Mn掺杂调控NiCo LDH活性位点用于H2O2与甲酸盐的节能耦合电合成

doi:10.1016/S1872-2067(26)65137-6

催化学报 ›› 2026, Vol. 88: 307-321.DOI: 10.1016/S1872-2067(26)65137-6

Mn掺杂调控NiCo LDH活性位点用于H₂O₂与甲酸盐的节能耦合电合成

张家雨^a, 王昆^a^,^*(), 于晶露^a, 徐凯洋^a^,^b, 杨璐^a, 饶佳丽^a, 宋树芹^a^,^*(), 王毅^a^,^*()

^a 中山大学化学工程与技术学院、材料科学与工程学院, 广东省低碳化学与过程节能重点实验室, 聚合物复合材料及功能材料教育部重点实验室(PCFM Lab), 广东珠海 519082
^b 松山湖材料实验室, 广东东莞 523429

收稿日期:2026-04-29 接受日期:2026-05-14 出版日期:2026-09-18 发布日期:2026-09-05
通讯作者: *电子信箱: wangk269@mail.sysu.edu.cn (王昆),
stsssq@mail.sysu.edu.cn (宋树芹),
wangyi76@mail.sysu.edu.cn (王毅).
基金资助:
榆林清洁能源创新研究院能源革命科技项目(E511030817);国家自然科学基金(22478450);国家自然科学基金(22478451);国家自然科学基金(22408408);催化基础国家重点实验室(2024SKL-A-013);广东省基础与应用基础研究基金(2024A1515012565);中山大学引进人才启动基金(76110-12256023)

Modulating active sites via Mn-doping in NiCo LDH for energy-saving paired electrosynthesis of H₂O₂ and formate

Jiayu Zhang^a, Kun Wang^a^,^*(), Jinglu Yu^a, Kaiyang Xu^a^,^b, Lu Yang^a, Jiali Rao^a, Shuqin Song^a^,^*(), Yi Wang^a^,^*()

^a The Key Laboratory of Low-Carbon Chemistry & Energy Conservation of Guangdong Province, PCFM Lab, School of Chemical Engineering and Technology, School of Materials Science and Engineering, Sun Yat-sen University, Zhuhai 519082, Guangdong, China
^b Songshan Lake Materials Laboratory (SLAB), Dongguan 523429, Guangdong, China

Received:2026-04-29 Accepted:2026-05-14 Online:2026-09-18 Published:2026-09-05
Supported by:
The Energy Revolution S&T Program of Yulin Innovation Institute of Clean Energy(E511030817);The National Natural Science Foundation of China(22478450);The National Natural Science Foundation of China(22478451);The National Natural Science Foundation of China(22408408);The National State Key Laboratory of Catalysis(2024SKL-A-013);The Guangdong Basic and Applied Basic Research Foundation(2024A1515012565);The Startup Fund for Recruited Talents of Sun Yat-sen University(76110-12256023)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)作为一种重要的绿色氧化剂, 其传统蒽醌生产工艺存在能耗高、流程繁琐及环境风险高等缺点. 基于两电子氧还原反应(2e^- ORR)的电化学合成技术, 可在温和条件下实现H₂O₂的绿色制备, 被视为理想替代方案. 然而, 在传统H₂O₂电合成体系中, 阴极2e^- ORR通常与阳极析氧反应(OER)配对. 受OER动力学迟缓、过电位高以及阳极产物O₂附加值较低等因素限制, 该体系整体能耗偏高、经济性不足, 严重制约了H₂O₂电合成技术的产业化应用. 针对上述问题, 本文提出以甲醇氧化反应(MOR)替代OER的耦合电解策略, 旨在降低系统能耗的同时, 联产高附加值甲酸盐.
为提升MOR催化性能(尤其降低其起始电位), 本文以泡沫镍为基底, 通过一步水热法原位制备了镍钴层状双氢氧化物(NiCo LDH)及不同锰掺杂量的Mn-NiCo LDH电极. X-射线衍射、透射电镜及X-射线光电子能谱等结果表明, 成功合成了Ni_0.61Co_0.39 LDH和一系列Mn-NiCo LDH电极. 电化学测试结果表明, 适量Mn掺杂可显著优化MOR动力学, 其中Ni_0.50Co_0.30Mn_0.20 LDH性能最优, 表现出优异的催化活性、选择性与稳定性: 在10 mA cm^-2下, 其MOR电位低至1.32 V_RHE, 优于未掺杂的Ni_0.61Co_0.39 LDH (1.37 V_RHE); 在100 mA cm^-2下可稳定运行超24 h, 工作电位仅1.38 V_RHE, 且甲酸盐法拉第效率高达92.92%. 结合原位拉曼光谱与密度泛函理论(DFT)计算阐明了Mn掺杂的催化增强机制. 原位拉曼结果显示, Mn掺杂使Ni³⁺-O特征峰出现电位负移, 促进了高活性Ni³⁺/NiOOH物种在更低电位下的生成. DFT计算进一步证实, Mn掺杂显著降低了Ni初始氧化的吉布斯自由能(从1.76降至0.97 eV)和MOR决速步能垒(从6.63降至3.45 eV). 综上, Mn掺杂通过促进活性Ni³⁺物种生成并优化局域电子结构, 加速了MOR的关键步骤, 从而显著提升了反应动力学. 将Ni_0.50Co_0.30Mn_0.20 LDH@NF作为阳极, 碳纳米管修饰的碳纸(CNTs@CP)作为阴极, 构建2e^- ORR||MOR耦合体系. 与传统2e^- ORR||OER体系相比, 该耦合体系在50 mA cm^-2电流密度时槽压降低了254 mV, H₂O₂合成的能耗降低10.3%, 净经济效益提升97.9%. 上述结果充分验证了以MOR替代OER在节能降耗与阳极产物增值方面的显著优势.
综上, 本研究不仅为高效MOR催化材料的设计提供了新思路, 也为构建兼具低能耗与高附加值联产特性的H₂O₂电合成耦合体系提供了坚实的理论与实践基础.

关键词: 过氧化氢电合成, 甲醇氧化反应, 耦合电解, 低能耗

Abstract:

Electrochemical H₂O₂ synthesis via the two-electron oxygen reduction reaction (2e^- ORR) offers a green alternative to the energy-intensive anthraquinone process, but its practical viability is hindered by the sluggish and low-value oxygen evolution reaction (OER) at the anode. Here, we present an energy-saving paired electrolysis strategy that replaces anodic OER with methanol oxidation reaction (MOR) using a ternary Mn-doped NiCo layered double hydroxide (Ni_0.50Co_0.30Mn_0.20 LDH) catalyst in situ grown on nickel foam (NF) by a one-step hydrothermal method. The optimized catalyst achieves a low MOR potential of 1.32 V_RHE at 10 mA cm^-2 and a formate Faradaic efficiency of 92.9%, outperforming its undoped counterpart (Ni_0.61Co_0.39 LDH, 1.37 V_RHE and 83.3%). In-situ Raman spectroscopy and density functional theory calculations reveal that Mn doping lowers the energy barrier for the Ni²⁺/Ni³⁺ redox transition, facilitating the generation of catalytically active Ni³⁺ species. When coupled with graphitized hydroxyl-functionalized multi-walled carbon nanotubes coated on carbon paper (CNTs@CP) as the 2e^- ORR cathode in a two-electrode electrolyzer, at the operation condition of 50 mA cm^-2, the 2e^- ORR||MOR system delivers a cell voltage reduction of 254 mV, enabling a 10.3% decrease in energy consumption for H₂O₂ production, compared with the conventional 2e^- ORR||OER system. Moreover, the simultaneous generation of value-added formate at the anode yields a 97.9% increase in net economic benefit. This work establishes a generalizable paired electrolysis paradigm for the decentralized, energy-efficient, and economically viable co-production of H₂O₂ and high-value chemicals.

Key words: Hydrogen peroxide electrosynthesis, Methanol oxidation reaction, Coupled electrolysis, Low energy

张家雨, 王昆, 于晶露, 徐凯洋, 杨璐, 饶佳丽, 宋树芹, 王毅. Mn掺杂调控NiCo LDH活性位点用于H₂O₂与甲酸盐的节能耦合电合成[J]. 催化学报, 2026, 88: 307-321.

Jiayu Zhang, Kun Wang, Jinglu Yu, Kaiyang Xu, Lu Yang, Jiali Rao, Shuqin Song, Yi Wang. Modulating active sites via Mn-doping in NiCo LDH for energy-saving paired electrosynthesis of H₂O₂ and formate[J]. Chinese Journal of Catalysis, 2026, 88: 307-321.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65137-6

https://www.cjcatal.com/CN/Y2026/V88/I9/307

图/表 7

Fig. 1. Schematic illustration of the conventional anthraquinone process (a), the conventional electrochemical system for H2O2 synthesis (b), and the coupled electrochemical system for co-producing H2O2 and formate in this work (c).

Fig. 2. (a) Synthesis process of Ni0.61Co0.39 LDH and Mn-NiCo LDH. (b) XRD patterns of Ni0.61Co0.39 LDH and Mn-NiCo LDH powders. (c-e) XPS spectra of Ni0.50Co0.30Mn0.20 LDH for Ni 2p (c), Co 2p (d) and Mn 2p (e). (f) SEM image of Ni0.50Co0.30Mn0.20 LDH. (g) HR-TEM image of Ni0.50Co0.30Mn0.20 LDH. (h) HAADF-STEM image and corresponding elemental mappings of Ni0.50Co0.30Mn0.20 LDH.

Fig. 3. (a) LSV curves of Ni0.61Co0.39 LDH and Mn-NiCo LDH series in 1.0 mol L-1 KOH + 1.0 mol L-1 CH3OH. (b) EIS of Ni0.61Co0.39 LDH and Mn-NiCo LDH series in 1.0 mol L-1 KOH + 1.0 mol L-1 CH3OH. (c,d) LSV curves and Tafel plots of Ni0.61Co0.39 LDH and Ni0.50Co0.30Mn0.20 LDH in 1.0 mol L-1 KOH with and without 1.0 mol L-1 CH3OH. (e) Cdl of Ni0.61Co0.39 LDH and Ni0.50Co0.30Mn0.20 LDH in 1.0 mol L-1 KOH. (f) Constant current measurement of Ni0.61Co0.39 LDH and Ni0.50Co0.30Mn0.20 LDH in 1.0 mol L-1 KOH + 1.0 mol L-1 CH3OH. (g) FE of formate for Ni0.61Co0.39 LDH and Ni0.50Co0.30Mn0.20 LDH with different cumulative times at 100 mA cm-2. (h) Comparison of MOR activities of various catalysts in 1.0 mol L-1 KOH + 1.0 mol L-1 CH3OH.

Fig. 4. (a) Schematic illustration of in-situ Raman spectroscopy setup. (b,c) 2D in-situ Raman spectra of Ni0.61Co0.39 LDH and Ni0.50Co0.30Mn0.20 LDH at different potentials in 1.0 mol L-1 KOH. (d,e) Corresponding in-situ Raman spectra for both catalysts at various potentials in 1.0 mol L-1 KOH. (f, g) In-situ Raman spectra for both catalysts at various potentials in 1.0 mol L-1 KOH + 1.0 mol L-1 CH3OH. (h) Multi-potential step curves of Ni0.50Co0.30Mn0.20 LDH in 1.0 mol L-1 KOH with or without 1.0 mol L-1 CH3OH.

Fig. 5. (a) Schematic illustration of the Ni2+ to Ni3+ transformation coupled with CH3OH adsorption at Ni sites, where Ni: gray, Co: blue, Mn: purple, O: red, H: white, C: brown. (b) Gibbs free energy diagram for the catalytic MOR process on Ni0.61Co0.39 LDH and Ni0.50Co0.30Mn0.20 LDH, respectively. (c) PDOS of Ni-3d electrons calculated for Ni0.61Co0.39 LDH and Ni0.50Co0.30Mn0.20 LDH. (d) Differential charge density plot of CH3OH adsorbed on Ni0.50Co0.30Mn0.20 LDH, blue and yellow represent electron depletion and accumulation.

Fig. 6. (a) Schematic illustration of the two-electrode 2e- ORR||MOR system. (b) LSV curves of 2e- ORR||MOR and conventional 2e- ORR||OER electrolyzers. (c) H2O2 production rate. (d) Faradaic efficiency of H2O2. (e) Energy consumption per mol of H2O2 produced. (f) Formate production rate in the 2e- ORR||MOR system. (g) Faradaic efficiency of formate. (h) Comparison of hourly net economic benefit between the 2e- ORR||MOR and 2e- ORR||OER systems.

Fig. 7. (a) Schematic illustration of the 2e- ORR||MOR electrolysis system in the flow cell. (b) Schematic illustration of the flow-cell device for the 2e- ORR||MOR electrolysis system. (c) LSV curves of 2e- ORR||MOR and conventional 2e- ORR||OER electrolysis in the flow cell. (d) Comparison of cell voltage and current density between this work and previous H2O2 electrosynthesis systems. (e) Stability test of the 2e- ORR||MOR electrolysis system in the flow cell.

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Mn掺杂调控NiCo LDH活性位点用于H₂O₂与甲酸盐的节能耦合电合成

Modulating active sites via Mn-doping in NiCo LDH for energy-saving paired electrosynthesis of H₂O₂ and formate

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