连续TiO_2纤维的制备及其光催化性能研究
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摘要
当前的环境污染状况日益严重,使得无毒、高效的TiO2光催化剂近年来成为新型无机功能材料研究的热点。但目前作为研究主体的TiO2纳米材料,如Ti02纳米粉体、TiO2纳米管及TiO2纳米纤维,仍存在两大基本问题：其一,由于尺寸的纳米化而难以分离回收；其二,仅在紫外光条件下具有光催化活性,可见光利用率低。这两大问题限制了该材料的工业化应用。因此,研究便于回收且光响应范围得到扩展的连续TiO2纤维对于TiO2催化剂的实际应用具有重要意义。本文采用溶胶-凝胶法制备了连续TiO2纤维(CTF),研究了具有可纺性钛溶胶的形成机制和热处理过程中工艺参数对CTF微观结构的影响规律；进行了CTF的表面造孔机理和晶粒生长动力学研究；对CTF进行无机非金属元素的掺杂改性,并以亚甲基蓝溶液和甲醛为目标降解物,研究了CTF的光催化活性。主要研究结果如下：
(1)研究了TiO2纤维先驱体结构形成机理,精确控制Ti02纤维先驱体的结构及其流变性,实现Ti02纤维先驱体可纺性。研究结果表明,在pH值为5、R小于或等于2、P为0.1%、油浴温度在120℃～135℃和油浴时间为1-2h的条件下制备的溶胶粘度为5-12Pa.s,具有可纺性。当pH值一定(pH=5)时,R≤2(molar ratio)的溶胶为线性结构,其分子式为Ti(OBu)3[OTi(OBu)2]n-1OH,溶胶具有可纺性；R>2(molar ratio)的溶胶形成网络状结构,溶胶失去可纺性。
(2)将可纺性的钛溶胶通过实验室自制高压纺丝机纺丝,热处理后得到CTF。研究了热处理方式、温度和时间对CTF纤维结构及化学组分的影响。研究发现,空气热处理和水汽活化热处理所制备的CTF直径一致(约为20-30μm),且组成纤维的纳米颗粒尺寸也一致,然而水汽活化热处理制备的CTF比表面积(32.27m2/g)比空气热处理制备的CTF的比表面积(26.66m2/g)大。热处理温度为500℃时,CTF由结晶良好的锐钛矿型和金红石型TiO2纳米晶粒组成,TiO2从锐钛矿转变为金红石型的晶型转变活化能为96kJ/mol。利用水汽活化热处理方式,在500℃下对原丝进行不同时间的热处理,对锐钛矿TiO2晶粒和金红石TiO2晶粒分别进行晶粒生长动力学研究。结果表明,500℃时,锐钛矿的晶粒生长指数为2,品粒生长速率常数为5.34×102nm2/h；金红石晶粒的生长指数为4,品粒生长速率常数为1.91×107nm4/h。水汽活化造孔机理为：CTF表面由于缺氧而碳化的有机物,与水蒸气分解所释放出的氧气发生气化反应,以CO2的形式逸出,从而在CTF表面形成孔隙。
(3)采用亚甲基蓝(MB)溶液和甲醛的光催化降解实验,评价CTF的光催化活性。在紫外灯功率(25W)和反应温度(25℃)一定的条件下,CTF对MB溶液光催化降解的最佳反应条件是：催化剂CTF的浓度为0.6g/L,pH值为7.0,MB溶液基本降解完全,且在重复使用8次后,降解率仍达到90.3%；对甲醛(10mg/L)光催化降解的最佳反应条件是：催化剂CTF浓度为0.6g/L,pH值为7.0,降解率达到98.6%。
(4)采用原位法制备了Si掺杂的连续TiO2纤维(Si-CTF),并在N2气氛下热处理,制各了Si、N共掺杂的连续Ti02纤维[(Si,N)-CTF]。结果表明,Si/Ti摩尔比(S)为5%时的溶胶具有可纺性,且在40℃以下Si掺杂可以提高溶胶粘度。Si掺杂能抑制TiO2晶粒的生长。另外,经500℃热处理后,在Si-CTF和(Si,N)-CTF的XRD图谱中仅有锐钛矿相TiO2,并未出现金红石相的衍射峰,说明Si掺杂或者Si、N共掺杂均可以抑制TiO2由锐钛矿相向金红石相转变。在可见光条件下,CTF对MB溶液基本无降解,Si-CTF对MB溶液的降解率为69.2%,(Si,N)-CTF对MB溶液的降解率则达到93.7%。
In recent years, the increasingly serious environment pollution prompts the rapid development in the photocatalytic technology with non-toxicity and high-efficiency. TiO2nano-material is perhaps the most prospecting photo-catalyst. However, the nano meter TiO2materials including TiO2nanopowder, TiO2nanotube and TiO2nanofiber, is hard to separate and recovery from the water. Therefore, a lot of studies on macroscopic and fibrous TiO2catalyst have been recently carried out. In this paper, continuous titanium dioxide fiber (CTF) was successfully synthesized by sol-gel method, and the Ti sol fabrication mechanism and the effects of the processing parameters on the CTF were investigated. The pore formation mechanism on the TiO2surface was analyzed and the grain growth kinetics was brifly investigated. Then methylene blue and formaldehyde were used as the target pollutant to study the photocatalytic activity of the CTF. In addition, the CTF was modified by Si doping and (Si, N) co-doping. The main conclusions were drawn as following:
Ti sol with spinnability was synthesized by sol-gel technique using the tetrabutyl orthotitanate as Ti source, and absolute alcohol as solvent. The effects of pH value, the molar ratio of distilled water to tetrabutyl orthotitanate (R), the molar ratio of PVP adhesive to tetrabutyl orthotitanate (P), oil bath temperature and time on the viscosity and rheological properties of the Ti sol were investigated, and the formation mechanism of spinning Ti sol was also analyzed. The optimal preparation conditions of Ti sol with spinnability were obtained:pH=5, R≤2, P=0.1%, the oil bath temperature120℃-135℃, and the oil bath time1-2hours. When R>2, the structure of the Ti sol changed from chain-like to three-dimensional network which presents poor spinnability.
The CTF were successfully prepared by the Ti sol spinning and subsequent calcination treatment. The effects of calcination methods, calcination temperature and time on the microstructure and composition of the CTF were examined by SEM, TEM and XRD. The results showed that the samples obtained by air calcination and steam activation calcination methods had similar fiber diameter (20-30μm) and nano-particle size. The CTF calcined by the two calcination methods at500℃contained anatase and rutile phases. However, the specific surface area of the steam activation sample (32.27m2·g-1) was higher than that of the air calcination one (26.66m2·g-1). Through the kinetics analysis of the DSC curves, the activation energy of phase transformation from anatase phase to rutile phase was about96kJ·mol-1
The grain growth kinetics of the CTF at500℃was researched. At500℃, the grain growth exponent and the rate constant is2,5.34×102nm2·h-1for anatase and4,1.91×107nm4·h-1for rutile TiO2phase. The carbonated organic on the surface of CTF could react with oxygen resulting from steam decomposition to form CO2. Then, the escape of CO2induced the pores formation on the surface of the CTF.
Under25℃(reaction temperature) and25W (UV lamp power), the optimal photocatalytic reaction condition for methylene blue was as follows:the CTF concentration is0.6g·L-1, and the pH value is7. Under the same condition, the optimal CTF concentration and pH value for formaldehyde (10mg·L-1) photocatalytic reaction is0.5g·L-1and5, respectively.
The Si-doped continuous TiO2fiber (Si-CTF) was prepared by in-situ method, then the (Si, N)-codoped continuous TiO2fiber ((Si, N)-CTF) was obtained by calcining the Si-CTF in nitrogen. Si-doping can improve the CTF precursor sol viscosity below40℃, and the sol has spinnability when the molar ratio S=5%(S=Si: TBOT). The diameter of nano-particles in Si-CTF (20nm) was smaller than that of CTF calcined at500℃, which indicate that the Si doping can inhibite the growth of TiO2nano-particle. In addition, XRD results showed that the Si doping or (Si, N) codoping could effectively depress the phase transformation from anatase to rutile. The MB degradation of Si-CTF and (Si, N)-CTF are69.2%and93.7%respectively.
(1)研究了TiO2纤维先驱体结构形成机理,精确控制Ti02纤维先驱体的结构及其流变性,实现Ti02纤维先驱体可纺性。研究结果表明,在pH值为5、R小于或等于2、P为0.1%、油浴温度在120℃～135℃和油浴时间为1-2h的条件下制备的溶胶粘度为5-12Pa.s,具有可纺性。当pH值一定(pH=5)时,R≤2(molar ratio)的溶胶为线性结构,其分子式为Ti(OBu)3[OTi(OBu)2]n-1OH,溶胶具有可纺性；R>2(molar ratio)的溶胶形成网络状结构,溶胶失去可纺性。
(2)将可纺性的钛溶胶通过实验室自制高压纺丝机纺丝,热处理后得到CTF。研究了热处理方式、温度和时间对CTF纤维结构及化学组分的影响。研究发现,空气热处理和水汽活化热处理所制备的CTF直径一致(约为20-30μm),且组成纤维的纳米颗粒尺寸也一致,然而水汽活化热处理制备的CTF比表面积(32.27m2/g)比空气热处理制备的CTF的比表面积(26.66m2/g)大。热处理温度为500℃时,CTF由结晶良好的锐钛矿型和金红石型TiO2纳米晶粒组成,TiO2从锐钛矿转变为金红石型的晶型转变活化能为96kJ/mol。利用水汽活化热处理方式,在500℃下对原丝进行不同时间的热处理,对锐钛矿TiO2晶粒和金红石TiO2晶粒分别进行晶粒生长动力学研究。结果表明,500℃时,锐钛矿的晶粒生长指数为2,品粒生长速率常数为5.34×102nm2/h；金红石晶粒的生长指数为4,品粒生长速率常数为1.91×107nm4/h。水汽活化造孔机理为：CTF表面由于缺氧而碳化的有机物,与水蒸气分解所释放出的氧气发生气化反应,以CO2的形式逸出,从而在CTF表面形成孔隙。
(3)采用亚甲基蓝(MB)溶液和甲醛的光催化降解实验,评价CTF的光催化活性。在紫外灯功率(25W)和反应温度(25℃)一定的条件下,CTF对MB溶液光催化降解的最佳反应条件是：催化剂CTF的浓度为0.6g/L,pH值为7.0,MB溶液基本降解完全,且在重复使用8次后,降解率仍达到90.3%；对甲醛(10mg/L)光催化降解的最佳反应条件是：催化剂CTF浓度为0.6g/L,pH值为7.0,降解率达到98.6%。
(4)采用原位法制备了Si掺杂的连续TiO2纤维(Si-CTF),并在N2气氛下热处理,制各了Si、N共掺杂的连续Ti02纤维[(Si,N)-CTF]。结果表明,Si/Ti摩尔比(S)为5%时的溶胶具有可纺性,且在40℃以下Si掺杂可以提高溶胶粘度。Si掺杂能抑制TiO2晶粒的生长。另外,经500℃热处理后,在Si-CTF和(Si,N)-CTF的XRD图谱中仅有锐钛矿相TiO2,并未出现金红石相的衍射峰,说明Si掺杂或者Si、N共掺杂均可以抑制TiO2由锐钛矿相向金红石相转变。在可见光条件下,CTF对MB溶液基本无降解,Si-CTF对MB溶液的降解率为69.2%,(Si,N)-CTF对MB溶液的降解率则达到93.7%。
In recent years, the increasingly serious environment pollution prompts the rapid development in the photocatalytic technology with non-toxicity and high-efficiency. TiO2nano-material is perhaps the most prospecting photo-catalyst. However, the nano meter TiO2materials including TiO2nanopowder, TiO2nanotube and TiO2nanofiber, is hard to separate and recovery from the water. Therefore, a lot of studies on macroscopic and fibrous TiO2catalyst have been recently carried out. In this paper, continuous titanium dioxide fiber (CTF) was successfully synthesized by sol-gel method, and the Ti sol fabrication mechanism and the effects of the processing parameters on the CTF were investigated. The pore formation mechanism on the TiO2surface was analyzed and the grain growth kinetics was brifly investigated. Then methylene blue and formaldehyde were used as the target pollutant to study the photocatalytic activity of the CTF. In addition, the CTF was modified by Si doping and (Si, N) co-doping. The main conclusions were drawn as following:
Ti sol with spinnability was synthesized by sol-gel technique using the tetrabutyl orthotitanate as Ti source, and absolute alcohol as solvent. The effects of pH value, the molar ratio of distilled water to tetrabutyl orthotitanate (R), the molar ratio of PVP adhesive to tetrabutyl orthotitanate (P), oil bath temperature and time on the viscosity and rheological properties of the Ti sol were investigated, and the formation mechanism of spinning Ti sol was also analyzed. The optimal preparation conditions of Ti sol with spinnability were obtained:pH=5, R≤2, P=0.1%, the oil bath temperature120℃-135℃, and the oil bath time1-2hours. When R>2, the structure of the Ti sol changed from chain-like to three-dimensional network which presents poor spinnability.
The CTF were successfully prepared by the Ti sol spinning and subsequent calcination treatment. The effects of calcination methods, calcination temperature and time on the microstructure and composition of the CTF were examined by SEM, TEM and XRD. The results showed that the samples obtained by air calcination and steam activation calcination methods had similar fiber diameter (20-30μm) and nano-particle size. The CTF calcined by the two calcination methods at500℃contained anatase and rutile phases. However, the specific surface area of the steam activation sample (32.27m2·g-1) was higher than that of the air calcination one (26.66m2·g-1). Through the kinetics analysis of the DSC curves, the activation energy of phase transformation from anatase phase to rutile phase was about96kJ·mol-1
The grain growth kinetics of the CTF at500℃was researched. At500℃, the grain growth exponent and the rate constant is2,5.34×102nm2·h-1for anatase and4,1.91×107nm4·h-1for rutile TiO2phase. The carbonated organic on the surface of CTF could react with oxygen resulting from steam decomposition to form CO2. Then, the escape of CO2induced the pores formation on the surface of the CTF.
Under25℃(reaction temperature) and25W (UV lamp power), the optimal photocatalytic reaction condition for methylene blue was as follows:the CTF concentration is0.6g·L-1, and the pH value is7. Under the same condition, the optimal CTF concentration and pH value for formaldehyde (10mg·L-1) photocatalytic reaction is0.5g·L-1and5, respectively.
The Si-doped continuous TiO2fiber (Si-CTF) was prepared by in-situ method, then the (Si, N)-codoped continuous TiO2fiber ((Si, N)-CTF) was obtained by calcining the Si-CTF in nitrogen. Si-doping can improve the CTF precursor sol viscosity below40℃, and the sol has spinnability when the molar ratio S=5%(S=Si: TBOT). The diameter of nano-particles in Si-CTF (20nm) was smaller than that of CTF calcined at500℃, which indicate that the Si doping can inhibite the growth of TiO2nano-particle. In addition, XRD results showed that the Si doping or (Si, N) codoping could effectively depress the phase transformation from anatase to rutile. The MB degradation of Si-CTF and (Si, N)-CTF are69.2%and93.7%respectively.
引文
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