3DOM LaMnO_3，Au/3DOM La_(0.6)Sr_(0.4)MnO_3，Au/meso Co_3O_4和3DOM BiVO_4催化剂可控制备及有机污染物氧化的催化性能研究
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摘要
多孔过渡金属氧化物具有高的比表面积和发达的孔结构使其在电、磁、吸附和催化等物理和化学领域具有很大的应用前景。多孔材料中的介孔可以选择性地容纳客体分子，所具有的高比表面积有利于气体分子吸附。大孔结构则可降低大分子传质阻力和有利于其到达活性位。此外，大孔或介孔载体也有利于活性组分在其表面的分散。众所周知，钙钛矿型氧化物（ABO_3）对挥发性有机物和CO氧化反应显示出优良的催化性能，这与ABO_3的非化学计量氧量、比表面积和氧化还原能力等因素有关。单斜白钨矿晶相的BiVO_4是一种对可见光响应的半导体光催化剂，在可见光照射下显示光催化活性。近年来，金催化成为研究的热点课题之一。金的催化作用与所用载体的性质有关。一般选用惰性载体来负载金属活性组分，金属与载体之间的强相互作用能够影响催化剂的物化性质。以具有氧化还原能力的过渡金属氧化物或复合氧化物作为载体的研究工作很少有文献报道。将纳米金负载到具有高比表面积的过渡金属氧化物或复合氧化物上，可以提高金的负载量和纳米金的分散度，有效地避免反应过程中可能引起的烧结现象。针对如何改善单一和复合金属氧化物的物化性质进而达到提高其催化性能的目的，本文研究了具有介孔孔壁的三维有序大孔（3DOM）LaMnO_3、Au/3DOMLa_(0.6)Sr_(0.4)MnO_3、Au/链条状大孔结构的LaMnO_3、MnO_x/3DOM LaMnO_3、空心球状LaMO_3（M=Mn, Co）、实心球状MOx（M=Mn, Co）、有序介孔Co_3O_4、Au/有序介孔Co_3O_4和3DOM BiVO_4的PMMA或KIT-6硬模板可控制备法，利用多种技术表征其物化性质，揭示了催化作用机制，评价了其对挥发性有机物（苯、甲苯、二甲苯或甲醇）和CO氧化反应的催化性能，以此建立催化剂的物化性质与反应之间的构效关系。主要研究内容和取得的研究结果如下：
（1）采用表面活性剂辅助的PMMA硬模板法制备了空心球状菱方相LaMO_3（M=Mn, Co）和实心球状立方相MO_x（M=Mn, Co）。结果表明，聚乙二醇和乙二醇的联用有利于形成具有球状复合金属氧化物和过渡金属氧化物。球状催化剂比其纳米粒子催化剂具有更高的比表面积（21-33m~2/g）和表面吸附氧浓度以及更好的低温还原性。对于CO和甲苯氧化反应，球形催化剂的活性优于相应的纳米粒子催化剂的，其中Co_3O_4实心球催化剂对CO氧化反应的活性最好[当空速（SV）为10000mL/(g h)时，其T_(90%)（转化率达90%时的反应温度）为109℃]，而LaCoO_3空心球催化剂对甲苯氧化的活性最好（当空速为20000mL/(g h)时，其T_(90%)为237℃）。
（2）采用表面活性剂辅助的PMMA硬模板法制备了具有介孔孔壁的菱方3DOMLaMnO_3催化剂。结果表明，表面活性剂P123和L-赖氨酸对于形成大孔孔壁上的介孔结构具有重要作用，双模孔结构的催化剂具有较高的比表面积（3239m~2/g）、较高的表面氧浓度和较好的低温还原性。在甲苯浓度为1000ppm、甲苯/O_2摩尔比为1/400和SV为20000mL/(g h)的反应条件下，具有大孔-介孔双模孔结构的LaMnO_3-PP-2或LaMnO_3-PL-2催化剂显示出最高的活性，其T50%为222226℃和T_(90%)为243249℃。与体相LaMnO_3催化剂的表观活化能（97kJ/mol）相比，多孔催化剂具有明显低的表观活化能（5762kJ/mol）。
（3）采用色氨酸辅助的PMMA硬模板法原位制备了yMnO_x/3DOM LaMnO_3（y=5,8,12,16wt%）催化剂，建立了一步法制备菱方相3DOM LaMnO_3负载的MnO_x纳米粒子催化剂的可控合成工艺。结果表明，yMnO_x/3DOM LaMnO_3催化剂的比表面积为1931m~2/g，MnO_x纳米颗粒（粒径为435nm）高度分散在3DOM LaMnO_3表面。与通过等体积浸渍法获得的12wt%MnO_x/体相LaMnO_3催化剂相比，yMnO_x/3DOM LaMnO_3催化剂具有更高的表面吸附氧浓度和比表面积以及较均匀的MnO_x纳米粒子（粒径为418nm）。在VOC（甲苯或甲醇）浓度为1000ppm、VOC/O_2摩尔比为1/400和SV为20000mL/(g h)的反应条件下，12wt%MnO_x/3DOM LaMnO_3催化剂的活性最佳，其对甲苯和甲醇氧化反应的T_(90%)分别为215℃和137℃。
（4）采用表面活性剂辅助的PMMA硬模板法制备了链条状大孔结构的菱方相LaMnO_3和菱方相3DOM La_(0.6)Sr_(0.4)_3催化剂，再利用聚乙烯醇保护的鼓泡还原法制备出了xAu/链条状大孔LaMnO_3（x=1.4,3.1,4.9wt%）和xAu/3DOM La_(0.6)Sr_(0.4)_3（x=3.4,6.4,7.9wt%）催化剂。结果表明，金纳米粒子尺寸在25nm范围内，均匀地分布在催化剂的孔道表面上。xAu/链条状大孔LaMnO_3和xAu/3DOM La_(0.6)Sr_(0.4)_3催化剂的比表面积分别为3033m~2/g和3133m~2/g。4.9wt%Au/链条状大孔LaMnO_3和6.4wt%Au/3DOM La_(0.6)Sr_(0.4)_3催化剂上的表面氧物种浓度较高和低温还原性较好，其催化活性也较高。4.9wt%Au/链条状大孔LaMnO_3和6.4wt%Au/3DOM La_(0.6)Sr_(0.4)_3催化剂对CO氧化反应的T_(90%)分别为91℃（当SV为20000mL/(g h)时）和3℃（当SV为10000mL/(g h)时），对甲苯氧化反应的T_(90%)分别为226℃和170℃（当SV为20000mL/(g h)时）。多孔链条状大孔LaMnO_3负载金催化剂对CO和甲苯氧化反应的表观活化能分别为2937kJ/mol和4752kJ/mol，低于在体相LaMnO_3催化剂上的（分别为63kJ/mol和97kJ/mol）；多孔3DOM La_(0.6)Sr_(0.4)_3负载金催化剂对CO和甲苯氧化反应的表观活化能分别为3132kJ/mol和4448kJ/mol，低于在体相La_(0.6)Sr_(0.4)_3催化剂上的（分别为57kJ/mol和74kJ/mol）。
（5）以KIT-6为硬模板通过纳米浇铸法制备了有序介孔立方晶相Co_3O_4（meso-Co_3O_4），并利用聚乙烯醇保护的还原法制得了xAu/meso-Co_3O_4（x=3.7,6.5,9.0wt%）催化剂。meso-Co_3O_4和xAu/meso-Co_3O_4催化剂的比表面积高达9194m~2/g。6.5wt%Au/meso-Co_3O_4催化剂显示出较高的表面氧浓度、较好的低温还原性和较强的Au与meso-Co_3O_4之间的相互作用，因而显示出较好的催化活性和稳定性。在CO浓度为1vol%和SV为60000mL/(g h)或VOC（苯、甲苯或二甲苯）浓度为1000ppm和SV为20000mL/(gh)的反应条件下，6.5wt%Au/meso-Co_3O_4催化剂对CO、苯、甲苯和二甲苯氧化反应的T_(90%)分别为45℃、189℃、138℃和162℃。
（6）采用抗坏血酸或柠檬酸辅助的PMMA硬模板法制备了单斜相3DOM BiVO_4光催化剂。3DOM BiVO_4光催化剂具有高的比表面积（1824m~2/g）。在所有光催化剂中，比表面积为24m~2/g的BiVO_4-AA-1光催化剂显示出最好的光催化性能。在苯酚初始浓度为0.1mmol/L和H_2O_2添加量为0.6mL条件下反应3小时后，苯酚转化率可达到94%。较低的苯酚初始浓度和适中的H_2O_2用量有助于改善催化剂的光催化性能。
（7）在所制得的每个系列催化剂中，Co_3O_4实心球、LaCoO_3空心球、具有大孔介孔双模孔结构的LaMnO_3-PP-2和LaMnO_3-PL-2、12wt%MnO_x/3DOMLaMnO_3、4.9wt%Au/链条状大孔LaMnO_3、6.4wt%Au/3DOMLa_(0.6)Sr_(0.4)_3、6.5wt%Au/meso-Co_3O_4和BiVO_4-AA-1催化剂对CO、VOC（苯、甲苯、二甲苯或甲醇）或苯酚氧化反应显示出最好的催化活性。基于表征结果和活性数据，我们认为这些催化剂优良的催化性能与其较高的比表面积、较高的吸附氧物种浓度、较好的低温还原性、金与载体之间的强相互作用、良好的多孔结构或较高氧缺陷密度相关。
Due to the high surface areas, large pore volumes, and high-quality pore structures,porous transition-metal oxides have been widely applied in physics and chemistry,such as electronics, magnetics, adsorption, and catalysis. The mesopores in porousmaterials can accommodate guest molecules selectively and the high surface areas ofmesoporous materials are beneficial for the adsorption of gaseous molecules. Theexistence of a macroporous structure can reduce the transfer resistance of guestmolecules and facilitate them to approach the active sites. In addition, macro-ormesoporous supports can also favor the dispersion of active components on theirsurface. It is well known that perovskite-type oxides (ABO_3) exhibit goodperformance in catalyzing the complete oxidation of volatile organic compounds(VOCs) and carbon monoxide, which is associated with the oxygen nonstoichometricamount, surface area, and redox ability. The monoclinic scheelite-type BiVO_4as avisible-light-responsive semiconductor photocatalyst is active photocatalyticallyunder visible-light illumination. In recent years, catalysis by gold has been one of thehot research topics. Catalysis over a supported gold material is related to the nature ofthe support. Usually, an inert support was used to load gold, and the metal-supportstrong interaction can influence the physicochemical properties of the supported metalcatalysts. The studies on the employment of reducible transition-metal oxides ormixed oxides as the support have been rarely reported. The loading of nano-sized goldon the surface of transition-metal oxides or mixed oxides with high surface areas isexpected to increase the loading and gold dispersion, thus effectively avoiding thepossible sintering phenomena during the reaction processes. In ordered to improve thephysicochemical properties of single transition-metal oxides or mixed oxides andhence to enhance their catalytic performance, we have in the present dissertation madeinvestigations on the controlled preparation of three-dimensionally ordered (3DOM)LaMnO_3,3DOM La_(0.6)Sr_(0.4)_3, chain-like macroporous LaMnO_3, and MnO_x/3DOMLaMnO_3with mesoporous skeletons, hollow spherical LaMO_3(M=Mn, Co), solidspherical MOx(M=Mn, Co),3D ordered mesoporous Co_3O_4, Au/3D orderedmesoporous Co_3O_4, and3DOM BiVO_4via the poly(methyl methacrylate)(PMMA) or3D ordered mesoporous silica (KIT-6) hard-templating routes. The physicochemicalproperties of these materials were characterized by means of a number of analyticaltechniques and the catalytic mechanisms were clarified. The catalytic activities of theas-prepared catalysts were evaluated for the oxidation of VOCs (benzene, toluene,xylene or methanol) and CO, so that the relationships between physicochemicalproperties and catalytic performance of the materials could be established. The maininvestigations and obtained results are as follows:
1. The hollow spherical rhombohedral LaMO_3(M=Mn and Co) and solid spherical cubic MOx(M=Mn and Co) nanoparticles were prepared using thesurfactant-assisted PMMA-templating strategy. It is shown that the use ofpolyethylene glycol (PEG) and ethylene glycol (EG) was favorable for theformation of hollow and solid spherical mixed oxides and transition-metal oxides.Compared to their nano-sized counterparts, the spherical LaMO_3and MOxcatalysts possessed much higher surface areas (2133m~2/g), higher adsorbedoxygen species concentrations, and better low-temperature reducibility. For theoxidation of CO and toluene, the catalytic activities of the spherical catalystswere higher than those of the nano-sized catalysts, in which the solid sphericalCo3O4catalyst performed the best for CO oxidation (the T_(90%)(the temperaturerequired for achieving90%CO conversion)=109℃at a space velocity (SV)=10,000mL/(g h)), whereas the hollow spherical LaCoO_3catalyst showed thehighest catalytic activity for toluene oxidation (To90%=237C at SV=20,000mL/(g h)).
2. The rhombohedral3DOM LaMnO_3catalysts with mesoporous skeletons wereprepared via the surfactant-assisted PMMA-templating route. P123or L-lysinemight play a critical role in the generation of mesopores on the macropore wallsof3DOM LaMnO_3. The LaMnO_3catalysts with dual pore structures showedhigher surface areas (3239m~2/g), higher surface oxygen species concentrations,and better low-temperature reducibility. Under the conditions of tolueneconcentration=1,000ppm, toluene/O_2molar ratio=1/400, and SV=20,000mL/(g h), the porous LaMnO_3samples were superior to the bulk counterpart incatalytic performance, with the LaMnO_3-PP-2and LaMnO_3-PL-2samples withmacro-and mesoporous structures performing the best (T50%=222226℃andT_(90%)=243249℃). The apparent activation energies (5762kJ/mol) over theporous catalysts were much lower than that (97kJ/mol) over the bulk counterpart.
3.3DOM-structured rhombohedral LaMnO_3and its supported MnO_xcatalysts(yMnO_x/3DOM LaMnO_3; y=5,8,12, and16wt%) were prepared using anin-situ tryptophan-assisted PMMA-templating strategy, and an one-pot methodfor the controlled preparation of rhombohedral LaMnO_3-supported MnO_xnano-sized catalysts has been established. It is shown that the surface areas ofyMnO_x/3DOM LaMnO_3were1931m~2/g, and the MnO_xnanoparticles (diameter=435nm) were highly dispersed on the surface of3DOM LaMnO_3. Comparedto the12wt%Au/bulk LaMnO_3catalyst derived from the incipient wetnessimpregnation process, the yMnO_x/3DOM LaMnO_3catalysts possessed highersurface areas and adsorbed oxygen species concentrations, low-temperaturereducibility, and more uniform MnO_xnanoparticles (diameter=418nm). Underthe conditions of toluene or methanol concentration=1000ppm, toluene or methanol/O_2molar ratio=1/400, and SV=20,000mL/(g h), the12wt%MnO_x/3DOM LaMnO_3catalyst performed the best (T_(90%)=215and137℃for theoxidation of toluene and methanol, respectively).
4. Chain-like macroporous rhombohedral LaMnO_3and rhombohedral3DOMLa_(0.6)Sr_(0.4)MnO_3and their supported gold (xAu/chain-like macroporous LaMnO_3(x=1.4,3.1, and4.9wt%) and xAu/3DOM La_(0.6)Sr_(0.4)MnO_3(x=3.4,6.4, and7.9wt%)) catalysts were prepared using the surfactant-assisted PMMA-templatingand gas bubble-assisted polyvinyl alcohol-protected reduction methods,respectively. It is shown that the sizes of gold particles were in the range of25nm, and the gold nanoparticles were uniformly distributed on the pore surface ofthe catalysts. xAu/chain-like macroporous LaMnO_3and xAu/3DOMLa_(0.6)Sr_(0.4)MnO_3catalysts possessed surface areas of3033and3133m~2/g,respectively. The4.9wt%Au/chain-like macroporous LaMnO_3and6.4wt%Au/3DOM La_(0.6)Sr_(0.4)MnO_3catalysts showed higher surface oxygen speciesconcentrations and better low-temperature reducibility, and hence higher catalyticperformance. The T_(90%)values obtained over the4.9wt%Au/chain-likemacroporous LaMnO_3and6.4wt%Au/3DOM La_(0.6)Sr_(0.4)MnO_3catalysts were91℃at SV=20,000mL/(g h) and3℃at SV=10,000mL/(g h) for CO oxidation,and226and170℃at SV=20,000mL/(g h) for toluene oxidation, respectively.The apparent activation energies of xAu/chain-like macroporous LaMnO_3catalysts for CO and toluene oxidation were respectively2937and4752kJ/mol, much lower than those (63and97kJ/mol, respectively) of the bulkLaMnO_3catalyst; the apparent activation energies of xAu/3DOM La_(0.6)Sr_(0.4)MnO_3catalysts for CO and toluene oxidation were respectively3132and4448kJ/mol, much lower than that (57and74kJ/mol, respectively) of the bulkLa_(0.6)Sr_(0.4)MnO_3catalyst.
5.3D ordered mesoporous cubic Co3O4(meso-Co3O4) and its supported Au(xAu/meso-Co3O4; x=3.7,6.5, and9.0wt%) nanocatalysts were prepared usingthe KIT-6nanocasting and PVA-protected reduction methods, respectively. Thesurface areas of xAu/meso-Co3O4were in the range of9194m~2/g. The6.5wt%Au/meso-Co3O4catalyst exhibited higher surface oxygen species concentration,better low-temperature reducibility, and stronger Au meso-Co3O4interaction, andhence better catalytic activity and stability. Under the conditions of COconcentration=1vol%and SV=60,000mL/(g h) or VOC (benzene, toluene orxylene) concentration=1000ppm and SV=20,000mL/(g h), the T_(90%)valuesover the6.5wt%Au/meso-Co3O4catalyst were45,189,138, and162℃for theoxidation of CO, benzene, toluene, and xylene, respectively.
6. Monoclinically crystallized3DOM-structured BiVO4photocatalysts with high surface areas (1824m~2/g) were prepared by using the ascorbic acid-or citricacid-assisted PMMA-templating strategy. Among the as-prepared BiVO_4photocatalysts, the one with a surface area of ca.24m~2/g showed the bestvisible-light-driven photocatalytic performance for phenol degradation (phenolconversion=ca.94%at phenol concentration=0.1mmol/L and in the presenceof0.6mL H_2O_2). The lower phenol concentration in aqueous solution and theaddition of an appropriate H_2O_2amount were beneficial for the enhancement inphotocatalytic performance.
7. Among each series of the as-prepared catalysts, solid spherical Co_3O_4, hollowspherical LaCoO_3, LaMnO_3-PP-2and LaMnO_3-PL-2with macro-andmesoporous structures,12wt%MnOx/3DOM LaMnO_3,4.9wt%Au/chain-likemacroporous LaMnO_3,6.4wt%Au/3DOM La0.6Sr0.4MnO_3,6.5wt%Au/meso-Co_3O_4, and BiVO_4-AA-1catalysts showed the highest performance forthe oxidation of CO, VOC (benzene, toluene, xylene or methanol) or phenol.Based on the characterization results and catalytic activity data, it is concludedthat the excellent catalytic performance of these materials might be associatedwith their higher surface areas, higher adsorbed oxygen species concentrations,better low-temperature reducibility, strong gold-support interaction, better qualityporous structures or higher oxygen deficiency density.
（1）采用表面活性剂辅助的PMMA硬模板法制备了空心球状菱方相LaMO_3（M=Mn, Co）和实心球状立方相MO_x（M=Mn, Co）。结果表明，聚乙二醇和乙二醇的联用有利于形成具有球状复合金属氧化物和过渡金属氧化物。球状催化剂比其纳米粒子催化剂具有更高的比表面积（21-33m~2/g）和表面吸附氧浓度以及更好的低温还原性。对于CO和甲苯氧化反应，球形催化剂的活性优于相应的纳米粒子催化剂的，其中Co_3O_4实心球催化剂对CO氧化反应的活性最好[当空速（SV）为10000mL/(g h)时，其T_(90%)（转化率达90%时的反应温度）为109℃]，而LaCoO_3空心球催化剂对甲苯氧化的活性最好（当空速为20000mL/(g h)时，其T_(90%)为237℃）。
（2）采用表面活性剂辅助的PMMA硬模板法制备了具有介孔孔壁的菱方3DOMLaMnO_3催化剂。结果表明，表面活性剂P123和L-赖氨酸对于形成大孔孔壁上的介孔结构具有重要作用，双模孔结构的催化剂具有较高的比表面积（3239m~2/g）、较高的表面氧浓度和较好的低温还原性。在甲苯浓度为1000ppm、甲苯/O_2摩尔比为1/400和SV为20000mL/(g h)的反应条件下，具有大孔-介孔双模孔结构的LaMnO_3-PP-2或LaMnO_3-PL-2催化剂显示出最高的活性，其T50%为222226℃和T_(90%)为243249℃。与体相LaMnO_3催化剂的表观活化能（97kJ/mol）相比，多孔催化剂具有明显低的表观活化能（5762kJ/mol）。
（3）采用色氨酸辅助的PMMA硬模板法原位制备了yMnO_x/3DOM LaMnO_3（y=5,8,12,16wt%）催化剂，建立了一步法制备菱方相3DOM LaMnO_3负载的MnO_x纳米粒子催化剂的可控合成工艺。结果表明，yMnO_x/3DOM LaMnO_3催化剂的比表面积为1931m~2/g，MnO_x纳米颗粒（粒径为435nm）高度分散在3DOM LaMnO_3表面。与通过等体积浸渍法获得的12wt%MnO_x/体相LaMnO_3催化剂相比，yMnO_x/3DOM LaMnO_3催化剂具有更高的表面吸附氧浓度和比表面积以及较均匀的MnO_x纳米粒子（粒径为418nm）。在VOC（甲苯或甲醇）浓度为1000ppm、VOC/O_2摩尔比为1/400和SV为20000mL/(g h)的反应条件下，12wt%MnO_x/3DOM LaMnO_3催化剂的活性最佳，其对甲苯和甲醇氧化反应的T_(90%)分别为215℃和137℃。
（4）采用表面活性剂辅助的PMMA硬模板法制备了链条状大孔结构的菱方相LaMnO_3和菱方相3DOM La_(0.6)Sr_(0.4)_3催化剂，再利用聚乙烯醇保护的鼓泡还原法制备出了xAu/链条状大孔LaMnO_3（x=1.4,3.1,4.9wt%）和xAu/3DOM La_(0.6)Sr_(0.4)_3（x=3.4,6.4,7.9wt%）催化剂。结果表明，金纳米粒子尺寸在25nm范围内，均匀地分布在催化剂的孔道表面上。xAu/链条状大孔LaMnO_3和xAu/3DOM La_(0.6)Sr_(0.4)_3催化剂的比表面积分别为3033m~2/g和3133m~2/g。4.9wt%Au/链条状大孔LaMnO_3和6.4wt%Au/3DOM La_(0.6)Sr_(0.4)_3催化剂上的表面氧物种浓度较高和低温还原性较好，其催化活性也较高。4.9wt%Au/链条状大孔LaMnO_3和6.4wt%Au/3DOM La_(0.6)Sr_(0.4)_3催化剂对CO氧化反应的T_(90%)分别为91℃（当SV为20000mL/(g h)时）和3℃（当SV为10000mL/(g h)时），对甲苯氧化反应的T_(90%)分别为226℃和170℃（当SV为20000mL/(g h)时）。多孔链条状大孔LaMnO_3负载金催化剂对CO和甲苯氧化反应的表观活化能分别为2937kJ/mol和4752kJ/mol，低于在体相LaMnO_3催化剂上的（分别为63kJ/mol和97kJ/mol）；多孔3DOM La_(0.6)Sr_(0.4)_3负载金催化剂对CO和甲苯氧化反应的表观活化能分别为3132kJ/mol和4448kJ/mol，低于在体相La_(0.6)Sr_(0.4)_3催化剂上的（分别为57kJ/mol和74kJ/mol）。
（5）以KIT-6为硬模板通过纳米浇铸法制备了有序介孔立方晶相Co_3O_4（meso-Co_3O_4），并利用聚乙烯醇保护的还原法制得了xAu/meso-Co_3O_4（x=3.7,6.5,9.0wt%）催化剂。meso-Co_3O_4和xAu/meso-Co_3O_4催化剂的比表面积高达9194m~2/g。6.5wt%Au/meso-Co_3O_4催化剂显示出较高的表面氧浓度、较好的低温还原性和较强的Au与meso-Co_3O_4之间的相互作用，因而显示出较好的催化活性和稳定性。在CO浓度为1vol%和SV为60000mL/(g h)或VOC（苯、甲苯或二甲苯）浓度为1000ppm和SV为20000mL/(gh)的反应条件下，6.5wt%Au/meso-Co_3O_4催化剂对CO、苯、甲苯和二甲苯氧化反应的T_(90%)分别为45℃、189℃、138℃和162℃。
（6）采用抗坏血酸或柠檬酸辅助的PMMA硬模板法制备了单斜相3DOM BiVO_4光催化剂。3DOM BiVO_4光催化剂具有高的比表面积（1824m~2/g）。在所有光催化剂中，比表面积为24m~2/g的BiVO_4-AA-1光催化剂显示出最好的光催化性能。在苯酚初始浓度为0.1mmol/L和H_2O_2添加量为0.6mL条件下反应3小时后，苯酚转化率可达到94%。较低的苯酚初始浓度和适中的H_2O_2用量有助于改善催化剂的光催化性能。
（7）在所制得的每个系列催化剂中，Co_3O_4实心球、LaCoO_3空心球、具有大孔介孔双模孔结构的LaMnO_3-PP-2和LaMnO_3-PL-2、12wt%MnO_x/3DOMLaMnO_3、4.9wt%Au/链条状大孔LaMnO_3、6.4wt%Au/3DOMLa_(0.6)Sr_(0.4)_3、6.5wt%Au/meso-Co_3O_4和BiVO_4-AA-1催化剂对CO、VOC（苯、甲苯、二甲苯或甲醇）或苯酚氧化反应显示出最好的催化活性。基于表征结果和活性数据，我们认为这些催化剂优良的催化性能与其较高的比表面积、较高的吸附氧物种浓度、较好的低温还原性、金与载体之间的强相互作用、良好的多孔结构或较高氧缺陷密度相关。
Due to the high surface areas, large pore volumes, and high-quality pore structures,porous transition-metal oxides have been widely applied in physics and chemistry,such as electronics, magnetics, adsorption, and catalysis. The mesopores in porousmaterials can accommodate guest molecules selectively and the high surface areas ofmesoporous materials are beneficial for the adsorption of gaseous molecules. Theexistence of a macroporous structure can reduce the transfer resistance of guestmolecules and facilitate them to approach the active sites. In addition, macro-ormesoporous supports can also favor the dispersion of active components on theirsurface. It is well known that perovskite-type oxides (ABO_3) exhibit goodperformance in catalyzing the complete oxidation of volatile organic compounds(VOCs) and carbon monoxide, which is associated with the oxygen nonstoichometricamount, surface area, and redox ability. The monoclinic scheelite-type BiVO_4as avisible-light-responsive semiconductor photocatalyst is active photocatalyticallyunder visible-light illumination. In recent years, catalysis by gold has been one of thehot research topics. Catalysis over a supported gold material is related to the nature ofthe support. Usually, an inert support was used to load gold, and the metal-supportstrong interaction can influence the physicochemical properties of the supported metalcatalysts. The studies on the employment of reducible transition-metal oxides ormixed oxides as the support have been rarely reported. The loading of nano-sized goldon the surface of transition-metal oxides or mixed oxides with high surface areas isexpected to increase the loading and gold dispersion, thus effectively avoiding thepossible sintering phenomena during the reaction processes. In ordered to improve thephysicochemical properties of single transition-metal oxides or mixed oxides andhence to enhance their catalytic performance, we have in the present dissertation madeinvestigations on the controlled preparation of three-dimensionally ordered (3DOM)LaMnO_3,3DOM La_(0.6)Sr_(0.4)_3, chain-like macroporous LaMnO_3, and MnO_x/3DOMLaMnO_3with mesoporous skeletons, hollow spherical LaMO_3(M=Mn, Co), solidspherical MOx(M=Mn, Co),3D ordered mesoporous Co_3O_4, Au/3D orderedmesoporous Co_3O_4, and3DOM BiVO_4via the poly(methyl methacrylate)(PMMA) or3D ordered mesoporous silica (KIT-6) hard-templating routes. The physicochemicalproperties of these materials were characterized by means of a number of analyticaltechniques and the catalytic mechanisms were clarified. The catalytic activities of theas-prepared catalysts were evaluated for the oxidation of VOCs (benzene, toluene,xylene or methanol) and CO, so that the relationships between physicochemicalproperties and catalytic performance of the materials could be established. The maininvestigations and obtained results are as follows:
1. The hollow spherical rhombohedral LaMO_3(M=Mn and Co) and solid spherical cubic MOx(M=Mn and Co) nanoparticles were prepared using thesurfactant-assisted PMMA-templating strategy. It is shown that the use ofpolyethylene glycol (PEG) and ethylene glycol (EG) was favorable for theformation of hollow and solid spherical mixed oxides and transition-metal oxides.Compared to their nano-sized counterparts, the spherical LaMO_3and MOxcatalysts possessed much higher surface areas (2133m~2/g), higher adsorbedoxygen species concentrations, and better low-temperature reducibility. For theoxidation of CO and toluene, the catalytic activities of the spherical catalystswere higher than those of the nano-sized catalysts, in which the solid sphericalCo3O4catalyst performed the best for CO oxidation (the T_(90%)(the temperaturerequired for achieving90%CO conversion)=109℃at a space velocity (SV)=10,000mL/(g h)), whereas the hollow spherical LaCoO_3catalyst showed thehighest catalytic activity for toluene oxidation (To90%=237C at SV=20,000mL/(g h)).
2. The rhombohedral3DOM LaMnO_3catalysts with mesoporous skeletons wereprepared via the surfactant-assisted PMMA-templating route. P123or L-lysinemight play a critical role in the generation of mesopores on the macropore wallsof3DOM LaMnO_3. The LaMnO_3catalysts with dual pore structures showedhigher surface areas (3239m~2/g), higher surface oxygen species concentrations,and better low-temperature reducibility. Under the conditions of tolueneconcentration=1,000ppm, toluene/O_2molar ratio=1/400, and SV=20,000mL/(g h), the porous LaMnO_3samples were superior to the bulk counterpart incatalytic performance, with the LaMnO_3-PP-2and LaMnO_3-PL-2samples withmacro-and mesoporous structures performing the best (T50%=222226℃andT_(90%)=243249℃). The apparent activation energies (5762kJ/mol) over theporous catalysts were much lower than that (97kJ/mol) over the bulk counterpart.
3.3DOM-structured rhombohedral LaMnO_3and its supported MnO_xcatalysts(yMnO_x/3DOM LaMnO_3; y=5,8,12, and16wt%) were prepared using anin-situ tryptophan-assisted PMMA-templating strategy, and an one-pot methodfor the controlled preparation of rhombohedral LaMnO_3-supported MnO_xnano-sized catalysts has been established. It is shown that the surface areas ofyMnO_x/3DOM LaMnO_3were1931m~2/g, and the MnO_xnanoparticles (diameter=435nm) were highly dispersed on the surface of3DOM LaMnO_3. Comparedto the12wt%Au/bulk LaMnO_3catalyst derived from the incipient wetnessimpregnation process, the yMnO_x/3DOM LaMnO_3catalysts possessed highersurface areas and adsorbed oxygen species concentrations, low-temperaturereducibility, and more uniform MnO_xnanoparticles (diameter=418nm). Underthe conditions of toluene or methanol concentration=1000ppm, toluene or methanol/O_2molar ratio=1/400, and SV=20,000mL/(g h), the12wt%MnO_x/3DOM LaMnO_3catalyst performed the best (T_(90%)=215and137℃for theoxidation of toluene and methanol, respectively).
4. Chain-like macroporous rhombohedral LaMnO_3and rhombohedral3DOMLa_(0.6)Sr_(0.4)MnO_3and their supported gold (xAu/chain-like macroporous LaMnO_3(x=1.4,3.1, and4.9wt%) and xAu/3DOM La_(0.6)Sr_(0.4)MnO_3(x=3.4,6.4, and7.9wt%)) catalysts were prepared using the surfactant-assisted PMMA-templatingand gas bubble-assisted polyvinyl alcohol-protected reduction methods,respectively. It is shown that the sizes of gold particles were in the range of25nm, and the gold nanoparticles were uniformly distributed on the pore surface ofthe catalysts. xAu/chain-like macroporous LaMnO_3and xAu/3DOMLa_(0.6)Sr_(0.4)MnO_3catalysts possessed surface areas of3033and3133m~2/g,respectively. The4.9wt%Au/chain-like macroporous LaMnO_3and6.4wt%Au/3DOM La_(0.6)Sr_(0.4)MnO_3catalysts showed higher surface oxygen speciesconcentrations and better low-temperature reducibility, and hence higher catalyticperformance. The T_(90%)values obtained over the4.9wt%Au/chain-likemacroporous LaMnO_3and6.4wt%Au/3DOM La_(0.6)Sr_(0.4)MnO_3catalysts were91℃at SV=20,000mL/(g h) and3℃at SV=10,000mL/(g h) for CO oxidation,and226and170℃at SV=20,000mL/(g h) for toluene oxidation, respectively.The apparent activation energies of xAu/chain-like macroporous LaMnO_3catalysts for CO and toluene oxidation were respectively2937and4752kJ/mol, much lower than those (63and97kJ/mol, respectively) of the bulkLaMnO_3catalyst; the apparent activation energies of xAu/3DOM La_(0.6)Sr_(0.4)MnO_3catalysts for CO and toluene oxidation were respectively3132and4448kJ/mol, much lower than that (57and74kJ/mol, respectively) of the bulkLa_(0.6)Sr_(0.4)MnO_3catalyst.
5.3D ordered mesoporous cubic Co3O4(meso-Co3O4) and its supported Au(xAu/meso-Co3O4; x=3.7,6.5, and9.0wt%) nanocatalysts were prepared usingthe KIT-6nanocasting and PVA-protected reduction methods, respectively. Thesurface areas of xAu/meso-Co3O4were in the range of9194m~2/g. The6.5wt%Au/meso-Co3O4catalyst exhibited higher surface oxygen species concentration,better low-temperature reducibility, and stronger Au meso-Co3O4interaction, andhence better catalytic activity and stability. Under the conditions of COconcentration=1vol%and SV=60,000mL/(g h) or VOC (benzene, toluene orxylene) concentration=1000ppm and SV=20,000mL/(g h), the T_(90%)valuesover the6.5wt%Au/meso-Co3O4catalyst were45,189,138, and162℃for theoxidation of CO, benzene, toluene, and xylene, respectively.
6. Monoclinically crystallized3DOM-structured BiVO4photocatalysts with high surface areas (1824m~2/g) were prepared by using the ascorbic acid-or citricacid-assisted PMMA-templating strategy. Among the as-prepared BiVO_4photocatalysts, the one with a surface area of ca.24m~2/g showed the bestvisible-light-driven photocatalytic performance for phenol degradation (phenolconversion=ca.94%at phenol concentration=0.1mmol/L and in the presenceof0.6mL H_2O_2). The lower phenol concentration in aqueous solution and theaddition of an appropriate H_2O_2amount were beneficial for the enhancement inphotocatalytic performance.
7. Among each series of the as-prepared catalysts, solid spherical Co_3O_4, hollowspherical LaCoO_3, LaMnO_3-PP-2and LaMnO_3-PL-2with macro-andmesoporous structures,12wt%MnOx/3DOM LaMnO_3,4.9wt%Au/chain-likemacroporous LaMnO_3,6.4wt%Au/3DOM La0.6Sr0.4MnO_3,6.5wt%Au/meso-Co_3O_4, and BiVO_4-AA-1catalysts showed the highest performance forthe oxidation of CO, VOC (benzene, toluene, xylene or methanol) or phenol.Based on the characterization results and catalytic activity data, it is concludedthat the excellent catalytic performance of these materials might be associatedwith their higher surface areas, higher adsorbed oxygen species concentrations,better low-temperature reducibility, strong gold-support interaction, better qualityporous structures or higher oxygen deficiency density.
引文
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