钛硅复合氧化物的制备及在微污染水处理中的应用研究
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摘要
有机微污染物口益严重的水源水已经给饮用水处理带来了严峻的挑战。微污染原水经过常规净水工艺处理后无法保证供水水质的安全性,需要在先前工艺的基础上增加深度处理工艺。近年来,TiO2因能使有机物彻底矿化,具有良好的杀菌和抑制病毒活性的作用等在环境治理和能源开发方面得到了普遍的关注。然而,因TiO2在光照时产生的e--h+对容易复合,而且禁带宽度较大不能充分利用太阳光,使其实际应用受到了很大限制。因此,对TiO2进行改性以提高光催化活性成为研究的热点。
本文采用两步溶胶凝胶法制备了SiO2/TiO2,通过对水中微污染有机物的降解选择出高活性的SiO2/TiO2光催化剂,并进一步对其进行修饰改性以获得更加高效的光催化剂。采用XRD、TG-DTA、FT-IR、UV-vis、XPS及TEM等测试手段对催化剂的结构进行了表征,并对其作用机理进行了深入的研究。在本实验中主要研究的内容如下：
(1)以正硅酸乙酯和钛酸四丁酯为硅源和钛源,无水乙醇为溶剂,乙酰丙酮为抑制剂,盐酸为催化剂(正硅酸乙酯水解时)制备了SiO2/TiO2。以水中微污染腐殖酸(HA)的降解效果确定了SiO2/TiO2的最佳制备条件,并对其进行了表征。结果表明,在相同焙烧温度下,硅的引入可抑制TiO2晶相的转变及催化剂晶粒的增大。当硅掺杂浓度为10%时SiO2/TiO2的最佳焙烧温度为800℃。
(2)硅掺杂浓度的大小决定着SiO2/TiO2焙烧温度的高低。水用量对催化剂的光催化活性影响较大。在此基础上于600℃下制备了硅掺杂浓度为5%的SiO2/TiO2,将其运用于水中微量甲基橙的降解中。经刻蚀前后的XPS表征分析可知,Si原子在热处理过程中向粉体颗粒的表面扩散,导致TiO2外表面出现Ti4+而在近表面产生Ti3+及氧空位。Ti3+和氧空位缺陷的联合作用、Ti4+与Ti3+的共同存在能有效分离电荷是导致SiO2/TiO2活性较高的关键原因。
(3)采用热沉积法制备了负载型TS2,550薄膜,研究了其对水中微污染HA的降解及E.coli的灭活效果。结果表明,该薄膜在光催化过程中对HA的降解速率要快于对E.coli的灭活速率。其机理为：薄膜在紫外线照射下产生了氧化还原能力较高的e-和h+。而e-和h+分别与溶解于水中的氧气和水反应生成了许多活性物种如·O2-和·OH等,这些活性物种使水中的HA氧化成无毒的物质,如CO2和H2O,并能破坏E.coli细胞致其死亡
(4)采用两步溶胶凝胶法制备了Gd3+掺杂SiO2/TiO2光催化材料,以水中微污染HA (pH=6.5)的降解及矿化研究了其光催化活性。结果表明,Gd-SiO2/TiO2光催化剂在150 min内可使水中HA彻底降解,并能使HA的矿化率达97%,比同等条件下TiO2的矿化率增加了38%,比SiO2/TiO2的矿化率增加了30%。可能的原因为：1)Gd3+的掺杂可有效抑制TiO2从锐钛矿相向金红石相的转变和晶粒的增长。同等条件下,Gd-SiO2/TiO2、SiO2/TiO2及TiO2的平均晶粒分别为25.5nm、35.2nm和37.8nm；2)Gd3+的掺杂不仅使催化剂在波长200-800nm内对光的吸收强度增强,而且使催化剂的吸收带边发生蓝移,即带隙能宽化。同等条件下,TiO2、SiO2/TiO2及Gd-SiO2/TiO2的禁带宽度分别为2.57eV、2.62eV和2.69eV；3)Gd3+的掺杂使Gd-SiO2/TiO2催化剂的表面缺陷Ti3+和晶格氧的数量增多。这些都将有利于提高催化剂的光催化活性。
(5)制备了Fe掺杂SiO2/TiO2可见光响应型光催化材料,选择微污染HA为降解目标物考察了催化剂的光催化活性。表征分析结果表明：Fe离子掺杂不仅使催化剂的吸收带边产生红移,而且增加了催化剂对可见光的吸收强度。另外,在催化剂表面出现了有利于e--h+对分离的Fe3+/Fe2+氧化还原电对。因此,Fe-SiO2/TiO2的可见光活性明显高于SiO2/TiO2和TiO2。
The increasing of organic micro-pollutants in source water has brought serious challenges for drinking water treatment. Micro-polluted raw water treated by regular water purification process can't guarantee the security of water quality. Therefore it needs to add depth process on the basis of the previous technology. In recent years, TiO2 has been attended in environmental treatment and energy exploitation due to thoroughly mineralization of organic matter, good bactericidal effect and inhibition of viral activity. However, the practical application of TiO2 has been very limited because the e--h+ pairs produced by TiO2 in the illumination are easy to recombine and TiO2 doesn't fully utilize solar energy with a larger band gap. There fore, modifications of TiO2 become a research focus to improve its photocatalytic activity.
In this paper, the SiO2/TiO2 composites were prepared by two-step sol-gel method. The degradation of micro-organic pollutant in water used to choose higher photocatalytic activity of SiO2/TiO2. And further to modify SiO2/TiO2 to obtain more efficient photocatalysts. The structures of the catalysts were characterized using XRD, TG-DTA, FT-IR, UV-vis, XPS and TEM methods.As well as, their mechanisms were studied in detail. In this experiment, the main contents of study were as follows:
(1) SiO2/TiO2 composites were prepared with tetraethoxysilane and tetrabutyl titanate as silicon source and titanium source respectively, anhydrous ethanol as solvent, acetyl acetone as inhibitor and hydrochloric acid as catalyst for hydrolysis of TEOS. The optimum preparation conditions of the SiO2/TiO2 were determined by photocatalytic degradation effects of micro-polluted humic acid in water and the characterizations of SiO2/TiO2 were analyzed. Results showed that the introduction of silicon inhibited phase transformation and particle size increase of TiO2 under the same calcining temperature. The best calcining temperature was 800℃when silicon doping concentration was 10% for SiO2/TiO2.
(2) The calcining temperature of SiO2/TiO2 was determined by silicon doping concentration. Water content was greatly impacted on the photocatalytic activity of SiO2/TiO2. In experiment,5% silicon doping concentration for SiO2/TiO2 was prepared at 600℃and was applied to degradation of trace methyl orange in water. Analysis's of SiO2/TiO2 characterized by XPS before and after etching showed that the Si atom was diffused to powder particle surface during heat treatment process, which leading to appear Ti4+at the outer surface, at the same time, Ti3+and oxygen at the near surface of TiO2. The key reasons for higher activity of SiO2/TiO2 were the combined effects of Ti3+ and oxygen vacancies with the co-existence of Ti4+and Ti3+could effectively separate charge.
(3) The loaded TS2.5-550 films were prepared by thermal deposition. Their degradation of HA in micro-polluted water and inactivation of E.coli were studied. The result showed that degradation rate of HA was faster than the inactivation rate of E.coli by TS25-550 films during photocatalytic process. The mechanism was that e--h+pairs produced on film under UV light illuminate had redox ability and lots of active species such as·OH and·O2- were generated when e- and h+pairs reacted with dissolved oxygen in water and water respectively. HA might be oxidized to nontoxic substances such as CO2 and H2O and E.coli cell might be damaged by these active species.
(4) Gd3+ doped SiO2/TiO2 photocatalytic materials were prepared using sol-gel method and their photocatalytic activities were studied by the mineralization of HA in slightly polluted water (pH=6.5). The results showed that HA in water was thoroughly degraded and the mineralization rate of HA was 97% by Gd-SiO2/TiO2 photocatalyst after 150 min. This was an increase nearly 38% to the value obtained for TiO2 and of 30% for that of SiO2/TiO2 when measured in parallel. We believed that the reasons for the higher activity of Gd-SiO2/TiO2 composites could be explained as follows:1) Gd3+doping inhibited the phase transformation of TiO2 from anatase to rutile, as well as grain growth. Under the same conditions, the average crystal grain of Gd-SiO2/TiO2, SiO2/TiO2 and TiO2, respectively, were 25.5 nm,35.2 nm and 37.8 nm; 2) Gd3+ doping not only enhanced the absorption light intensity within the wavelength 200 to 800 nm, but also moved the absorption band edge to shorter wavelengths, thereby broadening the band gap of the catalyst semiconductor. Under the same conditions, TiO2, SiO2/TiO2 and Gd-SiO2/TiO2 band gap was 2.57 eV,2.62 eV and 2.69 eV; 3) the amount of surface defect Ti3+ and lattice oxygen on the Gd-SiO2/TiO2 catalyst were increased. These would help to improve the photocatalytic activity.
(5) Fe doped SiO2/TiO2 photocatalysts responded to visible light were prepared and the degradation of HA in micro-polluted water was selected to investigate the photocatalytic activity of Fe-SiO2/TiO2. Characterization results showed that Fe doping not only made the absorption edge of catalyst red shift and increased the absorption intensity of visible light for the catalyst. In addition, the Fe3+/Fe2+ redox pairs were prepared on catalyst surface which were useful for separation of the e--h+ pairs. Therefore the visible light activity of Fe-SiO2/TiO2 was significantly higher than that of SiO2/TiO2 and TiO2.
本文采用两步溶胶凝胶法制备了SiO2/TiO2,通过对水中微污染有机物的降解选择出高活性的SiO2/TiO2光催化剂,并进一步对其进行修饰改性以获得更加高效的光催化剂。采用XRD、TG-DTA、FT-IR、UV-vis、XPS及TEM等测试手段对催化剂的结构进行了表征,并对其作用机理进行了深入的研究。在本实验中主要研究的内容如下：
(1)以正硅酸乙酯和钛酸四丁酯为硅源和钛源,无水乙醇为溶剂,乙酰丙酮为抑制剂,盐酸为催化剂(正硅酸乙酯水解时)制备了SiO2/TiO2。以水中微污染腐殖酸(HA)的降解效果确定了SiO2/TiO2的最佳制备条件,并对其进行了表征。结果表明,在相同焙烧温度下,硅的引入可抑制TiO2晶相的转变及催化剂晶粒的增大。当硅掺杂浓度为10%时SiO2/TiO2的最佳焙烧温度为800℃。
(2)硅掺杂浓度的大小决定着SiO2/TiO2焙烧温度的高低。水用量对催化剂的光催化活性影响较大。在此基础上于600℃下制备了硅掺杂浓度为5%的SiO2/TiO2,将其运用于水中微量甲基橙的降解中。经刻蚀前后的XPS表征分析可知,Si原子在热处理过程中向粉体颗粒的表面扩散,导致TiO2外表面出现Ti4+而在近表面产生Ti3+及氧空位。Ti3+和氧空位缺陷的联合作用、Ti4+与Ti3+的共同存在能有效分离电荷是导致SiO2/TiO2活性较高的关键原因。
(3)采用热沉积法制备了负载型TS2,550薄膜,研究了其对水中微污染HA的降解及E.coli的灭活效果。结果表明,该薄膜在光催化过程中对HA的降解速率要快于对E.coli的灭活速率。其机理为：薄膜在紫外线照射下产生了氧化还原能力较高的e-和h+。而e-和h+分别与溶解于水中的氧气和水反应生成了许多活性物种如·O2-和·OH等,这些活性物种使水中的HA氧化成无毒的物质,如CO2和H2O,并能破坏E.coli细胞致其死亡
(4)采用两步溶胶凝胶法制备了Gd3+掺杂SiO2/TiO2光催化材料,以水中微污染HA (pH=6.5)的降解及矿化研究了其光催化活性。结果表明,Gd-SiO2/TiO2光催化剂在150 min内可使水中HA彻底降解,并能使HA的矿化率达97%,比同等条件下TiO2的矿化率增加了38%,比SiO2/TiO2的矿化率增加了30%。可能的原因为：1)Gd3+的掺杂可有效抑制TiO2从锐钛矿相向金红石相的转变和晶粒的增长。同等条件下,Gd-SiO2/TiO2、SiO2/TiO2及TiO2的平均晶粒分别为25.5nm、35.2nm和37.8nm；2)Gd3+的掺杂不仅使催化剂在波长200-800nm内对光的吸收强度增强,而且使催化剂的吸收带边发生蓝移,即带隙能宽化。同等条件下,TiO2、SiO2/TiO2及Gd-SiO2/TiO2的禁带宽度分别为2.57eV、2.62eV和2.69eV；3)Gd3+的掺杂使Gd-SiO2/TiO2催化剂的表面缺陷Ti3+和晶格氧的数量增多。这些都将有利于提高催化剂的光催化活性。
(5)制备了Fe掺杂SiO2/TiO2可见光响应型光催化材料,选择微污染HA为降解目标物考察了催化剂的光催化活性。表征分析结果表明：Fe离子掺杂不仅使催化剂的吸收带边产生红移,而且增加了催化剂对可见光的吸收强度。另外,在催化剂表面出现了有利于e--h+对分离的Fe3+/Fe2+氧化还原电对。因此,Fe-SiO2/TiO2的可见光活性明显高于SiO2/TiO2和TiO2。
The increasing of organic micro-pollutants in source water has brought serious challenges for drinking water treatment. Micro-polluted raw water treated by regular water purification process can't guarantee the security of water quality. Therefore it needs to add depth process on the basis of the previous technology. In recent years, TiO2 has been attended in environmental treatment and energy exploitation due to thoroughly mineralization of organic matter, good bactericidal effect and inhibition of viral activity. However, the practical application of TiO2 has been very limited because the e--h+ pairs produced by TiO2 in the illumination are easy to recombine and TiO2 doesn't fully utilize solar energy with a larger band gap. There fore, modifications of TiO2 become a research focus to improve its photocatalytic activity.
In this paper, the SiO2/TiO2 composites were prepared by two-step sol-gel method. The degradation of micro-organic pollutant in water used to choose higher photocatalytic activity of SiO2/TiO2. And further to modify SiO2/TiO2 to obtain more efficient photocatalysts. The structures of the catalysts were characterized using XRD, TG-DTA, FT-IR, UV-vis, XPS and TEM methods.As well as, their mechanisms were studied in detail. In this experiment, the main contents of study were as follows:
(1) SiO2/TiO2 composites were prepared with tetraethoxysilane and tetrabutyl titanate as silicon source and titanium source respectively, anhydrous ethanol as solvent, acetyl acetone as inhibitor and hydrochloric acid as catalyst for hydrolysis of TEOS. The optimum preparation conditions of the SiO2/TiO2 were determined by photocatalytic degradation effects of micro-polluted humic acid in water and the characterizations of SiO2/TiO2 were analyzed. Results showed that the introduction of silicon inhibited phase transformation and particle size increase of TiO2 under the same calcining temperature. The best calcining temperature was 800℃when silicon doping concentration was 10% for SiO2/TiO2.
(2) The calcining temperature of SiO2/TiO2 was determined by silicon doping concentration. Water content was greatly impacted on the photocatalytic activity of SiO2/TiO2. In experiment,5% silicon doping concentration for SiO2/TiO2 was prepared at 600℃and was applied to degradation of trace methyl orange in water. Analysis's of SiO2/TiO2 characterized by XPS before and after etching showed that the Si atom was diffused to powder particle surface during heat treatment process, which leading to appear Ti4+at the outer surface, at the same time, Ti3+and oxygen at the near surface of TiO2. The key reasons for higher activity of SiO2/TiO2 were the combined effects of Ti3+ and oxygen vacancies with the co-existence of Ti4+and Ti3+could effectively separate charge.
(3) The loaded TS2.5-550 films were prepared by thermal deposition. Their degradation of HA in micro-polluted water and inactivation of E.coli were studied. The result showed that degradation rate of HA was faster than the inactivation rate of E.coli by TS25-550 films during photocatalytic process. The mechanism was that e--h+pairs produced on film under UV light illuminate had redox ability and lots of active species such as·OH and·O2- were generated when e- and h+pairs reacted with dissolved oxygen in water and water respectively. HA might be oxidized to nontoxic substances such as CO2 and H2O and E.coli cell might be damaged by these active species.
(4) Gd3+ doped SiO2/TiO2 photocatalytic materials were prepared using sol-gel method and their photocatalytic activities were studied by the mineralization of HA in slightly polluted water (pH=6.5). The results showed that HA in water was thoroughly degraded and the mineralization rate of HA was 97% by Gd-SiO2/TiO2 photocatalyst after 150 min. This was an increase nearly 38% to the value obtained for TiO2 and of 30% for that of SiO2/TiO2 when measured in parallel. We believed that the reasons for the higher activity of Gd-SiO2/TiO2 composites could be explained as follows:1) Gd3+doping inhibited the phase transformation of TiO2 from anatase to rutile, as well as grain growth. Under the same conditions, the average crystal grain of Gd-SiO2/TiO2, SiO2/TiO2 and TiO2, respectively, were 25.5 nm,35.2 nm and 37.8 nm; 2) Gd3+ doping not only enhanced the absorption light intensity within the wavelength 200 to 800 nm, but also moved the absorption band edge to shorter wavelengths, thereby broadening the band gap of the catalyst semiconductor. Under the same conditions, TiO2, SiO2/TiO2 and Gd-SiO2/TiO2 band gap was 2.57 eV,2.62 eV and 2.69 eV; 3) the amount of surface defect Ti3+ and lattice oxygen on the Gd-SiO2/TiO2 catalyst were increased. These would help to improve the photocatalytic activity.
(5) Fe doped SiO2/TiO2 photocatalysts responded to visible light were prepared and the degradation of HA in micro-polluted water was selected to investigate the photocatalytic activity of Fe-SiO2/TiO2. Characterization results showed that Fe doping not only made the absorption edge of catalyst red shift and increased the absorption intensity of visible light for the catalyst. In addition, the Fe3+/Fe2+ redox pairs were prepared on catalyst surface which were useful for separation of the e--h+ pairs. Therefore the visible light activity of Fe-SiO2/TiO2 was significantly higher than that of SiO2/TiO2 and TiO2.
引文
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