离子液体协同TiO_2光催化剂制备方法及降解氰、苯酚的性能与机理
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摘要
如何高效、环保的处理工业废水中的无机、有机污染物是当前世界范围内的一个重要的环境问题。而光催化技术作为最有发展前景的环境污染治理技术之一,越来越受到人们的重视。二氧化钛由于其自身优点,如无毒,光稳定,化学稳定,价廉,对反应底物的光催化降解彻底等,已经成为了目前最为常用的光催化剂。但是到目前为止,二氧化钛光催化技术仍然存在有两大问题有待解决,即较低的可见光利用率和较低的光量子产率。因此,如何通过改性有效地提高二氧化钛对可见光的利用,降低光生电子-空穴对的复合几率,提高量子效率,是当前二氧化钛光催化技术研究的重点。本文基于离子液体在微纳米材料制备方面的显著特性,采用离子液体作为二氧化钛制备的介质,对其进行改性,以期能够有效拓宽二氧化钛的激发光辐宽,改善其表面性质及结晶类型,提高可见光利用率和量子效率。
目前的水体污染物中,主要来源于工业废水排放的氰化物和苯酚是公认的强毒性难降解物质,对环境危害较大。本文分别选择氰化物和苯酚作为光催化降解的模型污染物,从二氧化钛光催化剂的改性制备入手,创新的以1-丁基-3-甲基咪唑六氟磷酸盐([Bmim]PF6)离子液体作为反应介质,利用微波辅助手段,采用溶胶-凝胶法制备了改性二氧化钛光催化剂以及多种金属离子掺杂的改性二氧化钛光催化剂,并对改性二氧化钛光催化降解含氰废水和苯酚废水的反应进行了系统研究,同时研究了改性二氧化钛光催化剂的固定化。通过X射线衍射(XRD)、电镜扫描(SEM)、紫外-可见吸收光谱(UV-Vis)等分析手段对制备的各种催化剂进行了表征,以自行设计的光催化反应器进行光催化降解反应,首次详细探讨了影响改性二氧化钛光催化剂降解含氰废水和苯酚废水的多种因素和可能的内在原因,为优化改性二氧化钛光催化剂和深入研究光催化机理提供了有意义的信息,为改性二氧化钛光催化的进一步应用打下了一定的基础,具体研究内容和结果如下：
1)以[Bmim]PF6离子液体作为反应介质,利用微波辅助手段,采用溶胶-凝胶法制备了改性二氧化钛光催化剂,得到的二氧化钛催化剂颗粒形状均匀、分散性较好、品貌良好,晶型结构主要以锐钛矿型存在,光吸收范围拓展至450nm左右。研究了微波辅助溶胶-凝胶法合成二氧化钛光催化剂的方法,并且考察了离子液体[Bmim]PF6的添加量对催化剂合成的影响,制备条件的最佳配比是[Bmim] PF6与钛酸丁酯((TTIP)的物质的量比为0.4：1。
2)利用自制的改性二氧化钛光催化剂对模拟含氰废水进行光催化降解研究,考察了一些操作参数对光催化降解苯酚的影响,如pH值、催化剂浓度、氰根离子浓度、催化剂晶型和光源条件等。通过实验验证了,经过10小时在8w的紫外灯光照射下进行光催化反应,在制备的改性二氧化钛催化剂的用量为300mg/L时,晶型配比金红石型和锐钛矿型二氧化钛以1：1的比例进行配制,在体系pH值为4,初始浓度为60mg/L,在较大的光照面积(800cm2)条件下,得到的光催化效率较高,对含氰废水的降解率可达100%。
3)利用自制的改性二氧化钛光催化剂对模拟苯酚废水进行光催化降解研究,考察了一些操作参数对光催化降解苯酚的影响,如pH值、催化剂浓度、苯酚浓度、催化剂晶型和光源条件等。通过实验验证了,经过20小时在8w的紫外灯光照射下进行光催化反应,制备的改性二氧化钛催化剂的用量为300mg/L时,晶型配比金红石型和锐钛矿型二氧化钛以1：2的比例进行配制,在体系pH值为4,初始浓度为50mg/L,在较大的光照面积(800cm2)下,得到的光催化活性较高,对苯酚废水的降解率可达100%。
4)首次采用溶胶凝胶法与微波法协同制备了以离子液体[Bmim]PF6为介质,利用Cu2+、Ni2+、Pb2+、Zn2+、Fe3+五种金属离子分别掺杂制备了二氧化钛光催化剂,发现金属离子的掺杂使得二氧化钛的光谱吸收发生了较为明显的红移,光响应波长范围拓宽至可见光范围。并利用上述五种催化剂在自制的光催化反应器中分别对模拟含氰废水和苯酚废水进行了光催化降解实验,考察了影响光催化活性的各种因素。
5)通过实验发现,Cu2+离子的掺杂可以有效提高二氧化钛光催化剂对含氰废水的降解效率,且在Cu2+离子掺杂浓度为0.5%(物质的量分数)时,得到的降解效率最高。在室内自然光的照射条件下,经过10小时的催化反应,对含氰废水的降解率达到了80.6%。Fe3+离子的掺杂可以有效提高二氧化钛光催化剂对苯酚废水的降解效率,且在Fe3+离子掺杂浓度为0.5%(物质的量分数)时,得到的降解效率最高。在室内自然光的照射条件下,经过20小时的催化反应,对苯酚废水的降解率达到了81.3%。
6)首次以天然沸石、改性蛇纹石、砂质粘土为载体,利用溶胶凝胶法制备了TiO2/沸石光催化剂,TiO2/改性蛇纹石光催化剂、TiO2/砂质粘土光催化剂。并利用XRD和SEM对制备好的复合材料进行了表征。通过光催化降解实验发现,天然沸石和改性蛇纹石均可显著提高光催化活性,可作为良好的二氧化钛载体材料,而砂质粘土则不适宜采用。
7)对以离子液体[Bmim]PF6作为介质、金属离掺杂在二氧化钛改性制备过程中的机理作用进行了研究,对改性二氧化钛光催化降解氰化物和苯酚的机理以及反应动力学进行初步的探讨和分析。
以上结果使设计和构建可见光下的高活性的二氧化钛催化剂成为可能,为寻求可实用化的降解水体污染的光催化剂提供了一定的理论基础及技术参考。
Industrial wastewater containing inorganic and organic pollutants has always been a main environmental concern throughout the world.The TiO2photocatalyst has been the focus of water purification processing studies because of its non-poisonous feature high activity,security,stability,low cost and other advantages.Electron-hole pairs will be generated upon excitation by light with energy equal to or greater than the bandgap of TiO2.Since the strong oxidative power of the photogenerated holes made it possible to oxidize most of the organic pollutants and to transform some of the toxic inorganic pollutants into harmless forms as well,photocatalysis of TiO2is significant for environmental remediation.Based on the distinct characteristics of ionic liquid in preparation of micro/nano materials,the ionic liquid was used as the medium in preparation of TiO2for modification.It is hoped that the inspire light width could be widened,the surface properties and crystallization type could be improved and the visible utilization and quantum efficiency could be enhanced.
The CN-and phenol were the main environmental pollutants from industrial waste water which recognized as the strong toxic and hard-degradation substances.This research aimed at removal of CN-and phenol respectively from water using photocatalysis and modified-Ti02and metal ions doped modified-TiO2,that were prepared by a sol-gel method which use [Bmim]PF6as reaction medium and microwave-assisted means.The oxidation and reduction capability of the TiO2powder have been studied comprehensively from some important factors of the photocatalytic CN-and phenol decomposition in the reaction and the immobilization of TiO2was also studied. With the help of X-ray diffraction(XRD),SEM,UV-Vis,after a series of photocatalytic experiments of degradation of CN" and phenol with using the new photoreactor which was built by ourselves,we studied many facators affecting the photocatalytic activity of TiO2powders.More information was provided to optimize TiO2powder photocatalyst and its may be helpful for further study of photocatalytic mechanisms.Some results are as follows.
1) The modified-TiO2was prepared by a sol-gel method which use [Bmim]PF6as reaction medium and microwave-assisted means and had an equality shape and high dispersion.The TiO2powder was made up mauly by anatase type and its absorption range of light was expanded to450nm.The sol-gel method with microwave-assisted means was studied and the adding amount of [Bmim]PF6was also investigated.The best ratio is n[Bmim] PF6:nTTIP=0.4:1.
2) The oxidation and reduction capability of the modified-TiO2had been studied comprehensively from some important factors of the photocatalytic CN-decompose in the reaction The effects of various operational parameters such as pH, catalyst concentration, CN-concentration, the quality proportion of anatase type and rutile type and illumination condition on the photocatalytic degradation of CN-were investigated. After10hours8w UV irradiation, the results showed that the pH of the aqueous solution was4,the initial concentration of CN-was60mg/L;,the quality proportion of anatase type and rutile type was1:1,ratio of the solution was300mgTiO2/L,800cm(?)illumination area, under such conditions,the degradation rate could be enhanced to about100%when the modified-Ti02was used.
3) The oxidation and reduction capability of the modified-TiO2had been studied comprehensively from some important factors of the photocatalytic phenol decompose in the reaction. The effects of various operational parameters such as pH, catalyst concentration, phenol concentration, the quality proportion of anatase type and rutile type and illumination condition on the photocatalytic degradation of pheno were investigated. After20hours8w UV irradiation, the results showed that the pH of the aqueous solution was4,the initial concentration of phenol was50mg/L;the quality proportion of anatase type and rutile type was1:2,ratio of the solution was300mgTiO2/L,800cm2illumination area, under such conditions,the degradation rate could be enhanced to about100%when the modified-TiO2was used.
4) The metal ions doped modified-TiO2was prepared by a sol-gel method which use [Bmim]PF6as reaction medium and microwave-assisted means and doped by Cu2+,Ni2+,Pb2+,Zn2+,Fe3+. In the studies of light absorption performance, the photon exeited wavelength of metal ions doped modified-TiO2powder were broaden to visible light.The oxidation and reduction capability of the metal ions doped modified-TiO2had been studied comprehensively from some important factors of the photocatalytic CN-and phenol decompose in the reaction.
5) Through the experiments it could be discovered that doped with Cu2+could enhance the degradation rate of CN".TiO2photocatalysts co-doped with Cu2+can gain the best degradation efficiency when the doping quality is0.5%.After10hours indoor nature light photocatalytic reaction,the degradation rate of CN-could achieve to about80%.Through the experiments it could be discovered that doped with Fe3+could enhance the degradation rate of phenol.TiO2photocatalysts co-doped with Fe3+can gain the best degradation efficiency when the doping quality is0.5%.After20hours indoor nature light photocatalytic reaction,the degradation rate of phenol could achieve to about81.3%.
6) The TiO2coated on natural zeolite,dauk and modified serpentine were prepared by sol-gel method.The TiO2/natural zeolite composite,TiO2dauk composite and TiO2/modified serpentine composite were charaeterized by XRD,and SEM.The laboratorial results showed that the natural zeolite and modified serpentine could consequently enhances the photocatalytic activity of TiO2while dauk could not.
7) The reaction mechanisms of TiO2preparation process which using [Bmim]PF6as reaction medium and doping with metal ions were studied.The mechanisms and reaction kinetics of photocatalytic degradation of CN-and phenol were preliminary discussed and analyzed.
The results above maybe helpful to design and construct photocatalyst which using to decompose CN-and phenol with high activity and provide certain theoretical foundation and technical reference for practical degradation of water pollution.
目前的水体污染物中,主要来源于工业废水排放的氰化物和苯酚是公认的强毒性难降解物质,对环境危害较大。本文分别选择氰化物和苯酚作为光催化降解的模型污染物,从二氧化钛光催化剂的改性制备入手,创新的以1-丁基-3-甲基咪唑六氟磷酸盐([Bmim]PF6)离子液体作为反应介质,利用微波辅助手段,采用溶胶-凝胶法制备了改性二氧化钛光催化剂以及多种金属离子掺杂的改性二氧化钛光催化剂,并对改性二氧化钛光催化降解含氰废水和苯酚废水的反应进行了系统研究,同时研究了改性二氧化钛光催化剂的固定化。通过X射线衍射(XRD)、电镜扫描(SEM)、紫外-可见吸收光谱(UV-Vis)等分析手段对制备的各种催化剂进行了表征,以自行设计的光催化反应器进行光催化降解反应,首次详细探讨了影响改性二氧化钛光催化剂降解含氰废水和苯酚废水的多种因素和可能的内在原因,为优化改性二氧化钛光催化剂和深入研究光催化机理提供了有意义的信息,为改性二氧化钛光催化的进一步应用打下了一定的基础,具体研究内容和结果如下：
1)以[Bmim]PF6离子液体作为反应介质,利用微波辅助手段,采用溶胶-凝胶法制备了改性二氧化钛光催化剂,得到的二氧化钛催化剂颗粒形状均匀、分散性较好、品貌良好,晶型结构主要以锐钛矿型存在,光吸收范围拓展至450nm左右。研究了微波辅助溶胶-凝胶法合成二氧化钛光催化剂的方法,并且考察了离子液体[Bmim]PF6的添加量对催化剂合成的影响,制备条件的最佳配比是[Bmim] PF6与钛酸丁酯((TTIP)的物质的量比为0.4：1。
2)利用自制的改性二氧化钛光催化剂对模拟含氰废水进行光催化降解研究,考察了一些操作参数对光催化降解苯酚的影响,如pH值、催化剂浓度、氰根离子浓度、催化剂晶型和光源条件等。通过实验验证了,经过10小时在8w的紫外灯光照射下进行光催化反应,在制备的改性二氧化钛催化剂的用量为300mg/L时,晶型配比金红石型和锐钛矿型二氧化钛以1：1的比例进行配制,在体系pH值为4,初始浓度为60mg/L,在较大的光照面积(800cm2)条件下,得到的光催化效率较高,对含氰废水的降解率可达100%。
3)利用自制的改性二氧化钛光催化剂对模拟苯酚废水进行光催化降解研究,考察了一些操作参数对光催化降解苯酚的影响,如pH值、催化剂浓度、苯酚浓度、催化剂晶型和光源条件等。通过实验验证了,经过20小时在8w的紫外灯光照射下进行光催化反应,制备的改性二氧化钛催化剂的用量为300mg/L时,晶型配比金红石型和锐钛矿型二氧化钛以1：2的比例进行配制,在体系pH值为4,初始浓度为50mg/L,在较大的光照面积(800cm2)下,得到的光催化活性较高,对苯酚废水的降解率可达100%。
4)首次采用溶胶凝胶法与微波法协同制备了以离子液体[Bmim]PF6为介质,利用Cu2+、Ni2+、Pb2+、Zn2+、Fe3+五种金属离子分别掺杂制备了二氧化钛光催化剂,发现金属离子的掺杂使得二氧化钛的光谱吸收发生了较为明显的红移,光响应波长范围拓宽至可见光范围。并利用上述五种催化剂在自制的光催化反应器中分别对模拟含氰废水和苯酚废水进行了光催化降解实验,考察了影响光催化活性的各种因素。
5)通过实验发现,Cu2+离子的掺杂可以有效提高二氧化钛光催化剂对含氰废水的降解效率,且在Cu2+离子掺杂浓度为0.5%(物质的量分数)时,得到的降解效率最高。在室内自然光的照射条件下,经过10小时的催化反应,对含氰废水的降解率达到了80.6%。Fe3+离子的掺杂可以有效提高二氧化钛光催化剂对苯酚废水的降解效率,且在Fe3+离子掺杂浓度为0.5%(物质的量分数)时,得到的降解效率最高。在室内自然光的照射条件下,经过20小时的催化反应,对苯酚废水的降解率达到了81.3%。
6)首次以天然沸石、改性蛇纹石、砂质粘土为载体,利用溶胶凝胶法制备了TiO2/沸石光催化剂,TiO2/改性蛇纹石光催化剂、TiO2/砂质粘土光催化剂。并利用XRD和SEM对制备好的复合材料进行了表征。通过光催化降解实验发现,天然沸石和改性蛇纹石均可显著提高光催化活性,可作为良好的二氧化钛载体材料,而砂质粘土则不适宜采用。
7)对以离子液体[Bmim]PF6作为介质、金属离掺杂在二氧化钛改性制备过程中的机理作用进行了研究,对改性二氧化钛光催化降解氰化物和苯酚的机理以及反应动力学进行初步的探讨和分析。
以上结果使设计和构建可见光下的高活性的二氧化钛催化剂成为可能,为寻求可实用化的降解水体污染的光催化剂提供了一定的理论基础及技术参考。
Industrial wastewater containing inorganic and organic pollutants has always been a main environmental concern throughout the world.The TiO2photocatalyst has been the focus of water purification processing studies because of its non-poisonous feature high activity,security,stability,low cost and other advantages.Electron-hole pairs will be generated upon excitation by light with energy equal to or greater than the bandgap of TiO2.Since the strong oxidative power of the photogenerated holes made it possible to oxidize most of the organic pollutants and to transform some of the toxic inorganic pollutants into harmless forms as well,photocatalysis of TiO2is significant for environmental remediation.Based on the distinct characteristics of ionic liquid in preparation of micro/nano materials,the ionic liquid was used as the medium in preparation of TiO2for modification.It is hoped that the inspire light width could be widened,the surface properties and crystallization type could be improved and the visible utilization and quantum efficiency could be enhanced.
The CN-and phenol were the main environmental pollutants from industrial waste water which recognized as the strong toxic and hard-degradation substances.This research aimed at removal of CN-and phenol respectively from water using photocatalysis and modified-Ti02and metal ions doped modified-TiO2,that were prepared by a sol-gel method which use [Bmim]PF6as reaction medium and microwave-assisted means.The oxidation and reduction capability of the TiO2powder have been studied comprehensively from some important factors of the photocatalytic CN-and phenol decomposition in the reaction and the immobilization of TiO2was also studied. With the help of X-ray diffraction(XRD),SEM,UV-Vis,after a series of photocatalytic experiments of degradation of CN" and phenol with using the new photoreactor which was built by ourselves,we studied many facators affecting the photocatalytic activity of TiO2powders.More information was provided to optimize TiO2powder photocatalyst and its may be helpful for further study of photocatalytic mechanisms.Some results are as follows.
1) The modified-TiO2was prepared by a sol-gel method which use [Bmim]PF6as reaction medium and microwave-assisted means and had an equality shape and high dispersion.The TiO2powder was made up mauly by anatase type and its absorption range of light was expanded to450nm.The sol-gel method with microwave-assisted means was studied and the adding amount of [Bmim]PF6was also investigated.The best ratio is n[Bmim] PF6:nTTIP=0.4:1.
2) The oxidation and reduction capability of the modified-TiO2had been studied comprehensively from some important factors of the photocatalytic CN-decompose in the reaction The effects of various operational parameters such as pH, catalyst concentration, CN-concentration, the quality proportion of anatase type and rutile type and illumination condition on the photocatalytic degradation of CN-were investigated. After10hours8w UV irradiation, the results showed that the pH of the aqueous solution was4,the initial concentration of CN-was60mg/L;,the quality proportion of anatase type and rutile type was1:1,ratio of the solution was300mgTiO2/L,800cm(?)illumination area, under such conditions,the degradation rate could be enhanced to about100%when the modified-Ti02was used.
3) The oxidation and reduction capability of the modified-TiO2had been studied comprehensively from some important factors of the photocatalytic phenol decompose in the reaction. The effects of various operational parameters such as pH, catalyst concentration, phenol concentration, the quality proportion of anatase type and rutile type and illumination condition on the photocatalytic degradation of pheno were investigated. After20hours8w UV irradiation, the results showed that the pH of the aqueous solution was4,the initial concentration of phenol was50mg/L;the quality proportion of anatase type and rutile type was1:2,ratio of the solution was300mgTiO2/L,800cm2illumination area, under such conditions,the degradation rate could be enhanced to about100%when the modified-TiO2was used.
4) The metal ions doped modified-TiO2was prepared by a sol-gel method which use [Bmim]PF6as reaction medium and microwave-assisted means and doped by Cu2+,Ni2+,Pb2+,Zn2+,Fe3+. In the studies of light absorption performance, the photon exeited wavelength of metal ions doped modified-TiO2powder were broaden to visible light.The oxidation and reduction capability of the metal ions doped modified-TiO2had been studied comprehensively from some important factors of the photocatalytic CN-and phenol decompose in the reaction.
5) Through the experiments it could be discovered that doped with Cu2+could enhance the degradation rate of CN".TiO2photocatalysts co-doped with Cu2+can gain the best degradation efficiency when the doping quality is0.5%.After10hours indoor nature light photocatalytic reaction,the degradation rate of CN-could achieve to about80%.Through the experiments it could be discovered that doped with Fe3+could enhance the degradation rate of phenol.TiO2photocatalysts co-doped with Fe3+can gain the best degradation efficiency when the doping quality is0.5%.After20hours indoor nature light photocatalytic reaction,the degradation rate of phenol could achieve to about81.3%.
6) The TiO2coated on natural zeolite,dauk and modified serpentine were prepared by sol-gel method.The TiO2/natural zeolite composite,TiO2dauk composite and TiO2/modified serpentine composite were charaeterized by XRD,and SEM.The laboratorial results showed that the natural zeolite and modified serpentine could consequently enhances the photocatalytic activity of TiO2while dauk could not.
7) The reaction mechanisms of TiO2preparation process which using [Bmim]PF6as reaction medium and doping with metal ions were studied.The mechanisms and reaction kinetics of photocatalytic degradation of CN-and phenol were preliminary discussed and analyzed.
The results above maybe helpful to design and construct photocatalyst which using to decompose CN-and phenol with high activity and provide certain theoretical foundation and technical reference for practical degradation of water pollution.
引文
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