水处理功能化介孔二氧化钛晶体纤维的制备、表征及其光催化活性
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摘要
以水中溶解氧为氧源,n型半导体,特别是TiO2为催化剂的光催化氧化是近廿年来水处理领域的研究热点之一。但常规的纳米TiO2悬浮相体系存在着催化剂易失活、易凝聚、难回收及光能利用率低等固有弊端,负载型的固定化技术在解决催化剂回收难问题的同时,又不可避免地带来光量子效率低和催化剂易脱落等不足,悬浮相和固定化技术各自固有的弊端业已成为光催化技术走向实用的瓶颈。
本文基于改进溶胶-凝胶法开发了两种TiO2纤维制备的新方法,结合干法纺丝和水蒸气活化热处理工艺,分别获得了Si掺杂TiO2纤维和纯的TiO2连续纤维。作为水处理功能化光催化新材料,特有的形态优势使其具有使用中耐水流冲击负荷,使用后易于固液分离等特点,为有效解决上述实用化难题提供了全新的途径。采用XRD、SEM、FT-IR、DSC-TG、UV-Vis DRS、XPS及N2吸附-脱附等多种现代分析表征手段对所制备的TiO2晶体纤维进行了结构解析。结合水中难降解偶氮染料X-3B为探针污染物的光催化实验结果,较为系统的研究了不同纤维产物的晶体结构、吸光特点、表面织构等理化特性,探讨了纤维结构与催化性能之间的构效关系,研究结果为研制具有实用化前景的光催化水处理新材料提供科学依据和技术储备。本文的实验内容主要分三个部分：
第一部分,以钛酸四丁酯为Ti源,正硅酸乙酯为Si源,采用改进的无模板剂的溶胶-凝胶法,结合离心纺丝工艺成功制备了Si掺杂介孔TiO2连续纤维。纤维产物直径为10-20μm,由具有丰富介孔结构的锐钛矿TiO2纳米晶构成。实验条件下,Si的引入可以形成Ti-O-Si网络结构,这是获得连续纤维的一个至关重要的因素。通过调节Si的掺杂量(Si/Ti摩尔比：0-0.20)和热处理温度,可以控制纤维的晶型晶貌、比表面积、孔结构和催化效能。研究发现,适量Si的掺杂可以在优化TiO2纤维的表面织构,增强热稳定性和晶型稳定性的同时显著提高其光催化活性。其中,当Si/Ti摩尔比为0.15,经700℃热处理后的TiO2纤维(0.15STF-700)具有最大的比表面积和孔容,分别为127.7 m2·g-1和0.25cm3·g-1。同时也显示出最佳的光催化活性：经紫外光照射75 min后,X-3B的降解率达到99.6%；经太阳光照射3 h后,X-3B的降解率和矿化率分别达到94.7%和58.9%。研究表明,自制Ti02纤维易于分离回收和循环利用,具有良好的光化学稳定性和机械稳定性,经6次重复利用后对底物的降解率依然保持在90%以上。水处理杀菌实验结果则显示,Si掺杂介孔Ti02纤维不仅在紫外光照射下具有良好的杀菌效果,而且在无光照条件下具有一定的抑菌性。
第二部分,以自制的TiO2晶体纤维(0.15STF-700)为原材料,用1.5%的HF水溶液和5%的稀HN03水溶液作为改性剂,对纤维进行了表面改性,实现了F、N两种元素的有效共掺杂,获得了具有丰富双(介)孔结构和表面羟基的改性纤维。该纤维通过静电引力和表面离子交换对阴离子染料X-3B表现出优良的吸附效能,单纯的吸附去除率即可达84%,为通过优化预吸附富集过程强化自制纤维的光催化作用提供了实验依据。实验表明,改性处理在大幅提高紫外光催化活性的同时显示出同样优异的可见光催化活性,可见光照射45 min后X-3B的降解率即可达98%,从而为研制开发宽频和可见光响应俱佳的实用新型光催化纤维材料提供了简便宜行的方法。
第三部分,以钛酸四丁酯为钛源,聚乙烯毗咯烷酮(PVP)为交联模板剂,冰醋酸为稳定剂和螯合剂,通过优化纺丝体系的可纺性,采用改进的溶胶-凝胶法方便快捷地制备了新型的Ti02晶体纤维前驱体。流变性实验结果,该纺丝体系属于假塑性流体,PVP的加入有助于控制TiO2凝胶的粘度,当表观粘度在数Pa·s范围内即可经干法纺丝制得直径约40μm且均匀有致的前驱体纤维；另一方面,PVP不仅可以有效降低TiO2的相转变温度,而且可以通过后续的热分解产生大量的介孔结构,增大纤维产物的孔容和比表面积。实验条件下,采用独特的程序升温热处理工艺,可抑制金红石相晶粒的快速生长,获得结晶良好且比例适中的锐钛矿／金红石混晶。实验表明,该混晶结构的Ti02晶体纤维具有优异的紫外光活性,光照120 min后50 mg·L-1的X-3B的降解率可达到95%。研究结果为制备介孔Ti02混晶型纤维提供了简单高效的方法。
Photocatalytic oxidation of n-type semiconductor using dissolved oxygen in water as O source, has already become a research focus in water treatment field in the last twenty years. However, the conventional nano-TiO2 suspended system has many inherent drawbacks, such as easy deactivation, easy agglomeration owned, difficult separation and low light utilization efficiency. The technology of mounting TiO2 on supports can solve the problem, but bring about low photo quantum efficiency and easy shedding. The above factors limit the application of photocatalytic technology.
In this paper, Si-doped and pure TiO2 fibers were synthesized by two kinds of processes based on modified sol-gel method combined with dry spinning and steam-activated heat treatment, which provided a bran-new way to solve the above problems availably for its advantages in morphology and specialty in endure current strike burthen. The prepared samples were deeply investigated by XRD, SEM, FT-IR, DSC-TG, UV-Vis DRS, XPS and N2 adsorption-desorption et al. Combined with the photocatalytic experimental results, we discussed the effects of crystal structure, absorption characteristics and surface texture for the photoactivity. This paper was divided into three parts as follows:
In the first section, Si-doped mesoporous TiO2 continuous fibers were prepared by improved sol-gel method using tetrabutyl titanate and tetraethyl orthosilicate as Ti and Si source followed by centrifugal spinning. The fibers with uniform diameters about 10-20μm were consisted of nanoparticles and abundant mesopores. The addition of silica was a crucial factor for obtaining long fibers because of the formation of Ti-O-Si networks. The crystal phase, crystal morphorlogy, surface area and pore structure were controlled by varying the contents of silica and heat treatment temperatures. It was found that the proper addition of Si could improve the surface texture and enhance the thermal stability and crystal stability. When Si/Ti molar ratio was 0.15, the product heated at 700℃retained the maximal surface area and pore volume of 127.7 m2·g-1 and 0.25 cm3·g-1 respectively. It displayed the highest photoactivity of all, and the degradation rate of X-3B in aqueous solution reached 99.6% after 75 min under UV irradiation. Also, the degradation rate and the mineralization rate of X-3B were 94.7% and 58.9% after 3 h under solar irradiation, respectively. In addition, the degradation rate was also more than 90% after 6 cycles. Furthermore, the results of bactericidal test showed that TiO2 fibers not only possess bactericidal properties under UV light but also antimicrobial properties in dark.
In the second section, F, N-modified fibers were prepared, which were consisted of double-mesopore structure and surface hydroxyl groups, using 0.15STF-700 as raw material, HF and HNO3 as modifiers. And they exhibited high adsorption efficiency with removal of X-3B being over 84% through electrostatic force and ion exchange. Furthermore, collaborative photocatalysis between TiO2 and adsorbed pollutants, which resulted a substantial increase in UV-active, occurred and led to visible light response with the degradation rate of X-3B being 98% after 45 min.
In the third section, TiO2 crystal fibers were prepared using tetrabutyl titanate as Ti source, polyvinylpyrrolidone (PVP) as template and acetic acid as stabilizer and chelating agent through a novel and facile sol-gel method. On the one hand, PVP could improve the viscosity of TiO2 gel to obtain the precursor fibers with uniform diameters about 40μm by dry spinning, while the apparent viscosity reached several Pa·S and the gel belonged to pseudoplastic fluid by rotational viscometer. On the other hand, PVP could lower phase transition temperature and produce abundant mesopores through the follow-up thermal decomposition, which was helpful for increasing surface area and pore volume. The unique stage-temperature-programmed technique, heat preservation at 500℃and up to 700℃, could suppress the growth of rutile particles and obtain mixed form of anatase and rutile with suitable proportion. The photocatalytic results showed that the fibers with mixed crystal exhibited high photocatalytic activity and the degradation rate of X-3B (50 mg·L-1) reached 95% after 120 min under UV irradiation.
本文基于改进溶胶-凝胶法开发了两种TiO2纤维制备的新方法,结合干法纺丝和水蒸气活化热处理工艺,分别获得了Si掺杂TiO2纤维和纯的TiO2连续纤维。作为水处理功能化光催化新材料,特有的形态优势使其具有使用中耐水流冲击负荷,使用后易于固液分离等特点,为有效解决上述实用化难题提供了全新的途径。采用XRD、SEM、FT-IR、DSC-TG、UV-Vis DRS、XPS及N2吸附-脱附等多种现代分析表征手段对所制备的TiO2晶体纤维进行了结构解析。结合水中难降解偶氮染料X-3B为探针污染物的光催化实验结果,较为系统的研究了不同纤维产物的晶体结构、吸光特点、表面织构等理化特性,探讨了纤维结构与催化性能之间的构效关系,研究结果为研制具有实用化前景的光催化水处理新材料提供科学依据和技术储备。本文的实验内容主要分三个部分：
第一部分,以钛酸四丁酯为Ti源,正硅酸乙酯为Si源,采用改进的无模板剂的溶胶-凝胶法,结合离心纺丝工艺成功制备了Si掺杂介孔TiO2连续纤维。纤维产物直径为10-20μm,由具有丰富介孔结构的锐钛矿TiO2纳米晶构成。实验条件下,Si的引入可以形成Ti-O-Si网络结构,这是获得连续纤维的一个至关重要的因素。通过调节Si的掺杂量(Si/Ti摩尔比：0-0.20)和热处理温度,可以控制纤维的晶型晶貌、比表面积、孔结构和催化效能。研究发现,适量Si的掺杂可以在优化TiO2纤维的表面织构,增强热稳定性和晶型稳定性的同时显著提高其光催化活性。其中,当Si/Ti摩尔比为0.15,经700℃热处理后的TiO2纤维(0.15STF-700)具有最大的比表面积和孔容,分别为127.7 m2·g-1和0.25cm3·g-1。同时也显示出最佳的光催化活性：经紫外光照射75 min后,X-3B的降解率达到99.6%；经太阳光照射3 h后,X-3B的降解率和矿化率分别达到94.7%和58.9%。研究表明,自制Ti02纤维易于分离回收和循环利用,具有良好的光化学稳定性和机械稳定性,经6次重复利用后对底物的降解率依然保持在90%以上。水处理杀菌实验结果则显示,Si掺杂介孔Ti02纤维不仅在紫外光照射下具有良好的杀菌效果,而且在无光照条件下具有一定的抑菌性。
第二部分,以自制的TiO2晶体纤维(0.15STF-700)为原材料,用1.5%的HF水溶液和5%的稀HN03水溶液作为改性剂,对纤维进行了表面改性,实现了F、N两种元素的有效共掺杂,获得了具有丰富双(介)孔结构和表面羟基的改性纤维。该纤维通过静电引力和表面离子交换对阴离子染料X-3B表现出优良的吸附效能,单纯的吸附去除率即可达84%,为通过优化预吸附富集过程强化自制纤维的光催化作用提供了实验依据。实验表明,改性处理在大幅提高紫外光催化活性的同时显示出同样优异的可见光催化活性,可见光照射45 min后X-3B的降解率即可达98%,从而为研制开发宽频和可见光响应俱佳的实用新型光催化纤维材料提供了简便宜行的方法。
第三部分,以钛酸四丁酯为钛源,聚乙烯毗咯烷酮(PVP)为交联模板剂,冰醋酸为稳定剂和螯合剂,通过优化纺丝体系的可纺性,采用改进的溶胶-凝胶法方便快捷地制备了新型的Ti02晶体纤维前驱体。流变性实验结果,该纺丝体系属于假塑性流体,PVP的加入有助于控制TiO2凝胶的粘度,当表观粘度在数Pa·s范围内即可经干法纺丝制得直径约40μm且均匀有致的前驱体纤维；另一方面,PVP不仅可以有效降低TiO2的相转变温度,而且可以通过后续的热分解产生大量的介孔结构,增大纤维产物的孔容和比表面积。实验条件下,采用独特的程序升温热处理工艺,可抑制金红石相晶粒的快速生长,获得结晶良好且比例适中的锐钛矿／金红石混晶。实验表明,该混晶结构的Ti02晶体纤维具有优异的紫外光活性,光照120 min后50 mg·L-1的X-3B的降解率可达到95%。研究结果为制备介孔Ti02混晶型纤维提供了简单高效的方法。
Photocatalytic oxidation of n-type semiconductor using dissolved oxygen in water as O source, has already become a research focus in water treatment field in the last twenty years. However, the conventional nano-TiO2 suspended system has many inherent drawbacks, such as easy deactivation, easy agglomeration owned, difficult separation and low light utilization efficiency. The technology of mounting TiO2 on supports can solve the problem, but bring about low photo quantum efficiency and easy shedding. The above factors limit the application of photocatalytic technology.
In this paper, Si-doped and pure TiO2 fibers were synthesized by two kinds of processes based on modified sol-gel method combined with dry spinning and steam-activated heat treatment, which provided a bran-new way to solve the above problems availably for its advantages in morphology and specialty in endure current strike burthen. The prepared samples were deeply investigated by XRD, SEM, FT-IR, DSC-TG, UV-Vis DRS, XPS and N2 adsorption-desorption et al. Combined with the photocatalytic experimental results, we discussed the effects of crystal structure, absorption characteristics and surface texture for the photoactivity. This paper was divided into three parts as follows:
In the first section, Si-doped mesoporous TiO2 continuous fibers were prepared by improved sol-gel method using tetrabutyl titanate and tetraethyl orthosilicate as Ti and Si source followed by centrifugal spinning. The fibers with uniform diameters about 10-20μm were consisted of nanoparticles and abundant mesopores. The addition of silica was a crucial factor for obtaining long fibers because of the formation of Ti-O-Si networks. The crystal phase, crystal morphorlogy, surface area and pore structure were controlled by varying the contents of silica and heat treatment temperatures. It was found that the proper addition of Si could improve the surface texture and enhance the thermal stability and crystal stability. When Si/Ti molar ratio was 0.15, the product heated at 700℃retained the maximal surface area and pore volume of 127.7 m2·g-1 and 0.25 cm3·g-1 respectively. It displayed the highest photoactivity of all, and the degradation rate of X-3B in aqueous solution reached 99.6% after 75 min under UV irradiation. Also, the degradation rate and the mineralization rate of X-3B were 94.7% and 58.9% after 3 h under solar irradiation, respectively. In addition, the degradation rate was also more than 90% after 6 cycles. Furthermore, the results of bactericidal test showed that TiO2 fibers not only possess bactericidal properties under UV light but also antimicrobial properties in dark.
In the second section, F, N-modified fibers were prepared, which were consisted of double-mesopore structure and surface hydroxyl groups, using 0.15STF-700 as raw material, HF and HNO3 as modifiers. And they exhibited high adsorption efficiency with removal of X-3B being over 84% through electrostatic force and ion exchange. Furthermore, collaborative photocatalysis between TiO2 and adsorbed pollutants, which resulted a substantial increase in UV-active, occurred and led to visible light response with the degradation rate of X-3B being 98% after 45 min.
In the third section, TiO2 crystal fibers were prepared using tetrabutyl titanate as Ti source, polyvinylpyrrolidone (PVP) as template and acetic acid as stabilizer and chelating agent through a novel and facile sol-gel method. On the one hand, PVP could improve the viscosity of TiO2 gel to obtain the precursor fibers with uniform diameters about 40μm by dry spinning, while the apparent viscosity reached several Pa·S and the gel belonged to pseudoplastic fluid by rotational viscometer. On the other hand, PVP could lower phase transition temperature and produce abundant mesopores through the follow-up thermal decomposition, which was helpful for increasing surface area and pore volume. The unique stage-temperature-programmed technique, heat preservation at 500℃and up to 700℃, could suppress the growth of rutile particles and obtain mixed form of anatase and rutile with suitable proportion. The photocatalytic results showed that the fibers with mixed crystal exhibited high photocatalytic activity and the degradation rate of X-3B (50 mg·L-1) reached 95% after 120 min under UV irradiation.
引文
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