纳米H_3PW_(12)O_(40)/TiO_2复合膜的制备、表征及光催化降解典型有机污染物研究
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摘要
采用溶胶-凝胶法结合程序升温水热技术和旋涂技术，制备纳米杂多酸/二氧化钛（H_3PW_(12)O_(40)/TiO_2）复合膜。通过调节饱和Keggin型磷钨酸H_3PW_(12)O_(40)、四异丙氧基钛（Titanium tetraisopropoxide，TTIP）、溶剂异丙醇及水之间的摩尔比，控制pH值、水热温度及旋涂速度，获得具有优异表面物理化学性质的新型复合材料，利用多种分析测试手段对其进行表征，揭示H_3PW_(12)O_(40)/TiO_2复合膜物化结构与光催化活性之间的关系。在模拟太阳光（波长范围为320nm-780nm）照射下，以典型有机污染物（染料罗丹明B、环境激素双酚A、抗生素磺胺甲噁唑等）作为目标化合物，对所制备的纳米H_3PW_(12)O_(40)/TiO_2复合膜光催化活性、影响因素、光催化氧化机理、回收利用性能及有机污染物光催化反应动力学、降解机理和矿化程度进行了研究。
具体结果如下：
1.通过电感耦合等离子体-原子发射光谱（ICP-AES）、能谱分析（EDS）、傅里叶红外光谱（FTIR）、拉曼光谱（Ramman）、X射线粉末衍射（XRD）、紫外-可见漫反射（UV-VisDRS）、氮气吸附-脱附（Nitrogen adsorption-desorption）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）多种分析测试手段，对纳米H_3PW_(12)O_(40)/TiO_2复合膜的组成、晶体结构、光吸收特性、孔结构特征、表面形貌等进行表征。结果表明，所制备的纳米H_3PW_(12)O_(40)/TiO_2复合膜具有如下特点：H_3PW_(12)O_(40)成功掺杂到TiO_2中，其Keggin结构保持完整，掺杂量在3.2-16.7%之间；复合膜中TiO_2均为锐钛矿晶型，晶粒尺寸的范围为8.48-12.32nm；复合膜中均匀分散着球形的纳米H_3PW_(12)O_(40)/TiO_2复合颗粒，无明显团聚现象；催化剂比表面积的范围为137.8-171.6m~2/g，具有三维交联海绵状结构；与纯TiO_2相比，复合膜催化剂吸收波长发生红移，对太阳光的利用率增强。
2.通过纳米H_3PW_(12)O_(40)/TiO_2复合膜对罗丹明B（RhB）、双酚A（BPA）和磺胺甲噁唑（SMZ）光催化降解的研究，考察H_3PW_(12)O_(40)掺杂量、反应液初始浓度（C0）、溶液pH值等因素对光催化活性的影响，得出光催化降解的最佳条件。其中，RhB的最佳降解条件为：H_3PW_(12)O_(40)掺杂量为14.7%，C0为25mg/L，溶液pH为4.4；BPA的最佳降解条件为：H_3PW_(12)O_(40)掺杂量为6.3%，C0为5mg/L，溶液pH为8.2；SMZ的最佳降解条件为：H_3PW_(12)O_(40)掺杂量为7.7%，C0为50mg/L，溶液pH为5.5。其光催化反应均符合一级Langmuir-Hinshelwood动力学方程。上述条件下，RhB、BPA和SMZ的反应速率常数分别为0.018、0.023和0.008min-1，光照240min后，光催化降解效率分别为98.5%、100.0%和87.0%。
3.以BPA作为目标污染物，通过自由基捕获实验研究了H_3PW_(12)O_(40)/TiO_2复合膜的光催化氧化机理。研究表明，H_3PW_(12)O_(40)和TiO_2之间能够产生协同作用，H_3PW_(12)O_(40)接受TiO_2表面的光生电子，使电子-空穴对得到有效分离，带有电子的H_3PW_(12)O_(40)负离子和空穴都可以进一步同水反应生成活性羟基（·OH）自由基，·OH自由基具有高度的氧化性，能够将有机污染物氧化降解。
4.通过对BPA光催化降解中间产物的鉴定，推测其降解途径为：BPA分子中的苯环最先受到·OH自由基的进攻，两个苯环基团发生断裂，产生对羟基苯丙醇、苯酚和对羟基苯甲醛，在·OH作用下进一步转化为对苯二酚和对羟基苯甲酸，最终开环生成甲酸、乙酸、二氧化碳和水等小分子化合物。
5.通过总有机碳（TOC）分析，分别考察了纳米H_3PW_(12)O_(40)/TiO_2复合膜对RhB、BPA和SMZ三种有机污染物的矿化作用。结果表明：在模拟太阳光条件下，光照12h后，其矿化程度分别为77.7%、76.7%和66.6%，均高于纯TiO_2膜（分别为63.3%、69.9%和53.2%）。
6.通过纳米H_3PW_(12)O_(40)/TiO_2复合膜对RhB和BPA的多次光催化降解，分别考察了复合膜的循环利用性能。结果表明：14.7-H_3PW_(12)O_(40)/TiO_2复合膜对RhB三次循环使用后的光催化降解率仍然保持在95%以上；6.3-H_3PW_(12)O_(40)/TiO_2复合膜对BPA三次循环使用后的光催化降解效率为96.2%，十次循环后，BPA光催化降解效率仍可达到70%以上。
Nanometer H_3PW_(12)O_(40)/TiO_2composite films were prepared by the sol-gel combinedtemperature programmed hydrothemal method and spin coating technique. The novelcomposite films had abtained excellent physical and chemical properties through adjusting themolar ratio of saturation Keggin-type H_3PW_(12)O_(40), titanium tetraisopropoxide, isopropylalcohol and water. The surface morphology of the as-prepared composite films wascharacterized by various analysis tests to reveal the quantity-effect relation between materialstructure and photocatalytic activity. Under simulated sunlight (wavelength extent:320nm-780nm) irradiation, the photocatalytic activities of the composite films were studied viathe degradation of many typical organic compounds (dyes, endocrine disrupters and antibioticdrugs). The various influences on degradation were investigated systematically, includingH_3PW_(12)O_(40)loadings, initial concentration and solution pH and so on. Photocatalytic oxidationmechanism and recycling performance of composite film, corresponding dynamic models,degradation pathway and mineralization degree of organic pollutant were also discussed indepth.
The main results was concluded as follows:
1.Composition, crystal structure, optical absorption, pore structure characteristic, surfacemorphology of the as-prepared composite film was characterized by various analysis tests,including ICP-AES, EDS, FTIR, Ramman, XRD, UV-Vis DRS, Nitrogenadsorption-desorption, SEM and TEM. The results indicated that H_3PW_(12)O_(40)could dopedprimely in TiO_2lattice structure and the Keggin-type unit retained intact in H_3PW_(12)O_(40)/TiO_2composite films, the doping amount was from3.2%to16.7%; TiO_2showed pure anatasecrystal in all as-prepared composite films, grain diameter was8.48-12.32nm; The sphericalcatalysts particles well-dispersed in H_3PW_(12)O_(40)/TiO_2composite films could not be foundobvious agglomeration phenomenon, specific surface area of the catalyst was137.8-171.6m2/g, the interior possessed microporous structure and the catalyst particles stacked eachother to form mesoporous and spongeous structure; The absorption wavelength of compositefilm happened redshift and enhanced the utiization ratio of the sunlight after dopingH_3PW_(12)O_(40).
2. Through the study and observation on photocatalytic activities of H_3PW_(12)O_(40)/TiO_2composite films and influencing factors for the degradation of RhB, BPA and SMZ, theoptimum reaction condition is comfirmed. The optimum condition of RhB: the H_3PW_(12)O_(40) loading is14.7%, initial concentration is25mg/L, solution pH is4.4; The optimum conditionof BPA: the H_3PW_(12)O_(40)loading is6.3%, initial concentration is5mg/L, solution pH is8.2;the optimum condition of SMZ: the H_3PW_(12)O_(40)loading is7.7%, initial concentration is50mg/L, solution pH is5.5. All photocatalytic reactions followed apparent first orderLangmuir-Hinshelwood kinetic model, the reaction rate constant of RhB, BPA and SMZrespectively is0.018,0.023and0.008min-1under the optimum condition; after240minirradiation, the efficiency of photocatalytic degradation is98.5%,100.0%and87.0%,respectively.
3. BPA as target pollutant, photocatalytic oxidation mechanism of composite film wasstudied through free radicals capture experiment. The result indicated that synergistic actionbetween H_3PW_(12)O_(40)and TiO_2inhibited effectively the recombination of e--h+pairs,H_3PW_(12)O_(40)possessed strong electron-accept capacity, and prompted h+reacting with H2Oadequately to generate more active hydroxyl radicals. Hydroxy free radicals are highlyoxidizing and no selectivtiy group can have degradation organic pollutants effectively.
4. The degradation pathway of BPA was presumed according to intermediate productsduring degradation process identified. It was that hydroxy radical attacked benzene rings ofBPA molecules at first, two groups of benzene happened breakage to produce p-hydroxybenzene propanol, phenol and p-hydroxybenzaldehyde, then further oxidized translated intohydroquinone and p-hydroxybenzoic acid, and finally opened aromatic ring to form formic,acetic acids, CO2and H2O.
5. Mineralization ability to H_3PW_(12)O_(40)/TiO_2composite films for RhB, BPA and SMZwas observed through TOC analysis. After simulated sunlight irradiation for12h,mineralization degree respectively was77.7%,76.7%and66.6%, higher than TiO_2film(63.3%,69.9%and53.2%).
6. Recycle and reuse of the H_3PW_(12)O_(40)/TiO_2composite films was studied throughdegradation RhB and BPA. The research found that above95.0%of RhB and BPA could stillbeen degraded after three times cycle by the composite film, and BPA photocatalyticdegradation efficiency still can achieve70%above after ten times cycle.
具体结果如下：
1.通过电感耦合等离子体-原子发射光谱（ICP-AES）、能谱分析（EDS）、傅里叶红外光谱（FTIR）、拉曼光谱（Ramman）、X射线粉末衍射（XRD）、紫外-可见漫反射（UV-VisDRS）、氮气吸附-脱附（Nitrogen adsorption-desorption）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）多种分析测试手段，对纳米H_3PW_(12)O_(40)/TiO_2复合膜的组成、晶体结构、光吸收特性、孔结构特征、表面形貌等进行表征。结果表明，所制备的纳米H_3PW_(12)O_(40)/TiO_2复合膜具有如下特点：H_3PW_(12)O_(40)成功掺杂到TiO_2中，其Keggin结构保持完整，掺杂量在3.2-16.7%之间；复合膜中TiO_2均为锐钛矿晶型，晶粒尺寸的范围为8.48-12.32nm；复合膜中均匀分散着球形的纳米H_3PW_(12)O_(40)/TiO_2复合颗粒，无明显团聚现象；催化剂比表面积的范围为137.8-171.6m~2/g，具有三维交联海绵状结构；与纯TiO_2相比，复合膜催化剂吸收波长发生红移，对太阳光的利用率增强。
2.通过纳米H_3PW_(12)O_(40)/TiO_2复合膜对罗丹明B（RhB）、双酚A（BPA）和磺胺甲噁唑（SMZ）光催化降解的研究，考察H_3PW_(12)O_(40)掺杂量、反应液初始浓度（C0）、溶液pH值等因素对光催化活性的影响，得出光催化降解的最佳条件。其中，RhB的最佳降解条件为：H_3PW_(12)O_(40)掺杂量为14.7%，C0为25mg/L，溶液pH为4.4；BPA的最佳降解条件为：H_3PW_(12)O_(40)掺杂量为6.3%，C0为5mg/L，溶液pH为8.2；SMZ的最佳降解条件为：H_3PW_(12)O_(40)掺杂量为7.7%，C0为50mg/L，溶液pH为5.5。其光催化反应均符合一级Langmuir-Hinshelwood动力学方程。上述条件下，RhB、BPA和SMZ的反应速率常数分别为0.018、0.023和0.008min-1，光照240min后，光催化降解效率分别为98.5%、100.0%和87.0%。
3.以BPA作为目标污染物，通过自由基捕获实验研究了H_3PW_(12)O_(40)/TiO_2复合膜的光催化氧化机理。研究表明，H_3PW_(12)O_(40)和TiO_2之间能够产生协同作用，H_3PW_(12)O_(40)接受TiO_2表面的光生电子，使电子-空穴对得到有效分离，带有电子的H_3PW_(12)O_(40)负离子和空穴都可以进一步同水反应生成活性羟基（·OH）自由基，·OH自由基具有高度的氧化性，能够将有机污染物氧化降解。
4.通过对BPA光催化降解中间产物的鉴定，推测其降解途径为：BPA分子中的苯环最先受到·OH自由基的进攻，两个苯环基团发生断裂，产生对羟基苯丙醇、苯酚和对羟基苯甲醛，在·OH作用下进一步转化为对苯二酚和对羟基苯甲酸，最终开环生成甲酸、乙酸、二氧化碳和水等小分子化合物。
5.通过总有机碳（TOC）分析，分别考察了纳米H_3PW_(12)O_(40)/TiO_2复合膜对RhB、BPA和SMZ三种有机污染物的矿化作用。结果表明：在模拟太阳光条件下，光照12h后，其矿化程度分别为77.7%、76.7%和66.6%，均高于纯TiO_2膜（分别为63.3%、69.9%和53.2%）。
6.通过纳米H_3PW_(12)O_(40)/TiO_2复合膜对RhB和BPA的多次光催化降解，分别考察了复合膜的循环利用性能。结果表明：14.7-H_3PW_(12)O_(40)/TiO_2复合膜对RhB三次循环使用后的光催化降解率仍然保持在95%以上；6.3-H_3PW_(12)O_(40)/TiO_2复合膜对BPA三次循环使用后的光催化降解效率为96.2%，十次循环后，BPA光催化降解效率仍可达到70%以上。
Nanometer H_3PW_(12)O_(40)/TiO_2composite films were prepared by the sol-gel combinedtemperature programmed hydrothemal method and spin coating technique. The novelcomposite films had abtained excellent physical and chemical properties through adjusting themolar ratio of saturation Keggin-type H_3PW_(12)O_(40), titanium tetraisopropoxide, isopropylalcohol and water. The surface morphology of the as-prepared composite films wascharacterized by various analysis tests to reveal the quantity-effect relation between materialstructure and photocatalytic activity. Under simulated sunlight (wavelength extent:320nm-780nm) irradiation, the photocatalytic activities of the composite films were studied viathe degradation of many typical organic compounds (dyes, endocrine disrupters and antibioticdrugs). The various influences on degradation were investigated systematically, includingH_3PW_(12)O_(40)loadings, initial concentration and solution pH and so on. Photocatalytic oxidationmechanism and recycling performance of composite film, corresponding dynamic models,degradation pathway and mineralization degree of organic pollutant were also discussed indepth.
The main results was concluded as follows:
1.Composition, crystal structure, optical absorption, pore structure characteristic, surfacemorphology of the as-prepared composite film was characterized by various analysis tests,including ICP-AES, EDS, FTIR, Ramman, XRD, UV-Vis DRS, Nitrogenadsorption-desorption, SEM and TEM. The results indicated that H_3PW_(12)O_(40)could dopedprimely in TiO_2lattice structure and the Keggin-type unit retained intact in H_3PW_(12)O_(40)/TiO_2composite films, the doping amount was from3.2%to16.7%; TiO_2showed pure anatasecrystal in all as-prepared composite films, grain diameter was8.48-12.32nm; The sphericalcatalysts particles well-dispersed in H_3PW_(12)O_(40)/TiO_2composite films could not be foundobvious agglomeration phenomenon, specific surface area of the catalyst was137.8-171.6m2/g, the interior possessed microporous structure and the catalyst particles stacked eachother to form mesoporous and spongeous structure; The absorption wavelength of compositefilm happened redshift and enhanced the utiization ratio of the sunlight after dopingH_3PW_(12)O_(40).
2. Through the study and observation on photocatalytic activities of H_3PW_(12)O_(40)/TiO_2composite films and influencing factors for the degradation of RhB, BPA and SMZ, theoptimum reaction condition is comfirmed. The optimum condition of RhB: the H_3PW_(12)O_(40) loading is14.7%, initial concentration is25mg/L, solution pH is4.4; The optimum conditionof BPA: the H_3PW_(12)O_(40)loading is6.3%, initial concentration is5mg/L, solution pH is8.2;the optimum condition of SMZ: the H_3PW_(12)O_(40)loading is7.7%, initial concentration is50mg/L, solution pH is5.5. All photocatalytic reactions followed apparent first orderLangmuir-Hinshelwood kinetic model, the reaction rate constant of RhB, BPA and SMZrespectively is0.018,0.023and0.008min-1under the optimum condition; after240minirradiation, the efficiency of photocatalytic degradation is98.5%,100.0%and87.0%,respectively.
3. BPA as target pollutant, photocatalytic oxidation mechanism of composite film wasstudied through free radicals capture experiment. The result indicated that synergistic actionbetween H_3PW_(12)O_(40)and TiO_2inhibited effectively the recombination of e--h+pairs,H_3PW_(12)O_(40)possessed strong electron-accept capacity, and prompted h+reacting with H2Oadequately to generate more active hydroxyl radicals. Hydroxy free radicals are highlyoxidizing and no selectivtiy group can have degradation organic pollutants effectively.
4. The degradation pathway of BPA was presumed according to intermediate productsduring degradation process identified. It was that hydroxy radical attacked benzene rings ofBPA molecules at first, two groups of benzene happened breakage to produce p-hydroxybenzene propanol, phenol and p-hydroxybenzaldehyde, then further oxidized translated intohydroquinone and p-hydroxybenzoic acid, and finally opened aromatic ring to form formic,acetic acids, CO2and H2O.
5. Mineralization ability to H_3PW_(12)O_(40)/TiO_2composite films for RhB, BPA and SMZwas observed through TOC analysis. After simulated sunlight irradiation for12h,mineralization degree respectively was77.7%,76.7%and66.6%, higher than TiO_2film(63.3%,69.9%and53.2%).
6. Recycle and reuse of the H_3PW_(12)O_(40)/TiO_2composite films was studied throughdegradation RhB and BPA. The research found that above95.0%of RhB and BPA could stillbeen degraded after three times cycle by the composite film, and BPA photocatalyticdegradation efficiency still can achieve70%above after ten times cycle.
引文
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