温水热合成的样品相比,高温处理得到的Ti02具有更强的光吸收,更多的表面缺陷,更高的空穴-电子分离效率,进而导致更高的“固有”光催化活性。此工作强调了高温煅烧对于提高TiO2光催化活性的重要性。
(3)考察了板钛矿Ti02的固有光催化活性。以二(2-羟基丙酸)二氢氧化二铵合钛为钛源,通过水热法合成了纯相板钛矿Ti02。采用02或Ag+作为电子捕获剂,通过比较不同Ti02光催化降解苯酚与光催化还原Cr6+,发现：当Ti02表面的电子捕获剂浓度相同时,无论是光催化降解有机物,还是光还原过程,板钛矿Ti02的“固有”光催化活性与锐钛矿和金红石相同,仅由煅烧温度决定。此外,板钛矿与金红石之间存在混晶效应,可能的原因是由于02从板钛矿表面扩散至金红石表面,进而释放出高结晶金红石的高固有活性。
(4)通过使用氧化铈修饰金红石Ti02提高了其光催化活性。采用O2或Ag+作为电子捕获剂,在紫外光照下考察了此种催化剂的光催化活性。结果表明,当使用02作为电子捕获剂时,Ce02的修饰可以显著提高金红石的光催化活性,且金红石的Ts越高,此种提高的效果越明显。而当使用Ag+作为电子捕获剂时,上述结果没有出现。另外,高温处理后的Ce02也不能改善金红石的光催化活性。通过综合考虑多种因素,我们认为低温处理的Ce02具有很强的储氧能力,当其与金红石接触后,Ce02贮存的O2会扩散至金红石的粒子表面,提高了光生载流子的分离效率,进而释放出高结晶金红石的高固有活性。
As a member of advanced oxidation technology, semiconductor photocatalytic technology becomes hot topic in today's environment and energy fields. By using the clean and renewable solar energy, photocatalytic technology can occur under milder reaction conditions, and completely mineralize the organic pollutants, without causing secondary pollution. The common photocatalysts are generally non-toxic, low prices, which have great application prospects in environmental field. Since1980's, photocatalysis in dealing with contaminants (water phase and gas phase) achieved full development, has become the hotspot in research. Semiconductor photocatalysts, such as TiO2and Fe2O3, have the advantages of high activity, low cost, environmentally friendly, and good stability, and the research in application and principles cause widespread attention.
Around this theme, from the basic principles of photocatalysis, we prepared the the photocatalyst of high activity and stability by Fe2O3dispersed on the alumina support. And by studying the intrinsic photocatalytic activity of anatase TiO2, we found that the thermally treated TiO2has more surface defects than the hydrothermally treated one, which would facilitate charge separation, and consequently accelerate phenol degradation at the solid-liquid interface. Furthermore, by studying the brookite TiO2, we confirm that TiO2has the same "intrinsic" photocatalytic activity, regardless of the solid structures in the form of anatase, rutile and brookite. By modifying rutile TiO2with CeO2, we found that the positive effect of CeO2was observed with rutile TiO2, but not with anatase or P25TiO2. This thesis is mainly divided into seven chapters, the main research contents and results are as follows:
(1) Silica supported hematite (Fe2O3/silica) that is more active but less stable than the supported hematite for organic photodegradation in aqueous solution has been reported. In this work, we report on alumina supported hematite (Fe2O3/alumina) with significantly improved activity and stability. The catalysts were prepared by mixing alumina with a pre-made colloidal iron oxide at various loading (0-100wt%), followed by sintering at different temperatures (200-900℃). Solid characterization with X-ray diffraction and N2adsorption showed that hematite particles were small in size, and large in surface area, as compared with the unsupported hematite prepared in parallel. The catalyst activity was evaluated with anionic Orange Ⅱ as a model substrate, and the reaction was carried out in aerated aqueous suspension under light irradiation at wavelengths longer than320nm. As the Fe2O3loading on alumina or the catalyst sintering temperature increased, the apparent rate constant of dye degradation increased, and then decreased. The maximum rate of dye degradation was obtained with25wt%Fe2O3/alumina, sintered at400℃. Moreover, five consecutive experiments for dye photodegradation showed that Fe2O3/alumina was much more stable than Fe2O3/silica, due to alumina that has a positively charged surface and thus facilitates the dissolved iron species back onto iron oxide. The higher activity of Fe2O3/alumina than Fe2O3/silica and bare hematite is ascribed to the combined effect between the reduced particle size of hematite and the enhanced surface adsorption of dye on the catalyst.
(2) Photocatalytic activity of anatase TiO2that increases with the increase of its synthesis temperature has been widely reported, but the reason for that remains incompletely understood. In this work, the positive effect of synthesis temperature, presumably due to the growth of particle size, has been examined. Three series of anatase samples with various particle sizes were prepared from the hydrolysis of TiOSO4in water at150℃, followed by calcination in air. The particle size of TiO2, estimated by X-ray diffraction, and/or by N2adsorption, increased with the increases of the hydrothermal time, calcination time, and calcination temperature, respectively. For phenol photodegradation in aerated aqueous suspension, three series of the samples showed different correlation between the activity and particle size of TiO2. However, for phenol photodegradation in a N2-purged aqueous suspension, these catalysts with the same amount of Ag+adsorbed on the oxide surface showed activities all in proportion to the particle size of TiO2, whereas at given particle size, the thermally treated TiO2was much more active than the hydrothermally treated one. The observed effect of particle size is discussed in terms of the solid crystallinity, surface area, exposed facets, surface hydroxyl groups and light absorption, but they only correlate with the trend in the number of surface defects, as revealed by photoluminescence spectroscopy. Moreover, at given particle size, the thermally treated TiO2has more surface defects than the hydrothermally treated one, which would facilitate charge separation, and consequently accelerate phenol degradation at the solid-liquid interface.
(3) It has been reported that with the same amount of electron scavenger on the catalyst surfaces, anatase and rutile actually have a similar "intrinsic" photocatalytic activity at a given sintering temperature (Ts), for organic degradation or water oxidation. But for brookite TiO2, its "intrinsic" photocatalytic has not been studied. In this work, the brookite was synthesized by using a hydrothermal method. The characterizations reveal that the brookite is in pure phase. In the aerated aqueous suspension of TiO2, the initial rate of phenol photodegradation, per surface area of the catalyst, brookite shows higher photocatalytic activity than anatase. By using Ag+as the electron scavenger, we found that at the same amount of electron acceptor adsorbed on the catalyst surfaces, anatase, brookite and rutile actually have a similar photocatalytic activity at a given Ts, for organic oxidation. And for Cr(VI) photoreduction process, the similar result is found. Moreover, there is a synergistic effect between brookite and rutile particles for organic degradation in aerated aqueous suspension, and the higher activity is caused by the process of O2on brookite diffusing onto the rutile sites nearby.
(4) Modification of anatase TiO2with CeO2resulting into enhancement in the photocatalytic activity for organic degradation has been widely reported, but the role of CeO2remains unclear. In this work, the biphase oxide has been prepared by mixing individual oxides together, without changes in the physical properties of TiO2itself. For phenol degradation in aqueous suspension under UV light, the positive effect of CeO2was observed with rutile TiO2, but not with anatase or P25TiO2. As the synthesis temperatures of rutile and CeO2increased, the activity enhancement of the mixed oxide increased and decreased, respectively. However, with the same amount of Ag+adsorbed on each catalyst for phenol degradation under N2, the CeO2-mixed TiO2was always less photoactive than parent TiO2(anatase, rutile and P25). Several factors were considered, including the photogeneration of H2O2, and the conduction band edge potentials measured with the oxides. It is proposed that nonstoichiometric CeO2produced at low temperature has ability to store and release oxygen to TiO2nearby, consequently exploring the masked photocatalytic activity of rutile for phenol degradation in aqueous suspension.
围绕这个主题,我们从光催化的基本原理入手,将Fe203分散于氧化铝载体上,制备了活性及稳定性较高的光催化剂。而通过对Ti02固有光催化活性的研究,首次发现高温处理得到的Ti02具有更强的光吸收,更多的表面缺陷,更高的空穴-电子分离效率,进而导致更高的“固有”光催化活性,强调了高温煅烧对于提高TiO2光催化活性的重要性。进一步,通过研究板钛矿TiO2的光催化活性,证实TiO2的固有光催化活性仅与煅烧温度有关,而与其晶型无直接联系。还通过使用氧化铈修饰金红石TiO2提高了其光催化活性。本论文分为七章,主要研究内容与成果如下：
(1)通过溶胶-凝胶法将Fe203分散于氧化铝载体上,有效地减小氧化铁的粒子大小,增加了有机物的吸附量,进而有效提高了氧化铁的光催化活性。氧化铁的含量为25wt%,且煅烧温度为400℃的负载样品具有最高的反应活性。此种活性不仅明显高于氧化铁本身,也高于氧化硅负载的氧化铁样品。通过循环试验,发现氧化铁/氧化铝负载催化剂的光稳定性明显强于氧化铁/氧化硅负载催化剂。
(2)通过水热法合成了三组具有不同粒径大小的锐钛矿Ti02：不同水热时间、不同煅烧温度及不同煅烧时间的TiO2。通过使用O2和Ag+作为电子捕获剂,考察了TiO2的煅烧温度和粒径对其降解苯酚速率的影响。研究结果清晰地表明：随着Ti02颗粒的增大,其“固有”光催化活性逐渐增大。然而,粒子大小并不是高温煅烧提高光催化活性的主要原因。在相同的粒子大小条件下,与低温水热合成的样品相比,高温处理得到的Ti02具有更强的光吸收,更多的表面缺陷,更高的空穴-电子分离效率,进而导致更高的“固有”光催化活性。此工作强调了高温煅烧对于提高TiO2光催化活性的重要性。
(3)考察了板钛矿Ti02的固有光催化活性。以二(2-羟基丙酸)二氢氧化二铵合钛为钛源,通过水热法合成了纯相板钛矿Ti02。采用02或Ag+作为电子捕获剂,通过比较不同Ti02光催化降解苯酚与光催化还原Cr6+,发现：当Ti02表面的电子捕获剂浓度相同时,无论是光催化降解有机物,还是光还原过程,板钛矿Ti02的“固有”光催化活性与锐钛矿和金红石相同,仅由煅烧温度决定。此外,板钛矿与金红石之间存在混晶效应,可能的原因是由于02从板钛矿表面扩散至金红石表面,进而释放出高结晶金红石的高固有活性。
(4)通过使用氧化铈修饰金红石Ti02提高了其光催化活性。采用O2或Ag+作为电子捕获剂,在紫外光照下考察了此种催化剂的光催化活性。结果表明,当使用02作为电子捕获剂时,Ce02的修饰可以显著提高金红石的光催化活性,且金红石的Ts越高,此种提高的效果越明显。而当使用Ag+作为电子捕获剂时,上述结果没有出现。另外,高温处理后的Ce02也不能改善金红石的光催化活性。通过综合考虑多种因素,我们认为低温处理的Ce02具有很强的储氧能力,当其与金红石接触后,Ce02贮存的O2会扩散至金红石的粒子表面,提高了光生载流子的分离效率,进而释放出高结晶金红石的高固有活性。
As a member of advanced oxidation technology, semiconductor photocatalytic technology becomes hot topic in today's environment and energy fields. By using the clean and renewable solar energy, photocatalytic technology can occur under milder reaction conditions, and completely mineralize the organic pollutants, without causing secondary pollution. The common photocatalysts are generally non-toxic, low prices, which have great application prospects in environmental field. Since1980's, photocatalysis in dealing with contaminants (water phase and gas phase) achieved full development, has become the hotspot in research. Semiconductor photocatalysts, such as TiO2and Fe2O3, have the advantages of high activity, low cost, environmentally friendly, and good stability, and the research in application and principles cause widespread attention.
Around this theme, from the basic principles of photocatalysis, we prepared the the photocatalyst of high activity and stability by Fe2O3dispersed on the alumina support. And by studying the intrinsic photocatalytic activity of anatase TiO2, we found that the thermally treated TiO2has more surface defects than the hydrothermally treated one, which would facilitate charge separation, and consequently accelerate phenol degradation at the solid-liquid interface. Furthermore, by studying the brookite TiO2, we confirm that TiO2has the same "intrinsic" photocatalytic activity, regardless of the solid structures in the form of anatase, rutile and brookite. By modifying rutile TiO2with CeO2, we found that the positive effect of CeO2was observed with rutile TiO2, but not with anatase or P25TiO2. This thesis is mainly divided into seven chapters, the main research contents and results are as follows:
(1) Silica supported hematite (Fe2O3/silica) that is more active but less stable than the supported hematite for organic photodegradation in aqueous solution has been reported. In this work, we report on alumina supported hematite (Fe2O3/alumina) with significantly improved activity and stability. The catalysts were prepared by mixing alumina with a pre-made colloidal iron oxide at various loading (0-100wt%), followed by sintering at different temperatures (200-900℃). Solid characterization with X-ray diffraction and N2adsorption showed that hematite particles were small in size, and large in surface area, as compared with the unsupported hematite prepared in parallel. The catalyst activity was evaluated with anionic Orange Ⅱ as a model substrate, and the reaction was carried out in aerated aqueous suspension under light irradiation at wavelengths longer than320nm. As the Fe2O3loading on alumina or the catalyst sintering temperature increased, the apparent rate constant of dye degradation increased, and then decreased. The maximum rate of dye degradation was obtained with25wt%Fe2O3/alumina, sintered at400℃. Moreover, five consecutive experiments for dye photodegradation showed that Fe2O3/alumina was much more stable than Fe2O3/silica, due to alumina that has a positively charged surface and thus facilitates the dissolved iron species back onto iron oxide. The higher activity of Fe2O3/alumina than Fe2O3/silica and bare hematite is ascribed to the combined effect between the reduced particle size of hematite and the enhanced surface adsorption of dye on the catalyst.
(2) Photocatalytic activity of anatase TiO2that increases with the increase of its synthesis temperature has been widely reported, but the reason for that remains incompletely understood. In this work, the positive effect of synthesis temperature, presumably due to the growth of particle size, has been examined. Three series of anatase samples with various particle sizes were prepared from the hydrolysis of TiOSO4in water at150℃, followed by calcination in air. The particle size of TiO2, estimated by X-ray diffraction, and/or by N2adsorption, increased with the increases of the hydrothermal time, calcination time, and calcination temperature, respectively. For phenol photodegradation in aerated aqueous suspension, three series of the samples showed different correlation between the activity and particle size of TiO2. However, for phenol photodegradation in a N2-purged aqueous suspension, these catalysts with the same amount of Ag+adsorbed on the oxide surface showed activities all in proportion to the particle size of TiO2, whereas at given particle size, the thermally treated TiO2was much more active than the hydrothermally treated one. The observed effect of particle size is discussed in terms of the solid crystallinity, surface area, exposed facets, surface hydroxyl groups and light absorption, but they only correlate with the trend in the number of surface defects, as revealed by photoluminescence spectroscopy. Moreover, at given particle size, the thermally treated TiO2has more surface defects than the hydrothermally treated one, which would facilitate charge separation, and consequently accelerate phenol degradation at the solid-liquid interface.
(3) It has been reported that with the same amount of electron scavenger on the catalyst surfaces, anatase and rutile actually have a similar "intrinsic" photocatalytic activity at a given sintering temperature (Ts), for organic degradation or water oxidation. But for brookite TiO2, its "intrinsic" photocatalytic has not been studied. In this work, the brookite was synthesized by using a hydrothermal method. The characterizations reveal that the brookite is in pure phase. In the aerated aqueous suspension of TiO2, the initial rate of phenol photodegradation, per surface area of the catalyst, brookite shows higher photocatalytic activity than anatase. By using Ag+as the electron scavenger, we found that at the same amount of electron acceptor adsorbed on the catalyst surfaces, anatase, brookite and rutile actually have a similar photocatalytic activity at a given Ts, for organic oxidation. And for Cr(VI) photoreduction process, the similar result is found. Moreover, there is a synergistic effect between brookite and rutile particles for organic degradation in aerated aqueous suspension, and the higher activity is caused by the process of O2on brookite diffusing onto the rutile sites nearby.
(4) Modification of anatase TiO2with CeO2resulting into enhancement in the photocatalytic activity for organic degradation has been widely reported, but the role of CeO2remains unclear. In this work, the biphase oxide has been prepared by mixing individual oxides together, without changes in the physical properties of TiO2itself. For phenol degradation in aqueous suspension under UV light, the positive effect of CeO2was observed with rutile TiO2, but not with anatase or P25TiO2. As the synthesis temperatures of rutile and CeO2increased, the activity enhancement of the mixed oxide increased and decreased, respectively. However, with the same amount of Ag+adsorbed on each catalyst for phenol degradation under N2, the CeO2-mixed TiO2was always less photoactive than parent TiO2(anatase, rutile and P25). Several factors were considered, including the photogeneration of H2O2, and the conduction band edge potentials measured with the oxides. It is proposed that nonstoichiometric CeO2produced at low temperature has ability to store and release oxygen to TiO2nearby, consequently exploring the masked photocatalytic activity of rutile for phenol degradation in aqueous suspension.
引文
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