分子筛负载纳米TiO_2的制备及其吸附与光催化性能研究
摘要
纳米TiO_2因光催化氧化还原能力强、价廉、无毒和物理化学性质稳定等优点备受人们关注。精细纳米TiO_2粉末直接用于废水处理中尽管其降解效率高，但存在分离回收难且易失活等问题，限制了其实际应用。制备负载型纳米TiO_2光催化剂，既可以解决催化剂分离回收的难题，还可以克服催化剂颗粒易团聚和稳定性差的缺点，甚至在载体-TiO_2复合物表面产生一个底物富集环境，提高光催化降解效率。本文在查阅大量文献的基础上，综述了分子筛负载TiO_2催化剂及其疏水改性的研究进展，确定了本文关于微孔HZSM-5负载纳米TiO_2降解甲基橙的研究和含模板剂具有疏水性的MCM-41及其负载TiO_2对有机氯化物的吸附与光催化降解研究在理论和实际中的意义。
分别以钛氧草酸铵、钛酸丁酯和P25型TiO_2为钛源，相应采用浸渍法、溶胶-凝胶法和固相扩散法制备了三种HZSM-5分子筛负载型纳米TiO_2光催化剂，并在紫外光下对甲基橙（MO，methyl orange）进行了光催化降解性能考察。结果表明，采用方法简单易控制且无需有机溶剂的浸渍法制备的催化剂对MO的去除效果相较用溶胶-凝胶法和固相扩散法制备的样品更好。在此基础上，采用浸渍法制备催化剂，考察了TiO_2负载量和分子筛的Si/Al比对甲基橙降解率的影响。实验表明，TiO_2负载量为15 wt%、HZSM-5分子筛Si/Al=500时，TiO_2/HZSM-5催化剂对降解MO具有更高的催化活性。应用X射线衍射（XRD）、紫外-可见漫反射光谱（UV-vis DRS）和BET比表面积分析等技术对催化剂结构进行表征，结果表明，光催化剂具有较高的比表面积，并且TiO_2在分子筛外表面分散良好，导致其具有高的光催化活性。
以未煅烧含有机模板剂的MCM-41（记作MCM-41-dry）和已煅烧MCM-41（记作MCM-41-cal）为吸附剂对邻氯苯酚（o-CP，To-chlorophenolT）和邻氯硝基苯（o-CNB，To-chloronitrobenzeneT）进行吸附实验。结果表明，相比MCM-41-cal，MCM-41-dry对o-CP和o-CNB有更高的吸附能力，这可能归因于模板剂的存在使MCM-41-dry具有更高的疏水性。此外，还研究了吸附剂的用量、pH值、目标污染的初始浓度和共存离子等因素对MCM-41-dry吸附效果的影响。研究表明，pH值和共存的离子对MCM-41-dry的吸附效果影响较大，MCM-41-dry对o-CP的吸附容量高于o-CNB，MCM-41-dry对o-CP和o-CNB的吸附符合Freundlich吸附平衡模型。
分别以MCM-41-dry和MCM-41-cal为载体制备负载型纳米TiO_2催化剂，并在紫外光下对o-CP进行了光催化降解性能考察。结果表明，含模板剂的TiO_2/MCM-41-dry催化剂对o-CP及其中间产物有更短的降解去除时间。此外，还研究了溶液pH值和o-CP初始浓度对TiO_2/MCM-41-dry光催化降解o-CP的影响。结果表明，在pH值为2~11范围内，pH值越高，光催化完全降解o-CP的时间越短；反应物的初始浓度越高，相同反应条件下，其完全降解o-CP的时间越长。
Nano-TiO_2 has received much attention due to its strong redox ability, chemical stability,non-toxicity, and cheapness. However, the nano-TiO_2 powder is easy to lose in liquid-phasephotocatalytic reaction and difficult to be collected after the reaction, which disturbs therecycle of photocatalyst and hampers the practical applications of nano-TiO_2 powder.Immobilization of nano-TiO_2 overcomes the difficulties in separation and recycles ofphotocatalyst, enhances the concentration of substrates near the TiO_2, as well as restrainsaggregation and deactivation of the catalyst particles. In this work, the research on nano-TiO_2supported on zeolites or porous silica and their hydrophobical modification was reviewed.Therefore, the significance of theory and practice about the study on photocatalyticdegradation of MO over TiO_2/HZSM-5, as well as adsorption and photocatalytic properties ofTiO_2/MCM-41, which includes cationic template within the framework of MCM-41-drymaterials, has been shown in this paper.
TiO_2/HZSM-5 photocatalysts were prepared by impregnation, sol-gel, and solid statedispersion methods, using ammonium titanyl oxalate, tetrabutyl titanate, and P-25 as titaniumsource, respectively. The photocatalytic reactivity of the prepared samples for the degradationof methyl orange (MO) under UV light irradiation were investigated. The catalyst prepared bysimple, easy to control and organic-solvent-free impregnation method showed a higherphotocatalytic activity than that prepared by sol-gel and solid state dispersion methods. Inaddition, effect of Si/Al ratios and TiOB2 Bloadings on catalyst, which prepared by impregnation,for photocatalytic activity of degradation of MO were investigated. It was found that, at 15wt% and Si/Al=500, TiO_2/HZSM-5 showed a higher photocatalytic activity. The structure ofthe catalysts were characterized by XRD、UV-vis DRS and BET technologies. It was foundthat TiO_2/HZSM-5 prepared by impregnation had a higher surface area and the nano-TiO_2particles well dispersed on the surface of zeolite leading to a higher photocatalytic activity.
The effect of surfactant template in MCM-41 on the removal of o-CP and o-CNB wasinvestigated. The comparison of adsorption of o-CP and o-CNB on uncalcined MCM-41noted as MCM-41-dry) and calcined MCM-41 (noted as MCM-41-cal) was investigated.MCM-41-dry exhibited significant adsorption capacity for o-CP and o-CNB as compared to MCM-41-cal, which may be because of the hydrophobicity created by surfactant template inMCM-41-dry. In addition, batch adsorption studies were carried out to study the effect ofvarious parameters like adsorbent dose, pH, initial concentration and the presence ofco-existing ions. It was found that adsorption of o-CP and o-CNB depends upon the solutionpH as well as co-existing ions present in the aqueous solution. . From the sorption studies itwas observed that the uptake of o-CP was higher than that of o-CNB. The equilibriumadsorption data for o-CP and o-CNB was analyzed by using Freundlich adsorption isothermmodel.
The photocatalytic activity of TiO_2 supported on MCM-41-dry and MCM-41-cal wasinvestigated using the photooxidation of o-CP as test reactions. The photocatalytic activity ofTiO_2 supported on MCM-41-dry was observed to be higher than that of TiO_2 supported onMCM-41-cal. Moreover, it was found that the photocatalytic activity of TiO_2/MCM-41-dryincreased with the increase in pH value of reactant solution and decrease in initialconcentration of o-CP.
分别以钛氧草酸铵、钛酸丁酯和P25型TiO_2为钛源，相应采用浸渍法、溶胶-凝胶法和固相扩散法制备了三种HZSM-5分子筛负载型纳米TiO_2光催化剂，并在紫外光下对甲基橙（MO，methyl orange）进行了光催化降解性能考察。结果表明，采用方法简单易控制且无需有机溶剂的浸渍法制备的催化剂对MO的去除效果相较用溶胶-凝胶法和固相扩散法制备的样品更好。在此基础上，采用浸渍法制备催化剂，考察了TiO_2负载量和分子筛的Si/Al比对甲基橙降解率的影响。实验表明，TiO_2负载量为15 wt%、HZSM-5分子筛Si/Al=500时，TiO_2/HZSM-5催化剂对降解MO具有更高的催化活性。应用X射线衍射（XRD）、紫外-可见漫反射光谱（UV-vis DRS）和BET比表面积分析等技术对催化剂结构进行表征，结果表明，光催化剂具有较高的比表面积，并且TiO_2在分子筛外表面分散良好，导致其具有高的光催化活性。
以未煅烧含有机模板剂的MCM-41（记作MCM-41-dry）和已煅烧MCM-41（记作MCM-41-cal）为吸附剂对邻氯苯酚（o-CP，To-chlorophenolT）和邻氯硝基苯（o-CNB，To-chloronitrobenzeneT）进行吸附实验。结果表明，相比MCM-41-cal，MCM-41-dry对o-CP和o-CNB有更高的吸附能力，这可能归因于模板剂的存在使MCM-41-dry具有更高的疏水性。此外，还研究了吸附剂的用量、pH值、目标污染的初始浓度和共存离子等因素对MCM-41-dry吸附效果的影响。研究表明，pH值和共存的离子对MCM-41-dry的吸附效果影响较大，MCM-41-dry对o-CP的吸附容量高于o-CNB，MCM-41-dry对o-CP和o-CNB的吸附符合Freundlich吸附平衡模型。
分别以MCM-41-dry和MCM-41-cal为载体制备负载型纳米TiO_2催化剂，并在紫外光下对o-CP进行了光催化降解性能考察。结果表明，含模板剂的TiO_2/MCM-41-dry催化剂对o-CP及其中间产物有更短的降解去除时间。此外，还研究了溶液pH值和o-CP初始浓度对TiO_2/MCM-41-dry光催化降解o-CP的影响。结果表明，在pH值为2~11范围内，pH值越高，光催化完全降解o-CP的时间越短；反应物的初始浓度越高，相同反应条件下，其完全降解o-CP的时间越长。
Nano-TiO_2 has received much attention due to its strong redox ability, chemical stability,non-toxicity, and cheapness. However, the nano-TiO_2 powder is easy to lose in liquid-phasephotocatalytic reaction and difficult to be collected after the reaction, which disturbs therecycle of photocatalyst and hampers the practical applications of nano-TiO_2 powder.Immobilization of nano-TiO_2 overcomes the difficulties in separation and recycles ofphotocatalyst, enhances the concentration of substrates near the TiO_2, as well as restrainsaggregation and deactivation of the catalyst particles. In this work, the research on nano-TiO_2supported on zeolites or porous silica and their hydrophobical modification was reviewed.Therefore, the significance of theory and practice about the study on photocatalyticdegradation of MO over TiO_2/HZSM-5, as well as adsorption and photocatalytic properties ofTiO_2/MCM-41, which includes cationic template within the framework of MCM-41-drymaterials, has been shown in this paper.
TiO_2/HZSM-5 photocatalysts were prepared by impregnation, sol-gel, and solid statedispersion methods, using ammonium titanyl oxalate, tetrabutyl titanate, and P-25 as titaniumsource, respectively. The photocatalytic reactivity of the prepared samples for the degradationof methyl orange (MO) under UV light irradiation were investigated. The catalyst prepared bysimple, easy to control and organic-solvent-free impregnation method showed a higherphotocatalytic activity than that prepared by sol-gel and solid state dispersion methods. Inaddition, effect of Si/Al ratios and TiOB2 Bloadings on catalyst, which prepared by impregnation,for photocatalytic activity of degradation of MO were investigated. It was found that, at 15wt% and Si/Al=500, TiO_2/HZSM-5 showed a higher photocatalytic activity. The structure ofthe catalysts were characterized by XRD、UV-vis DRS and BET technologies. It was foundthat TiO_2/HZSM-5 prepared by impregnation had a higher surface area and the nano-TiO_2particles well dispersed on the surface of zeolite leading to a higher photocatalytic activity.
The effect of surfactant template in MCM-41 on the removal of o-CP and o-CNB wasinvestigated. The comparison of adsorption of o-CP and o-CNB on uncalcined MCM-41noted as MCM-41-dry) and calcined MCM-41 (noted as MCM-41-cal) was investigated.MCM-41-dry exhibited significant adsorption capacity for o-CP and o-CNB as compared to MCM-41-cal, which may be because of the hydrophobicity created by surfactant template inMCM-41-dry. In addition, batch adsorption studies were carried out to study the effect ofvarious parameters like adsorbent dose, pH, initial concentration and the presence ofco-existing ions. It was found that adsorption of o-CP and o-CNB depends upon the solutionpH as well as co-existing ions present in the aqueous solution. . From the sorption studies itwas observed that the uptake of o-CP was higher than that of o-CNB. The equilibriumadsorption data for o-CP and o-CNB was analyzed by using Freundlich adsorption isothermmodel.
The photocatalytic activity of TiO_2 supported on MCM-41-dry and MCM-41-cal wasinvestigated using the photooxidation of o-CP as test reactions. The photocatalytic activity ofTiO_2 supported on MCM-41-dry was observed to be higher than that of TiO_2 supported onMCM-41-cal. Moreover, it was found that the photocatalytic activity of TiO_2/MCM-41-dryincreased with the increase in pH value of reactant solution and decrease in initialconcentration of o-CP.
引文
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