用于间甲酚高效加氢脱氧制芳烃的负载型W2C纳米催化剂的活性位研究

doi:10.1016/S1872-2067(24)60138-5

催化学报 ›› 2024, Vol. 67: 91-101.DOI: 10.1016/S1872-2067(24)60138-5

用于间甲酚高效加氢脱氧制芳烃的负载型W₂C纳米催化剂的活性位研究

杨艳玲^a^,^b^,^c^,¹, 韩沛杰^a^,¹, 张元宝^a^,¹, 林敬东^a, 万绍隆^a, 王勇^d, 刘海超^e, 王帅^a()

^a固体表面物理化学国家重点实验室, 能源材料化学协同创新中心, 厦门大学化学化工学院, 福建厦门 361005, 中国
^b集美大学轮机工程学院, 福建厦门 361000, 中国
^c厦门市海洋腐蚀与智能防护材料重点实验室, 福建厦门 361000, 中国
^d华盛顿州立大学化学工程与生物工程学院, 华盛顿州, 美国
^e北京大学化学与分子工程学院, 北京分子科学国家研究中心, 北京 100871, 中国

收稿日期:2024-06-27 接受日期:2024-09-09 出版日期:2024-12-18 发布日期:2024-11-30
通讯作者: 王帅
作者简介:
¹共同第一作者.
基金资助:
国家重点研发计划(2021YFA1501104);国家自然科学基金(21922201);国家自然科学基金(22202041);国家自然科学基金(21872113);中央高校基本科研基金(20720220008)

Site requirements of supported W₂C nanocatalysts for efficient hydrodeoxygenation of m-cresol to aromatics

Yanling Yang^a^,^b^,^c^,¹, Peijie Han^a^,¹, Yuanbao Zhang^a^,¹, Jingdong Lin^a, Shaolong Wan^a, Yong Wang^d, Haichao Liu^e, Shuai Wang^a()

^aState Key Laboratory for Physical Chemistry of Solid Surfaces, Collaborative Innovation Center of Chemistry for Energy Materials, and College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, Fujian, China
^bCollege of Marine Engineering, Jimei University, Xiamen 361000, Fujian, China
^cKey Laboratory for Marine Corrosion and Intelligent Protection Materials of Xiamen, Jimei University, Xiamen 361000, Fujian, China
^dVoiland School of Chemical Engineering and Bioengineering, Washington State University, Pullman, WA 99164, United States
^eBeijing National Laboratory for Molecular Sciences, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China

Received:2024-06-27 Accepted:2024-09-09 Online:2024-12-18 Published:2024-11-30
Contact: Shuai Wang
About author:
¹Contributed equally to this work.
Supported by:
National Key Research and Development Program of China(2021YFA1501104);National Natural Science Foundation of China(21922201);National Natural Science Foundation of China(22202041);National Natural Science Foundation of China(21872113);Fundamental Research Funds for the Central Universities(20720220008)

摘要/Abstract

摘要：

生物质作为地球上最主要的可再生有机碳资源, 其高效转化制取液体燃料和化学品对推动“碳中和”具有重要意义. 木质素是仅次于纤维素的第二大类生物质组分, 含有丰富的含氧官能团和芳香环结构. 将木质素衍生物通过选择性加氢脱氧反应制取芳香族化合物为木质素资源的优化利用提供了一条极具潜力的途径. 加氢脱氧反应通常使用过渡金属为催化剂, 但该类催化剂在促进木质素衍生物中C-O键断裂的同时, 往往会造成芳香环的过度加氢, 导致反应选择性不理想. 近年研究表明, 金属碳化物催化剂兼具较好的促进C-O键氢解能力和抑制C=C键加氢能力. 但这些研究多以块体催化剂为主, 对催化剂的构-效关系尚缺乏深入认识, 严重阻碍了金属碳化物催化剂的合理设计与优化.

合成粒径均一且可调变的金属碳化物纳米粒子有利于深入考察金属碳化物催化剂在加氢脱氧反应中的构-效关系. 本文采用液相原子层沉积法在较宽的负载量范围(WO₃: 1.0 wt%-50 wt%)内将WO₃前驱体嫁接于SiO₂载体表面. 紫外-可见光谱和高分辨透视电镜表征结果证实, 此合成方法可将WO₃均匀分散在SiO₂载体上. 以此为基础, 在优化条件下对WO₃/SiO₂前体进行碳化处理, 获得了相应W₂C粒径均一且可在0.7-15 nm范围调控的W₂C/SiO₂催化剂. 以木质素衍生物间甲酚的加氢脱氧转化为模型反应, 不同W₂C粒径的W₂C/SiO₂催化剂在350 °C下均表现出较好的甲苯选择性(>95%). 在其他氧化物载体上负载W₂C催化剂(如TiO₂, ZrO₂等)或以其他木质素衍生物为加氢脱氧反应的底物(如苯甲醇、苯甲醚、愈创木酚等)同样可获得高C-O键氢解选择性, 体现了W₂C在催化C-O键氢解反应中的优越性. 基于W₂C单位质量考察催化活性, 粒径为~7 nm的W₂C/SiO₂催化剂上的加氢脱氧速率最高; 而将催化活性为归结至催化剂表面暴露的W位点时结果表明, 在0.7-15 nm粒径范围内, 随W₂C粒径的逐渐增大, 催化剂表面W位点的本征活性呈单调上升变化. 高分辨率透射电镜结果则表明, 该粒径效应与负载在SiO₂上的大粒径W₂C表面易暴露高指数晶面相关. 结合催化动力学、多种探针分子的程序升温脱附实验及理论计算结果表明, W₂C纳米颗粒在反应条件下被间甲酚或由其衍生得到的反应中间体所覆盖饱和, 且间甲酚加氢脱氧反应的速控步骤为H原子进攻C₇H₇*中间体生成甲苯, 而非间甲酚的C-O键断裂步骤. 此外, 以W₂C(001)和W₂C(102)表面模型来考察W₂C催化剂的粒径效应. 理论计算表明, 相较于低指数晶面, 高指数晶面上所暴露出的高不饱和度位点能够更为有效地稳定反应中间体和过渡态, 进而带来更高的加氢脱氧活性.

综上, 本文通过系统考察负载型W₂C催化剂的构-效关系, 揭示了W₂C催化剂在木质素衍生物加氢脱氧反应中独特的粒径效应. 该独特性源于由W₂C强亲氧性所诱导的催化活性位与氧化物载体之间的强相互作用, 可为进一步设计和构筑高性能金属碳化物基催化剂提供有益参考.

关键词: 木质素衍生物, 加氢脱氧, 碳化钨, 多相催化, 构-效关系, 尺寸效应, 动力学, 密度泛函理论计算

Abstract:

Selective hydrodeoxygenation of lignin derivatives into aromatic compounds is a promising route for the upgrading of lignin feedstocks. Metal carbide catalysts have exhibited excellent selectivity in hydrodeoxygenation reactions, while their structure-activity relationship is still in ambiguity. Herein, a liquid-phase atomic layer deposition method was employed to synthesize W₂C/SiO₂ catalysts with uniform and size-controllable W₂C nanoparticles. For gas-phase hydrodeoxygenation of lignin-derived m-cresol at 350 °C, these W₂C/SiO₂ catalysts showed superior toluene selectivities (>95%) regardless of the W₂C particle size. An optimal W₂C particle size of ~7 nm was obtained for achieving the highest W₂C-based hydrodeoxygenation rate. In contrast, the turnover rate per surface W site increased almost monotonously as the W₂C particle size increased within 0.7‒15 nm, attributable to high-index planes appeared on the larger W₂C nanoparticles. Kinetic effects of m-cresol and H₂, taken together with temperature-programmed desorption of probe molecules and theoretical treatments, further indicate that the W₂C surface is nearly saturated by adsorbed m-cresol or its derivates under the reaction condition and the H-addition of the C₇H₇* intermediate to form toluene, instead of the initial C-O cleavage in m-cresol, acts as the rate-determining step. A side-by-side comparison between W₂C(102) and W₂C(001) catalyst surfaces in theoretical simulations of m-cresol hydrodeoxygenation verifies that high-index planes can stabilize kinetically-relevant transition states more effectively than the low-index ones, as a result of more available less-coordinated active sites on the former. The above findings bring new mechanistic insights into the site requirements of supported W₂C nanocatalysts, distinct from those metal-catalyzed hydrodeoxygenation of oxygenates.

Key words: Lignin derivative, Hydrodeoxygenation, Tungsten carbide, Heterogeneous catalysis, Structure-activity relationship, Size effect, Kinetics, Density functional theory calculation

杨艳玲, 韩沛杰, 张元宝, 林敬东, 万绍隆, 王勇, 刘海超, 王帅. 用于间甲酚高效加氢脱氧制芳烃的负载型W₂C纳米催化剂的活性位研究[J]. 催化学报, 2024, 67: 91-101.

Yanling Yang, Peijie Han, Yuanbao Zhang, Jingdong Lin, Shaolong Wan, Yong Wang, Haichao Liu, Shuai Wang. Site requirements of supported W₂C nanocatalysts for efficient hydrodeoxygenation of m-cresol to aromatics[J]. Chinese Journal of Catalysis, 2024, 67: 91-101.

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图/表 8

Fig. 1. Structural characterization of WO3/SiO2 precursors with bulk WO3 as reference. (a) Illustration of the synthesis strategy of high-loading WO3/SiO2 samples via the liquid-phase atomic layer deposition method. XRD patterns (b), UV-vis-determined edge energy values (c), and surface area and averaged WO3 size values (d) for the xWO3/SiO2 and bulk WO3 samples. Representative TEM images and corresponding statistical results of WO3 particle size for 1.0WO3/SiO2 (e) and 15WO3/SiO2 (f).

Fig. 2. Characterization of WO3/SiO2 precursors in the carburization process. (a) Mass singles of CH4, H2O and H2 during the temperature-programmed carbonization process of 15WO3/SiO2 in flowing 20% CH4/H2. (b) XRD patterns of 15WO3/SiO2 after the carbonization at 650 °C for 3 and 6 h with the standard diffraction peak positions of metallic W labeled. (c) Schematics of the stepwise conversion of WO3/SiO2 in the carburization process.

Fig. 3. Structural characterization of W2C/SiO2 and bulk W2C catalysts. XRD patterns (a) and TEM-determined average W2C particle sizes (b) for the W2C/SiO2 and bulk W2C catalysts. (c-h) (HR)TEM images of W2C/SiO2-3.0 nm and W2C-14.9 nm catalysts with corresponding fast Fourier transformed (FFT) patterns. (i) Schematics of exposed planes of W2C on the SiO2 support varied with the W2C loading.

Fig. 4. Evaluation of W2C/SiO2 catalysts in hydrodeoxygenation of m-cresol. (a) Schematics of m-cresol hydrodeoxygenation to toluene on W2C. (b) Effects of W2C particle size on hydrodeoxygenation rates and toluene selectivity. (c) Turnover rate of m-cresol hydrodeoxygenation as a function of W2C particle size. Effects of m-cresol (d) and H2 (e) partial pressures on the hydrodeoxygenation rate of m-cresol. Reaction conditions: 350 °C, 0.5 kPa m-cresol, 40 kPa H2, ca. 20% m-cresol conversion obtained by varying catalyst amount, balanced by N2, if not stated otherwise. The partial pressure of H2 was kept at 40 kPa in (d), and the corresponding value of m-cresol was kept at 0.15 kPa in (e).

Table 1 Proposed elementary steps of m-cresol hydrodeoxygenation on W2C surface a.

Fig. 5. Structure-activity relationship of W2C-based catalysts in m-cresol hydrodeoxygenation. (a) Parity plot for all measured m-cresol hydrodeoxygenation rates vs. those predicted using Eq. (3) (measured data adopted from Fig. 4). (b) Regression-fitted kinetic parameters of Eq. (3) for the m-cresol hydrodeoxygenation rates shown in (a). (c) Desorption temperature of m-cresol on W2C/SiO2 or bulk W2C determined by TGA. (d) CO-TPD profiles for W2C/SiO2 and W2C bulk catalysts.

Fig. 6. Comparison of m-cresol adsorption on W2C(001) and W2C(102) surfaces. (a) DFT-optimized structures for adsorbed m-cresol. (b) Corresponding adsorption energies in terms of electronic energy, enthalpy, and Gibbs free energy (300 °C and 100 kPa). Charge density difference analysis for adsorbed m-cresol on W2C(001) (c) and W2C(102) (d) surfaces. Cyan and yellow stand for positive and negative charge regions, respectively.

Fig. 7. Reaction pathway and activity of m-cresol hydrodeoxygenation on W2C surfaces. (a) DFT-derived Gibbs free energy diagram of m-cresol hydrodeoxygenation on W2C(001) (red) and W2C(102) (black) surfaces at 300 °C and 100 kPa. (b) DFT-optimized structures for the transition states involved in (a). The balls refer to the atoms of W (blue), C (grey), O (red), and H (white), respectively.

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用于间甲酚高效加氢脱氧制芳烃的负载型W₂C纳米催化剂的活性位研究

Site requirements of supported W₂C nanocatalysts for efficient hydrodeoxygenation of m-cresol to aromatics

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