高密度Au-OV协同位点促进串联光催化CO2加氢制CH3OH

doi:10.1016/S1872-2067(24)60205-6

催化学报 ›› 2025, Vol. 69: 303-314.DOI: 10.1016/S1872-2067(24)60205-6

高密度Au-O_V协同位点促进串联光催化CO₂加氢制CH₃OH

李兴娟^a, 郭昱昊^b, 管勤辉^b, 李晓^a, 张璐璐^a, 冉维广^a, 李娜^a^,^*(), 颜廷江^a^,^b^,^*()

^a曲阜师范大学化学与化工学院, 山东省高校催化转化与清洁能源重点实验室, 山东曲阜 273165
^b陕西科技大学化学与化工学院, 陕西西安 710021

收稿日期:2024-10-22 接受日期:2024-11-22 出版日期:2025-02-18 发布日期:2025-02-10
通讯作者: *电子信箱: lina20201130@163.com (李娜), tingjiangn@163.com (颜廷江).
基金资助:
国家自然科学基金(22172086);国家自然科学基金(22105117);山东省泰山学者人才项目(tsqn202103064);山东省自然科学重大基础研究项目(ZR2021ZD06);山东省自然科学基金项目(ZR2021QB041);山东省自然科学基金项目(ZR2020QE053)

High-density Au-O_V synergistic sites boost tandem photocatalysis for CO₂ hydrogenation to CH₃OH

Xingjuan Li^a, Yuhao Guo^b, Qinhui Guan^b, Xiao Li^a, Lulu Zhang^a, Weiguang Ran^a, Na Li^a^,^*(), Tingjiang Yan^a^,^b^,^*()

^aKey Laboratory of Catalytic Conversion and Clean Energy in Universities of Shandong Province, School of Chemistry and Chemical Engineering, Qufu Normal University, Qufu 273165, Shandong, China
^bCollege of Chemistry and Chemical Engineering, Shaanxi University of Science and Technology, Xi’an 710021, Shannxi, China

Received:2024-10-22 Accepted:2024-11-22 Online:2025-02-18 Published:2025-02-10
Contact: *E-mail: lina20201130@163.com (N. Li), tingjiangn@163.com (T. Yan).
Supported by:
National Natural Science Foundation of China(22172086);National Natural Science Foundation of China(22105117);Taishan Scholars Program of Shandong Province(tsqn202103064);Major Basic Research Project of Shandong Province(ZR2021ZD06);Natural Science Foundation of Shandong Province(ZR2021QB041);Natural Science Foundation of Shandong Province(ZR2020QE053)

摘要/Abstract

摘要：

近年来, CO₂大量排放带来了一系列环境问题, 资源化利用CO₂来开展绿色减碳排放是一项紧迫任务. 利用光催化将CO₂转化为有价值的化学物质, 如一氧化碳(CO)、甲烷(CH₄)、甲醇(CH₃OH), 甚至C₂₊产品, 是解决能源短缺和减少CO₂排放的理想途径. 然而, 传统的单一半导体催化剂通常仅有单一活性位点, 存在光生电子-空穴对的快速复合和反应产物选择性差等问题. 因此, 为了高效、高选择性地实现光催化CO₂还原反应, 有必要设计一种具有多个活性位点协同作用的催化剂.

本文首先利用钼粉、乙醇和H₂O₂为原料在溶剂热条件下合成出三氧化钼(MoO₃), 然后将其在还原气氛中煅烧处理制备出富含氧空位的氧化钼(MoO₃_-x和MoO₂), 进一步通过光沉积技术在三种氧化钼表面负载金纳米颗粒, 最终得到了用于光催化CO₂加氢反应的催化剂(Au/MoO₃, Au/MoO₃_-x和Au/MoO₂). 光催化实验结果表明, Au/MoO₂催化剂在光催化CO₂加氢反应中产生的CH₃OH产物的产率呈现递增的趋势, CH₃OH的生成来自于另一产物CO的加氢反应. X射线粉末衍射、扫描电镜和高分辨透射电镜等结果表明, 相比MoO₃和MoO₃_-x, 氧空位浓度最高的MoO₂更利于Au纳米颗粒的锚定和均匀负载, 金属-氧化物界面作用更强. 光电流响应和阻抗图谱等结果表明, Au/MoO₂催化剂界面形成的肖特基结, 显著提高了光生载流子的传输和分离效率. CO₂和H₂程序升温脱附结果表明, Au/MoO₂催化剂上的CO₂和H₂吸附活化能力强于Au/MoO₃和Au/MoO₃_-x催化剂. 原位红外实验表明, Au/MoO₂催化剂上CO₂经HCOO^*和HCO₃^*中间体加氢生成甲醇, 且Au/MoO₂催化剂上的HCOO^*和HCO₃^*物种浓度显著高于其它催化剂. 由于MoO₂具有丰富的氧空位, 更容易吸附和活化CO₂分子; Au位点的存在促进了H₂解离并增加了^*H覆盖率, 使其提供大量的H原子更易与吸附在Mo位点上的CO₂结合形成吸附中间体^*CO或CO. Au/MoO₂催化剂中的Au和MoO₂之间建立的强界面相互作用, 有利于CO在Mo位点上的吸附并进一步实现串联反应合成甲醇.

综上所述, 本文系统研究了Au负载不同氧空位浓度的MoO_x催化剂的结构对光催化CO₂还原产物的影响规律, 揭示了氧空位和Au纳米颗粒协同促进串联光催化CO₂加氢制甲醇的反应机理, 为设计具有多种活性位点协同串联机制的光催化CO₂还原催化剂提供了一种新思路.

关键词: CO₂加氢, 串联催化, 甲醇, Au/MoO₂, 光催化

Abstract:

The production of renewable methanol (CH₃OH) via the photocatalytic hydrogenation of CO₂ is an ideal method to ameliorate energy shortages and mitigate CO₂ emissions: however, the highly selective synthesis of methanol at atmospheric pressure remains challenging owing to the competing reverse water-gas shift (RWGS) reaction. Herein, we present a novel approach for the synthesis of CH₃OH via photocatalytic CO₂ hydrogenation using a catalyst featuring highly dispersed Au nanoparticles loaded on oxygen vacancy (O_V)-rich molybdenum dioxide (MoO₂), resulting in a remarkable selectivity of 43.78%. The active sites in the Au/MoO₂ catalyst are high-density Au-oxygen vacancies, which synergistically promote the tandem methanol synthesis via an initial RWGS reaction and subsequent CO hydrogenation. This work provides comprehensive insights into the design of metal-vacancy synergistic sites for the highly selective photocatalytic hydrogenation of CO₂ to CH₃OH.

Key words: CO₂ hydrogenation, Tandem catalysis, Methanol, Au/MoO₂, Photocatalysis

李兴娟, 郭昱昊, 管勤辉, 李晓, 张璐璐, 冉维广, 李娜, 颜廷江. 高密度Au-O_V协同位点促进串联光催化CO₂加氢制CH₃OH[J]. 催化学报, 2025, 69: 303-314.

Xingjuan Li, Yuhao Guo, Qinhui Guan, Xiao Li, Lulu Zhang, Weiguang Ran, Na Li, Tingjiang Yan. High-density Au-O_V synergistic sites boost tandem photocatalysis for CO₂ hydrogenation to CH₃OH[J]. Chinese Journal of Catalysis, 2025, 69: 303-314.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60205-6

https://www.cjcatal.com/CN/Y2025/V69/I2/303

图/表 7

Fig. 1. (a) Schematic illustration of the synthesis of MoOx. (b) XRD patterns of Au/MoOx. High-resolution Au 4f (c), Mo 3d (d) and O 1s (e) XPS spectra of Au/MoOx.

Fig. 2. SEM images of Au/MoO3 (a), Au/MoO3-x (b) and Au/MoO2 (c). TEM images and corresponding particle size distributions of Au/MoO3 (d), Au/MoO3-x (e) and Au/MoO2 (f). HR-TEM images of Au/MoO3 (g), Au/ MoO3-x (h) and Au/MoO2 (i).

Fig. 3. Photocatalytic CO2 hydrogenation performances. CO production rate of MoO3 (a), MoO3-x (b), MoO2 (c) with and without solar irradiation at various reaction temperatures. CH3OH (top) and CO (bottom) production rate over Au/MoO3 (d), Au/MoO3-x (e), Au/MoO2 (f) at various reaction temperatures with and without solar irradiation.

Fig. 4. Long-term performance of Au/MoO3 (20 h) (a), Au/MoO3-x (20 h) (b) and Au/MoO2 (25 h) (c) in catalyzing the hydrogenation of CO2 at 225 °C with light irradiation. (d) Long-term (20 h) performance of Au/MoO3, Au/MoO3-x and Au/MoO2 in catalyzing the hydrogenation of CO at 225 °C with light irradiation.

Fig. 5. (a) UV-vis absorption spectra of MoOx and Au/MoOx. (b) Energy band diagram of Au/MoO2. In situ XPS spectra of Au/MoO2 with and without irradiation: Au 4f (c) and (d) Mo 3d spectra. Transient photocurrent response curves (e) and EIS Nyquist plots (f) MoO2 and Au/MoOx.

Fig. 6. CO2 adsorption isotherms (a), CO2-TPD spectra (b), CO-TPD spectra (c) and H2-TPD spectra (d) of MoO2 and the Au/MoOx catalysts.

Fig. 7. In situ DRIFTS of CO2 hydrogenation on Au/MoO3 (a), Au/MoO3-x (b), Au/MoO2 (c) and MoO2 (d) catalysts under light irradiation at 225 °C. (e) Proposed mechanism of methanol synthesis on Au/MoO2 via tandem CO2 hydrogenation.

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高密度Au-O_V协同位点促进串联光催化CO₂加氢制CH₃OH

High-density Au-O_V synergistic sites boost tandem photocatalysis for CO₂ hydrogenation to CH₃OH

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