纳米二氧化钛制备方法研究、性能研究及其应用
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摘要
纳米二氧化钛因其化学性质稳定、无毒、成本低廉且具有催化、紫外屏蔽等性能,在半导体、催化剂、纺织品功能整理等领域有着广泛应用。通过多种改性手段改善纳米二氧化钛的活性,提高其光催化效率和抗紫外整理性能是将这一技术推向实际应用的重要环节。本文采用微乳液法、溶胶—凝胶法和低温水解法制备纳米二氧化钛,并利用UV-VIS、TG-DTA、IR、XRD、SEM、TEM等多种测试手段,对改性纳米二氧化钛催化剂的光催化性能和抗紫外整理性能进行了系统的研究。
采用微乳液法在Triton X-100/正丁醇/环己烷体系中,制备了纳米二氧化钛,考察反应时间、水与表面活性剂浓度比等反应条件的影响,探讨了纳米二氧化钛的形成机制,经650℃和1000℃煅烧后可分别得到分散性较好的锐钛矿型和金红石型纳米二氧化钛粒子,其粒径分别为20～35nm和40～60nm。
利用溶胶—凝胶法通过钛酸正丁酯水解制备稀土(钆、铈、镧)掺杂和双元素铈—银、铈—铜)掺杂纳米二氧化钛,通过X射线衍射、透射电镜及紫外—可见光吸收光谱分析,稀土元素的掺杂提高了纳米二氧化钛的相变温度,而双元素掺杂则能降低纳米二氧化钛的相变温度；稀土掺杂和双元素掺杂都能减小纳米二氧化钛的粒径,其粒径在8-16nm；稀土掺杂和双元素掺杂都能提高二氧化钛的光催化活性和织物的抗紫外性能。
利用低温水解法合成纳米二氧化钛,通过控制反应时间和溶液浓度可以获得不同晶型的二氧化钛,并用1mo1·1-1的硅酸钠溶液对其进行包覆,通过光催化实验发现：催化剂中混晶的比例不同,光催化效率也不同,锐钛矿质量分数为69.8%、金红石质量分数为30.2%时,光催化降解率最高可达95.7%。通过对纳米二氧化钛整理后的织物进行测试,发现经整理后的棉织物具有突出的抗紫外性能和服用性能,将织物进行10次洗涤后,其紫外透过率基本上没有发生改变,SiO2：TiO2=5%包覆时抗紫外效果最好,金红石型次之,最后是锐钛矿。
Nanometer titania has been widely used in such fields as semiconductor, catalyst and functional finishing of textile because of its stable chemical property, no toxicity, low cost, reasonable photocatalytic and UV resistance performance. Photocatalyst is the key part in photocatalysis, and further improvement on its activity, efficiency and UV resistance by selective treatment to modify the properties of the particles is an essential step to apply this novel technology. In this dissertation, titania nanoparticles (nano-TiO2) were prepared by microemulsion, sol-gel and low-temperature hydrolysis process. The photocatalytic activity and UV resistance finishing capacity of modified nanoparticle TiO2have been characterized by UV-VIS、TG-DTA、 IR、XRD、SEM、TEM.
Titania nanoparticles were prepared by microemulsion process with titanium chloride and aqueous ammonia in Triton X-100/n-butyl alcohol/cyclohexane. Particle size of the hydrated TiO2increases with increase in reaction time as well as surfactant-to-water molar ratio. Hydrated TiO2was calcined at650℃and1000℃and characterised by UV-VIS, TGA, DTA, XRD and TEM analyses. XRD and TEM results demonstrate that the anatase and rutile nano-TiO2possess better dispersity, with particle size20-35nm and40-60nm respectively.
The rare earth(Gd, Ce, La) doped and the double metallic ions (Ce-Cu, Ce-Ag) doped titania nanoparticles were prepared by a sol-gel process with Ti(OC4H9)4as precursor and characterized by XRD, TEM and UV-VIS. The morphologies of the particles varied with the doping condition. The rare earth doping increases the phase transition temperature converting anatase phase into rutile phase. The double metallic ions doping decreases the phase transition temperature. The doping (either the rare earth doping or the double metallic ions doping) can decrease the grain size of TiO2particles, which was8-16nm. The photocatalytic activities of the doped nano-TiO2were investigated by the photocatalytic degradation of methyl orange under ultraviolet lamp. The results showed that the photocatalytic performance of TiO2and UV resistance of finished fabrics was enhanced greatly owing to doping ions.
Titania nanoparticles were prepared through low-temperature hydrolysis, and the initial material was Ti(OC4H9)4. Anatase, rutile and mixed nano-TiO2were synthesized by changing the ratio of initial materials and reaction time, and were wrapped with lmol·l-1sodium silicate. XRD, TEM, UV-VIS, IR and TG spectra were employed to characterize the nanometer particles. The photocatalytic activities of the samples were investigated by the photocatalytic degradation of methyl orange. The results revealed that the photocatalytic activity was excellent when TiO2powers contain69.8%anatase and30.2%rutile phase, and methyl orange was degraded by95.7%. The cotton fabrics were finished by nano-TiO2and its clothing performance was tested and analyzed. The results revealed that functional finishing on cotton fabrics was feasible by liquid phase at low temperature, the ultraviolet transmitting rate changed a little after10times of washing, and the fabrics treated with the finishing agent had excellent UV resistance and wear ability. UV resistance of the fabrics is best when SiO2:TiO2is5%.
采用微乳液法在Triton X-100/正丁醇/环己烷体系中,制备了纳米二氧化钛,考察反应时间、水与表面活性剂浓度比等反应条件的影响,探讨了纳米二氧化钛的形成机制,经650℃和1000℃煅烧后可分别得到分散性较好的锐钛矿型和金红石型纳米二氧化钛粒子,其粒径分别为20～35nm和40～60nm。
利用溶胶—凝胶法通过钛酸正丁酯水解制备稀土(钆、铈、镧)掺杂和双元素铈—银、铈—铜)掺杂纳米二氧化钛,通过X射线衍射、透射电镜及紫外—可见光吸收光谱分析,稀土元素的掺杂提高了纳米二氧化钛的相变温度,而双元素掺杂则能降低纳米二氧化钛的相变温度；稀土掺杂和双元素掺杂都能减小纳米二氧化钛的粒径,其粒径在8-16nm；稀土掺杂和双元素掺杂都能提高二氧化钛的光催化活性和织物的抗紫外性能。
利用低温水解法合成纳米二氧化钛,通过控制反应时间和溶液浓度可以获得不同晶型的二氧化钛,并用1mo1·1-1的硅酸钠溶液对其进行包覆,通过光催化实验发现：催化剂中混晶的比例不同,光催化效率也不同,锐钛矿质量分数为69.8%、金红石质量分数为30.2%时,光催化降解率最高可达95.7%。通过对纳米二氧化钛整理后的织物进行测试,发现经整理后的棉织物具有突出的抗紫外性能和服用性能,将织物进行10次洗涤后,其紫外透过率基本上没有发生改变,SiO2：TiO2=5%包覆时抗紫外效果最好,金红石型次之,最后是锐钛矿。
Nanometer titania has been widely used in such fields as semiconductor, catalyst and functional finishing of textile because of its stable chemical property, no toxicity, low cost, reasonable photocatalytic and UV resistance performance. Photocatalyst is the key part in photocatalysis, and further improvement on its activity, efficiency and UV resistance by selective treatment to modify the properties of the particles is an essential step to apply this novel technology. In this dissertation, titania nanoparticles (nano-TiO2) were prepared by microemulsion, sol-gel and low-temperature hydrolysis process. The photocatalytic activity and UV resistance finishing capacity of modified nanoparticle TiO2have been characterized by UV-VIS、TG-DTA、 IR、XRD、SEM、TEM.
Titania nanoparticles were prepared by microemulsion process with titanium chloride and aqueous ammonia in Triton X-100/n-butyl alcohol/cyclohexane. Particle size of the hydrated TiO2increases with increase in reaction time as well as surfactant-to-water molar ratio. Hydrated TiO2was calcined at650℃and1000℃and characterised by UV-VIS, TGA, DTA, XRD and TEM analyses. XRD and TEM results demonstrate that the anatase and rutile nano-TiO2possess better dispersity, with particle size20-35nm and40-60nm respectively.
The rare earth(Gd, Ce, La) doped and the double metallic ions (Ce-Cu, Ce-Ag) doped titania nanoparticles were prepared by a sol-gel process with Ti(OC4H9)4as precursor and characterized by XRD, TEM and UV-VIS. The morphologies of the particles varied with the doping condition. The rare earth doping increases the phase transition temperature converting anatase phase into rutile phase. The double metallic ions doping decreases the phase transition temperature. The doping (either the rare earth doping or the double metallic ions doping) can decrease the grain size of TiO2particles, which was8-16nm. The photocatalytic activities of the doped nano-TiO2were investigated by the photocatalytic degradation of methyl orange under ultraviolet lamp. The results showed that the photocatalytic performance of TiO2and UV resistance of finished fabrics was enhanced greatly owing to doping ions.
Titania nanoparticles were prepared through low-temperature hydrolysis, and the initial material was Ti(OC4H9)4. Anatase, rutile and mixed nano-TiO2were synthesized by changing the ratio of initial materials and reaction time, and were wrapped with lmol·l-1sodium silicate. XRD, TEM, UV-VIS, IR and TG spectra were employed to characterize the nanometer particles. The photocatalytic activities of the samples were investigated by the photocatalytic degradation of methyl orange. The results revealed that the photocatalytic activity was excellent when TiO2powers contain69.8%anatase and30.2%rutile phase, and methyl orange was degraded by95.7%. The cotton fabrics were finished by nano-TiO2and its clothing performance was tested and analyzed. The results revealed that functional finishing on cotton fabrics was feasible by liquid phase at low temperature, the ultraviolet transmitting rate changed a little after10times of washing, and the fabrics treated with the finishing agent had excellent UV resistance and wear ability. UV resistance of the fabrics is best when SiO2:TiO2is5%.
引文
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