双位点CuS-Co9S8异质结实现高效选择性甘油电催化氧化

doi:10.1016/S1872-2067(26)65032-2

催化学报 ›› 2026, Vol. 85: 272-285.DOI: 10.1016/S1872-2067(26)65032-2

双位点CuS-Co₉S₈异质结实现高效选择性甘油电催化氧化

李昱伟, 何语馨, 郭宗瑶, 张静怡, 吴义志, 蒋铭坤, 陈诗语, 吴丹()

武汉工程大学材料科学与工程学院, 湖北省等离子体化学与新材料重点实验室, 磷矿及其共伴生资源绿色高效开发利用全国重点实验室, 湖北武汉 430205

收稿日期:2025-11-25 接受日期:2025-12-29 出版日期:2026-06-18 发布日期:2026-05-18
通讯作者: *电子信箱: wudan@wit.edu.cn (吴丹).
基金资助:
国家自然科学基金(22402153);武汉工程大学科学研究基金(K2024006)

Dual-site CuS-Co₉S₈ heterojunctions for efficient and selective glycerol electrooxidation

Yuwei Li, Yuxin He, Zongyao Guo, Jingyi Zhang, Yizhi Wu, Mingkun Jiang, Shiyu Chen, Dan Wu()

State Key Laboratory of Green and Efficient Development of Phosphorus Resources, Hubei Key Laboratory of Plasma Chemistry and New Materials, School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430205, Hubei, China

Received:2025-11-25 Accepted:2025-12-29 Online:2026-06-18 Published:2026-05-18
Contact: *E-mail: wudan@wit.edu.cn (D. Wu).
Supported by:
National Natural Science Foundation of China(22402153);Scientific Research Fund Project of Wuhan Institute of Technology(K2024006)

摘要/Abstract

摘要：

随着全球对可再生能源需求的增长, 生物柴油产业迅速扩张, 导致其主要副产物甘油出现严重的供过于求, 将其转化为低价值的废弃物流, 给生物柴油产业的经济性和环境可持续性带来了巨大挑战. 电催化甘油氧化(GOR)被视为一种极具前景的解决方案, 它能够在阴极产生清洁氢气的同时, 在阳极将甘油转化为甲酸等高附加值化学品. 然而, GOR的实际应用受到核心瓶颈的限制, 即甘油分子与氢氧根离子(OH^-)在催化剂表面存在激烈的竞争吸附. 这种竞争不仅降低了反应效率, 还导致反应中间体浓度失衡, 使得析氧反应(OER)作为副反应占据主导, 严重影响了目标产物的选择性和电流密度. 目前的单金属或传统掺杂催化剂难以在分子水平上精准调控二者吸附平衡. 因此, 开发具有独特吸附特性的新型异质结催化剂, 破解竞争吸附限制并实现高效、高选择性的甘油转化, 对于生物质能源的升级利用具有重要的科学意义和应用价值.

为了解决上述竞争吸附难题, 本文提出了一种基于“双位点协同”的催化剂设计策略, 通过两步水热硫化法在泡沫镍(NF)上成功构建了具有空间和功能解耦特性的CuS-Co₉S₈/NF异质结催化剂. 在该体系中, 利用CuS与Co₉S₈的吸附选择性差异实现了反应物吸附的精准调控: CuS优先吸附甘油分子, 而Co₉S₈则优先吸附OH^-并且作为主要活性位点促进甘油的氧化, 协同平衡表面反应物的浓度, 有效抑制了OER副反应. 实验结果表明, 该CuS-Co₉S₈/NF电极表现出卓越的电催化性能, 仅需1.24 V (vs. RHE)的低电位即可达到200 mA cm^-2的工业级电流密度, 并在1.5 V下实现了对甲酸盐94.8%的高法拉第效率. 原位拉曼光谱、Mott-Schottky分析及密度泛函理论计算揭示了其深层机理: p-n异质结的形成诱导了界面电子重排, 产生内建电场, 电子从n型Co₉S₈转移至p型CuS. 这种电子相互作用不仅稳定了高价钴物种(Co³⁺/Co⁴⁺), 作为高效氧化中心促进C-C键的选择性断裂, 还通过调整d带中心优化了反应中间体的吸附能, 实现了双位点协同催化. 此外, 该催化剂在流动型膜电极组件(MEA)中表现出优异的稳定性, 在200 mA cm^-2电流密度下连续运行超过100 h无明显衰减, 甲酸盐产率高达86.1 kg m^-2. 技术经济分析进一步证实, 该工艺处理每吨甘油具有约775美元的潜在净利润, 显示出极高的商业化潜力.

综上, 本研究开发的高效CuS-Co₉S₈异质结催化剂, 不仅克服了甘油电氧化中长期存在的吸附竞争瓶颈, 实现并验证了高电流密度下的长效稳定运行; 更重要的是, 确立了一种通用的“双位点界面吸附调控”设计原则, 它为解决复杂多元醇电氧化反应中的选择性与活性难题提供了理论指导, 为生物质资源的高值化利用及可再生能源驱动的绿色化工生产开辟了新的技术路径.

关键词: 电催化甘油氧化, 异质结, 硫化作用, 共吸附, 生物质高值化利用

Abstract:

Electrocatalytic oxidation of surplus glycerol from biodiesel production is fundamentally limited by the competitive adsorption of glycerol and OH^- ions on catalyst surfaces. To overcome this challenge, a CuS-Co₉S₈ heterojunction was fabricated via a two-step hydrothermal sulfidation method. This catalyst features spatially and functionally decoupled active sites, in which CuS domains preferentially adsorbs glycerol and Co₉S₈ promotes OH^- activation, thereby balancing surface reactant concentrations and suppressing oxygen evolution side reactions. In-situ Raman spectroscopy and theoretical calculations reveal that interfacial electron redistribution stabilizes high-valent cobalt species and enables dual-site cooperative reactivity. The resulting electrode delivers an industrially relevant current density of 200 mA cm^-2 at a low potential of 1.24 V (vs. RHE) with a Faradaic efficiency of 94.8% for formate at 1.5 V. In a flow-type membrane electrode assembly, stable operation over 100 h at 200 mA cm^-2 is achieved, yielding a formate production rate of ’86.1 kg m^-2. Techno-economic analysis indicates a net profit potential of ’$775 per ton of glycerol processed. This study establishes a general dual-site design principle for overcoming adsorption competition in polyol electrooxidation, offering a scalable pathway for efficient biomass valorization.

Key words: Electrocatalytic glycerol oxidation, Heterojunction, Sulfurization, Co-adsorption, Biomass valorization

李昱伟, 何语馨, 郭宗瑶, 张静怡, 吴义志, 蒋铭坤, 陈诗语, 吴丹. 双位点CuS-Co₉S₈异质结实现高效选择性甘油电催化氧化[J]. 催化学报, 2026, 85: 272-285.

Yuwei Li, Yuxin He, Zongyao Guo, Jingyi Zhang, Yizhi Wu, Mingkun Jiang, Shiyu Chen, Dan Wu. Dual-site CuS-Co₉S₈ heterojunctions for efficient and selective glycerol electrooxidation[J]. Chinese Journal of Catalysis, 2026, 85: 272-285.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65032-2

https://www.cjcatal.com/CN/Y2026/V85/I6/272

图/表 8

Fig. 1. (a) Schematic illustration of the CuS-Co9S8/NF electrode preparation process. XRD pattern (b), SEM images (c-e), STEM-EDS elemental mappings (f), TEM images (g,h), and Mott-Schottky plots (i) of the CuS-Co9S8/NF electrode.

Fig. 2. FTIR spectrum (a) and Raman spectra (b) of CuS-Co9S8/NF. XPS spectra of Co 2p for CuS-Co9S8/NF and Co9S8/NF (c), Cu 2p for CuS-Co9S8/NF and CuS/NF (d). (e) Cu LMM Auger spectra for CuS-Co9S8/NF and CuS/NF. (f) XPS spectra of S 2p for CuS-Co9S8/NF, CuS/NF, and Co9S8/NF.

Fig. 3. Electrochemical GOR performance of different electrodes. LSV curves (a), potentials at different current densities (b), comparison of catalyst performance (c, d), Tafel plots (e), Cdl fitting plots (f), and FEs (g) of formic acid for CuS/NF, Co9S8/NF, and CuS-Co9S8/NF electrodes in 1 mol L-1 KOH + 0.1 mol L-1 glycerol. Stability test at 1.5 V with FEs of GOR products (h) and glycerol conversion and formic acid yield (i) for the CuS-Co9S8/NF electrode.

Fig. 4. (a) CV curves of CuS-Co9S8/NF in 1 mol L-1 KOH and 1 mol L-1 KOH + 0.1 mol L-1 glycerol electrolytes. (b) DPV curves of CuS-Co9S8/NF and Co9S8/NF in 1 mol L-1 KOH. (c,d) Multi-step potential tests on CuS-Co9S8/NF. FEs of oxidation products in 1 mol L-1 KOH + 0.1 mol L-1 glyceraldehyde (e), 1 mol L-1 KOH + 0.1 mol L-1 glycolic acid (f), and 1 mol L-1 KOH + 0.1 mol L-1 glycerol (g) at 1.45 V under different pH values. (h) Proposed GOR pathway over the CuS-Co9S8/NF electrode. In-situ Raman spectra measured at different anodic potentials in 1 mol L-1 KOH (i) and 1 mol L-1 KOH + 0.1 mol L-1 glycerol (j) on CuS-Co9S8/NF.

Fig. 5. In-situ Bode plots of CuS-Co9S8/NF (a), CuS /NF (b), and Co9S8/NF (c) electrodes under different potentials in 1 mol L-1 KOH + 0.1 glycerol. (d) Equivalent circuit model representing interfacial processes during GOR. (e) Potential-dependent Rct. (f) Inductive impedance in the mid-frequency region. (g) OCP responses of the three electrodes in 1 mol L-1 KOH before (left) and after (right) 0.1 mol L-1 glycerol injection.

Fig. 6. LSV curves of Co9S8 (a), CuS (b), and CuS-Co9S8 (c) in 0.1 mol L-1 glycerol with different KOH concentrations (Inset: GOR current density at 1.4 V as a function of cKOH. LSV curves of Co9S8 (d), CuS (f), and CuS-Co9S8 (g) in 1 mol L-1 KOH with different glycerol concentrations (Inset: GOR current density at 1.4 V as a function of cglycerol. Apparent redox rate constants (Ks) in 1 mol L-1 KOH with (g) and without (h) 0.1 mol L-1 glycerol.

Fig. 7. Adsorption energies of glycerol (a) and OH- (b) on Co9S8/NF, CuS/NF, and CuS-Co9S8/NF. (c) DOS profiles of three electrodes.

Fig. 8. (a) Schematic illustration of the MEA device. (b) LSV curves comparing OER‖HER and GOR‖HER configurations using CuS-Co9S8/NF as the anode. (c) Stability test of the GOR‖HER electrolyzer at 200 mA cm-2. (d) FEs and yield of formate as a function of time. (e,f) TEA of the proposed electro-upcycling strategy for glycerol valorization.

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双位点CuS-Co₉S₈异质结实现高效选择性甘油电催化氧化

Dual-site CuS-Co₉S₈ heterojunctions for efficient and selective glycerol electrooxidation

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