超低负载的0.1(PtMnFeCoNi)/TiO2催化剂: 通过高熵策略调节活性金属位点的电子状态以促进CO的氧化

doi:10.1016/S1872-2067(25)64770-X

催化学报 ›› 2025, Vol. 76: 173-184.DOI: 10.1016/S1872-2067(25)64770-X

超低负载的0.1(PtMnFeCoNi)/TiO₂催化剂: 通过高熵策略调节活性金属位点的电子状态以促进CO的氧化

赵永奇^a, 蒋俊杰^a, 邹洋^a, 王璞^a, 李雪^a, 刘霄龙^a^,^b^,^*(), 朱廷钰^a

^a中国科学院过程工程研究所, 绿色过程与工程重点实验室, 北京 100190
^b中国科学院, 盐湖资源绿色高值化利用重点实验室, 青海西宁 810008

收稿日期:2025-04-03 接受日期:2025-06-19 出版日期:2025-09-18 发布日期:2025-09-10
通讯作者: 刘霄龙
基金资助:
国家自然科学基金(52170118);国家自然科学基金(52322004);国家自然科学基金(52400141);中国博士后科学基金面上基金(2024M763296)

Ultra-low doping 0.1(PtMnFeCoNi)/TiO₂ catalysts: Modulating the electronic states of active metal sites to enhance CO oxidation through high entropy strategy

Yongqi Zhao^a, Junjie Jiang^a, Yang Zou^a, Pu Wang^a, Xue Li^a, Xiaolong Liu^a^,^b^,^*(), Tingyu Zhu^a

^aCAS Key Laboratory of Green Process and Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China
^bKey Laboratory of Green and High-value Utilization of Salt Lake Resources, Chinese Academy of Sciences, Xining 810008, Ningxia, China

Received:2025-04-03 Accepted:2025-06-19 Online:2025-09-18 Published:2025-09-10
Contact: Xiaolong Liu
Supported by:
National Natural Science Foundation of China(52170118);National Natural Science Foundation of China(52322004);National Natural Science Foundation of China(52400141);China Postdoctoral Science Foundation(2024M763296)

摘要/Abstract

摘要：

在钢铁生产过程中, 排放的烧结烟气中高浓度CO已经成为制约我国改善大气环境质量的关键因素. 目前, 催化氧化技术是实现CO减排的重要手段, 但其大规模应用受限于催化剂成本. 本文旨在通过简单的煅烧工艺制备了一种超低负载量的高熵催化剂, 不仅实现烧结烟气中CO的高效稳定催化净化, 也进一步减少了贵金属活性组分的用量, 实现催化剂成本的降低. 研究表明, 高熵催化剂中多个位点的协同效应有助于同时实现高活性(组成设计)和低成本(非贵金属替代), 为烧结烟气CO催化剂的实际应用提供了研究思路.

本文设计了一种超低负载量(0.1 wt%)的0.1(PtMnFeCoNi)/TiO₂催化剂, 通过将过渡金属(Mn, Fe, Co和Ni)与贵金属Pt复合, 锚定在锐钛矿型TiO₂载体表面, 并与之形成了强金属-载体相互作用(SMSI). 实验结果表明, 相比于0.1Pt/TiO₂催化剂, 0.1(PtMnFeCoNi)/TiO₂催化剂对CO的完全氧化温度从270 °C降至230 °C; 并且在H₂O和SO₂存在的条件下, 催化剂氧化活性仍然保持在80%以上. X射线衍射、高分辨率透射电子显微镜和拉曼光谱分析表明, 高熵活性组分均匀分散在TiO₂表面, 且未改变TiO₂的晶体结构. X射线光电子能谱结果表明, 与单一或双活性组分相比, 高熵活性组分为TiO₂的晶格氧原子提供了一种新的电子获取途径. 多种金属元素(Pt, Mn, Fe, Co和Ni)之间的协同作用有效地调节了活性金属位点与载体之间的电子状态, 从而增强了从Ti到O的电子传输, 使得电子从高电负性元素(如O)转移到钛的3d轨道, 从而增加了Ti周围的电子密度, 减弱了钛与配体氧之间的相互作用, 促进了TiO₂表面晶格氧转化为反应性氧物种. 原位漫反射红外光谱和密度泛函理论计算结果表明, 高熵活性组分的引入增加了TiO₂表面的局部电子密度, 促进了催化剂表面的电子分散现象. 高熵活性组分与TiO₂之间显著的电荷相互作用导致了晶格的扭曲, 这种扭曲有利于催化剂系统中的电子转移, 从而使CO和O₂分子更容易转化为CO*和O*. 通过将金属间隙电子填充到TiO₂的亚间隙状态, 促进了晶格氧的活化, 从而增强了高熵组分与TiO₂载体之间的SMSI, 进而提高了CO和O₂的吸附效率. CO在0.1(PtMnFeCoNi)/TiO₂催化剂吸附并与活化的O物种生成大量的碳酸盐物质, 因此CO在0.1(PtMnFeCoNi)/TiO₂催化剂上的催化氧化过程遵循M-vK反应机制.

综上, 本研究通过研究高熵组分间的多元素协同效应, 成功激活了TiO₂晶格氧活化机制, 阐明高熵催化剂多组分协同促进CO催化氧化的本质, 为烧结烟气CO催化净化技术的应用提供新的研究思路. 本文对于在原子水平上理解多金属组分对催化剂活性的协同调节具有重要意义, 也为有效降低催化剂中贵金属使用量提供了一种策略.

关键词: 高熵催化剂, 超低负载, CO氧化, 烧结烟气, 金属-载体间强相互作用

Abstract:

The catalyst cost is a key factor limiting the CO purification of sintering flue gas. Here, an ultra-low-loading high-entropy catalyst was prepared by simple calcination process. By anchoring multiple active metal sites in the stable anatase TiO₂ phase, it shows efficient CO catalytic oxidation activity. The metal components (Pt, Mn, Fe, Co, Ni) were uniformly dispersed on the surface of TiO₂ in the form of high-entropy compounds and undergo strong metal and support interaction with TiO₂. The results showed that 0.1(PtMnFeCoNi)/TiO₂ achieved complete oxidation of CO at 230 °C, and its catalytic oxidation ability was significantly better than that of the corresponding monometallic and bimetallic catalysts. The high-entropy component adjusts the electronic environment between the TiO₂ support and the metal to promote the reduction of the Ti₃_d band gap, enhances the electron-induced ability of the catalytic system to gas molecules (CO and O₂), and exhibits excellent resistance to SO₂ and H₂O. The work is of great significance to understand the synergistic regulation of catalyst activity by multiple metal at the atomic level and provides a strategy for effectively reducing the content of precious metals in the catalyst.

Key words: High-entropy catalysts, Ultra-low doping, CO oxidation, Sintering flue gas, Strong metal and support interaction

赵永奇, 蒋俊杰, 邹洋, 王璞, 李雪, 刘霄龙, 朱廷钰. 超低负载的0.1(PtMnFeCoNi)/TiO₂催化剂: 通过高熵策略调节活性金属位点的电子状态以促进CO的氧化[J]. 催化学报, 2025, 76: 173-184.

Yongqi Zhao, Junjie Jiang, Yang Zou, Pu Wang, Xue Li, Xiaolong Liu, Tingyu Zhu. Ultra-low doping 0.1(PtMnFeCoNi)/TiO₂ catalysts: Modulating the electronic states of active metal sites to enhance CO oxidation through high entropy strategy[J]. Chinese Journal of Catalysis, 2025, 76: 173-184.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64770-X

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Fig. 1. (a) Synthesis process of high-entropy 0.1(PtMnFeCoNi)/TiO2 catalyst. TEM (b) and HRTEM (c) images, SEAD (d) and elemental mapping (e-k) of 0.1(PtMnFeCoNi)/TiO2 catalyst.

Fig. 2. H2-TPR (a), O2-TPD (b), CO-TPR (c), and CO-TPD (d) profiles of the 0.1Pt/TiO2, 0.1(PtM)/TiO2, and 0.1(PtMnFeCoNi)/TiO2 catalysts.

Fig. 3. Ti 2p XPS analysis of the 0.1Pt/TiO2, 0.1(PtM)/TiO2 and 0.1(PtMnFeCoNi)/TiO2 catalyst.

Fig. 4. O 1s XPS analysis of the 0.1Pt/TiO2 (a), 0.1(PtM)/TiO2 (b-e) and 0.1(PtMnFeCoNi)/TiO2 (f) catalyst.

Fig. 5. Pt 4f XPS spectrum analysis of the 0.1Pt/TiO2 (a), 0.1(PtM)/TiO2 (b-e) and 0.1(PtMnFeCoNi)/TiO2 (f) catalyst.

Fig. 6. CO oxidation performance and stability of the catalysts, 0.1Pt/TiO2, 0.1(PtM)/TiO2 and 0.1(PtMnFeCoNi)/TiO2 (a), 0.1(Pt1M4)/TiO2 (b), the stability evaluation (c) at 60000 h-1 and 230 °C.

Fig. 7. In-situ DRIFTs spectra of 0.1Pt/TiO2 and 0.1(PtMnFeCoNi)/TiO2 catalysts. (a,d) Instantaneous changes of 1% CO adsorption for 30 min at 250 °C. (b,e) Instantaneous changes of 1% CO + 16% O2 adsorption for 30 min at 250 °C. (c,f) Changes of CO + O2 surface reaction with temperature.

Fig. 8. Optimized structure and corresponding charge density differences of CO and O2 adsorbed on 0.1Pt/TiO2 (a-d) and 0.1(PtMnFeCoNi)/TiO2 (e-h). (i,j) PDOS profiles of 0.1Pt/TiO2 and 0.1(PtMnFeCoNi)/TiO2.

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超低负载的0.1(PtMnFeCoNi)/TiO₂催化剂: 通过高熵策略调节活性金属位点的电子状态以促进CO的氧化

Ultra-low doping 0.1(PtMnFeCoNi)/TiO₂ catalysts: Modulating the electronic states of active metal sites to enhance CO oxidation through high entropy strategy

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