化工学报 ›› 2021, Vol. 72 ›› Issue (6): 2972-3001.DOI: 10.11949/0438-1157.20210108
收稿日期:
2021-01-18
修回日期:
2021-04-06
出版日期:
2021-06-05
发布日期:
2021-06-05
通讯作者:
杨宇森
作者简介:
周石杰(1998—),女,硕士研究生,基金资助:
ZHOU Shijie(),REN Zhen,YANG Yusen(),WEI Min
Received:
2021-01-18
Revised:
2021-04-06
Online:
2021-06-05
Published:
2021-06-05
Contact:
YANG Yusen
摘要:
金属氧化物作为一类重要工业催化剂,广泛应用于合成氨工业、能源化工、精细化工等重要的工业生产过程。金属氧化物的形貌对其性能有重要的影响,具有特定形貌的金属氧化物催化剂因其结构上的优势,使其在许多方面表现出不同于常规块体材料的独特性能,成为当前材料科学领域的研究热点。本文总结了不同形貌的金属氧化物的制备方法、生长机制及其结构特性,聚焦于金属氧化物在氧化反应、加氢反应以及蒸汽重整反应中的最新研究进展。最后,进一步讨论了金属氧化物催化剂未来的发展趋势以及面临的挑战,并提出了解决这些问题的有效方案。
中图分类号:
周石杰, 任祯, 杨宇森, 卫敏. 不同形貌金属氧化物的制备及其在工业催化反应中的应用[J]. 化工学报, 2021, 72(6): 2972-3001.
ZHOU Shijie, REN Zhen, YANG Yusen, WEI Min. Preparation and application of metal oxides with various morphology for industrial catalysis[J]. CIESC Journal, 2021, 72(6): 2972-3001.
图1 在160℃下前体氧化物合成的FE-SEM图:2 h (a)、3 h (b)、4 h (c)、5 h (d)、6 h (e) [48]
Fig.1 FE-SEM images of the precursors synthesized at 160℃ for 2 h (a), 3 h (b), 4 h (c), 5 h (d), 6 h (e)[48]
图2 多壳ZnO空心微球的演化过程。碳微球在加热之前(室温)和在不同温度(400℃、400℃下30 min、420℃、440℃、460℃、480℃和500℃)下加热后浸入硝酸锌溶液中的透射电子显微镜图像。3 mol/L和5 mol/L硝酸锌溶液分别用于样品Ⅰ、Ⅱ、Ⅲ和样品Ⅳ、Ⅴ、Ⅵ、Ⅶ、Ⅷ、Ⅸ。样品Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ和Ⅵ中使用的碳质微球的直径为3 μm, 样品Ⅶ、Ⅷ和Ⅸ中使用的碳质微球的直径为4 μm。快速加热模式和中速加热模式下的温度分别在2和1℃/min下直接升高到500℃而慢速加热模式下的温度在1℃/min下直接升高到500℃并且在400℃保持30 min。在第一列中,样品Ⅰ~Ⅵ比例尺为1 μm,样品Ⅶ~Ⅸ比例尺为1.3 μm。第二列中的所有样品比例尺均为0.5 μm, 而第三列及更高列中样品比例尺均为0.3 μm(a)。通过不同的加热过程形成多壳ZnO中空微球的图示(b) [57]
Fig.2 Evolution process of the family of multishelled ZnO hollow microspheres. Transmission electron microscopy images of carbonaceous microspheres after immersion in zinc nitrate solutions before heating (room temperature) and after heating at different temperatures (400℃, 400℃ for 30 min, 420℃, 440℃, 460℃, 480℃ and 500℃). 3 and 5 mol/L zinc nitrate solutions were used in samples Ⅰ, Ⅱ, Ⅲ and samples Ⅳ, Ⅴ, Ⅵ, Ⅶ, Ⅷ, Ⅸ, respectively. The diameters of carbonaceous microspheres used in samples Ⅰ, Ⅱ, Ⅲ, Ⅳ, Ⅴ and Ⅵ are 3 μm, and those used in samples Ⅶ, Ⅷ, and Ⅸ are 4 μm. The temperature in the fast and medium heating modes is directly increased to 500℃ at 2 and 1℃/min respectively, while the temperature in the slow heating mode is increased to 500℃ at 1℃/minwith 30 min holding at 400℃. The scale bars are 1 μm for the samples from Ⅰ to Ⅵ and 1.3 μm for samples from Ⅶ to Ⅸ in the first column. All the scale bars in the second column are 0.5 μm, while the scale bars in the third and higher columns are all 0.3 μm(a). Illustration of the formation of multishelled ZnO hollow microspheres through different heating processes(b) [57]
图3 三种形貌的焙烧后的Co3O4的SEM图像及其结构模型: Co3O4立方体[(a)~(c)], Co3O4截短的八面体[(d)~(f)]和Co3O4八面体[(g)~(i)][58]
Fig.3 SEM images of the three types of calcined Co3O4 and their structure models: Co3O4 cubes[(a)~(c)], Co3O4 truncated octahedra[(d)—(f)], and Co3O4 octahedra[(g)—(i)] [58]
图5 ZnO纳米晶体随时间演变为具有双蛋黄结构的ZnO空心球: 1 h (a), 12 h (b), 24 h (c), 相应演变过程的示意图(d) [64]
Fig.5 Time-dependent evolution of ZnO nanocrystals to ZnO hollow spheres with double-yolk egg structure: 1 h (a), 12 h (b), 24 h (c). The corresponding schematic graphs of the evolution process (d) [64]
图6 制备BHC-TiO2的总流程图[(a)~(d)]: 相应的BHC-TiO2制备程序的FESEM[(e)~(h)], BSE-SEM[(i)~(l)]和TEM[(m)~(p)]图。白色箭头表示破裂的空心立方结构。(e)~(h) 比例尺为1 μm, (i)~(p) 比例尺为500 nm[66]
Fig.6 Overall flowchart for fabrication of BHC-TiO2[(a)—(d)]; Corresponding FESEM[(e)—(h)], BSE-SEM [(i)—(l)] and TEM images[(m)—(p)] of the BHC-TiO2 fabrication procedure. The white arrows indicate the cracked hollow cubic structures. The scale bars are 1 μm [(e)—(h)] and 500 nm[(i)—(p)][66]
图7 MIL-53(Fe)的生长过程及其相应的铁氧化物的形貌(a)以及Fe2O3-2和Fe2O3-6的形成过程的示意图(b) [67]
Fig.7 Schematic illustration of the process of MIL-53(Fe) growth and morphology of their corresponding iron oxides (a) and the formation process of Fe2O3-2 and Fe2O3-6 (b) [67]
图8 在9.55 kW/cm2(a), 15.92 kW/cm2 (b), 22.29 kW/cm2 (c), 28.66 kW/cm2 (d)和200 kHz的激光功率密度下生长5 min的ZnO晶体的SEM图像。动力学控制(左侧)和热力学控制(右侧)过程中晶体生长的示意图(e)。所有比例尺代表长度均为500 nm[68]
Fig.8 SEM pictures of ZnO crystals grown under laser power density of 9.55 kW/cm2 (a), 15.92 kW/cm2 (b), 22.29 kW/cm2 (c), 28.66 kW/cm2 (d) in 200 kHz for 5 min. Schematic illustration of crystal growth in kinetically controlled (left direction) and thermodynamically controlled (right direction) processes (e). All scale bars represent 500 nm in length[68]
图9 Tdep对Co3O4薄膜的TC(220)、(311)、(111)、(400)和(511)的影响(a), (111)面的生长机理(b), 放大的FESEM图像(c)和在773 K下制备的Co3O4薄膜的纳米墙结构示意图(d) [69]
Fig.9 Effect of Tdep on TC(220), (311), (111), (400) and (511) of Co3O4 films (a), growth mechanism of (111) planes (b), enlarged FESEM image (c) and schematic of nanowall structure of Co3O4 film prepared at 773 K(d) [69]
图10 在不同温度下制备的样品的SEM和TEM图像: S-600[(a),(b)], S-750[(c),(d)], S-850[(e),(f)]和S-950[(g),(h)][70]
Fig.10 SEM and TEM images of samples prepared at different temperatures: S-600[(a),(b)], S-750[(c),(d)], S-850[(e),(f)] and S-950[(g),(h)][70]
图11 高温还原产生的额外的Ce3+位点有利于反应物和中间体的吸附的示意图[75]
Fig.11 Additional Ce3+ sites derived from high-temperature reduction favoring adsorption of the reactant and intermediate[75]
图12 CeO2-R[(a),(b)], CeO2-P[(c),(d)], CeO2-C[(e),(f)]的TEM和高分辨率TEM (HRTEM) 图像, CeO2-O的SEM(g)和HRTEM(h)图像, 插图为CeO2-R, CeO2-P, CeO2-C和CeO2-O的暴露晶面[78]
Fig.12 TEM and high-resolution TEM (HRTEM) images of CeO2-R[(a),(b)], CeO2-P[(c),(d)], CeO2-C[(e),(f)], SEM(g) and HRTEM(h) images of CeO2-O. The insets schematically illustrate the crystal planes exposed on the CeO2-R, CeO2-P, CeO2-C and CeO2-O[78]
图13 具有8或4个吸附的CO分子的Au/CeO2(100) (a)和Au/CeO2(111) (b)催化的示意性CO氧化途径表明尽管Au/CeO2(111)对于附加的O—C—O形成步骤是必须的[(b)图,步骤②], 但CO氧化发生在Au-CeO2界面[86]
Fig.13 Schematic CO oxidation pathways catalyzed by Au/CeO2(100) (a) and Au/CeO2(111) (b) with 8 or 4 adsorbed CO molecules show that CO oxidation occurs at the Au-CeO2 interface, although an additional O—C—O formation step [(b), step②] is required for Au/CeO2(111) [86]
图14 α-Fe2O3-THB样品的TEM图[(ⅰ),(ⅱ)], HRTEM图(ⅲ), IFFT图像(ⅳ)(a). α-Fe2O3-QC样品的TEM图[(ⅰ),(ⅱ)], HRTEM图(ⅲ), IFFT图(ⅳ)(b). α-Fe2O3-HS样品的 TEM图(ⅰ), SAED模式(ⅱ)和示意图(ⅲ)(c)[87]
Fig.14 TEM images [(ⅰ),(ⅱ)], HRTEM image (ⅲ), IFFT image (ⅳ) of the α-Fe2O3-THB sample(a). TEM images [(ⅰ),(ⅱ)], HRTEM image (ⅲ), IFFT image (ⅳ) of α-Fe2O3-QC sample (b). TEM image (ⅰ), SAED pattern (ⅱ), and schematic illustration (ⅲ) of α-Fe2O3-HS sample(c)[87]
图15 在甲醇转化率为30%~40%时, Pd/ZnO-N (a)和Pd/ZnO-P(b)的CO选择性(反应条件: 100~200 mg催化剂, 甲醇浓度 6.4%(mol), 催化剂质量/进料气流速=0.037~0.123 g?s/ml, T = 250℃)[88]
Fig.15 CO selectivity of Pd/ZnO-N (a) and Pd/ZnO-P (b) with Pd loading amount under methanol conversion of 30%—40% [88]
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