理论和实验相结合研究NiCo2O4纳米片用于甘油电氧化反应机制

doi:10.1016/S1872-2067(23)64585-1

催化学报 ›› 2024, Vol. 57: 68-79.DOI: 10.1016/S1872-2067(23)64585-1

理论和实验相结合研究NiCo₂O₄纳米片用于甘油电氧化反应机制

段妍^a^,^c^,¹, 薛米风^b^,¹, 刘彬^a, 张曼^a, 王宇辰^a, 王宝俊^b, 章日光^b^,^*(), 严凯^a^,^*()

^a中山大学环境科学与工程学院, 广东省环境污染控制与修复技术重点实验室, 广东广州 510275
^b太原理工大学化学工程与技术学院, 煤炭清洁高效利用国家重点实验室, 山西太原 030024
^c广东工业大学环境科学与工程学院, 广东广州 510006

收稿日期:2023-11-01 接受日期:2023-12-20 出版日期:2024-02-18 发布日期:2024-02-10
通讯作者: * 电子信箱: zhangriguang@tyut.edu.cn (章日光),yank9@mail.sysu.edu.cn (严凯).
作者简介:¹共同第一作者.
基金资助:
国家重点研发计划(2023YFC3905804);广州市科技计划项目(202206010145);国家自然科学基金项目(22078374);国家自然科学基金项目(22378434);广东省科技计划项目(2021B1212040008);广东省岭南现代农业重点实验室项目(NT2021010)

Integration of theory prediction and experimental electrooxidation of glycerol on NiCo₂O₄ nanosheets

Yan Duan^a^,^c^,¹, Mifeng Xue^b^,¹, Bin Liu^a, Man Zhang^a, Yuchen Wang^a, Baojun Wang^b, Riguang Zhang^b^,^*(), Kai Yan^a^,^*()

^aGuangdong Provincial Key Laboratory of Environmental Pollution Control and Remediation Technology, School of Environmental Science and Engineering, Sun Yat-sen University, Guangzhou 510275, Guangdong, China
^bState Key Laboratory of Clean and Efficient Coal Utilization, College of Chemical Engineering and Technology, Taiyuan University of Technology, Taiyuan 030024, Shanxi, China
^cSchool of Environmental Science and Engineering, Guangdong University of Technology, Guangzhou 510006, Guangdong, China

Received:2023-11-01 Accepted:2023-12-20 Online:2024-02-18 Published:2024-02-10
Contact: * E-mail: zhangriguang@tyut.edu.cn (R. Zhang), yank9@mail.sysu.edu.cn (K. Yan).
About author:¹ Contributed to this work equally.
Supported by:
National Key R&D Program of China(2023YFC3905804);Scientific and Technological Planning Project of Guangzhou(202206010145);National Natural Science Foundation of China(22078374);National Natural Science Foundation of China(22378434);Science and Technology Planning Project of Guangdong Province, China(2021B1212040008);Guangdong Laboratory for Lingnan Modern Agriculture Project(NT2021010)

摘要/Abstract

摘要：

甘油是生物质精炼的主要副产物(约占10%), 年过剩量与低利用率导致其市场价格(0.24-0.6 US kg^-1)较低. 甘油是具有三个活性羟基的多元醇, 被认为是生产高价值产品的理想原料. 甲酸作为甘油转化最重要的产品之一, 广泛应用于农药、皮革、染料和医药行业, 将甘油电氧化(EGOR)为甲酸(FA)不仅能有效避免资源过剩造成浪费, 而且能满足未来对甲酸燃料电池的需求. 然而甘油电催化氧化途径较为复杂, 涉及反应中间产物的脱氢、吸附/解吸和C-C键裂解.

本文将密度泛函理论(DFT)与实验相结合, 研究了在精细构建的NiCo₂O₄纳米片上通过EGOR生产FA的反应机制. DFT计算结果表明, 活性羟基(OH*)物种可以改变EGOR生产FA过程的决速步骤(RDS), 通过调节吸附中间体的吸附能可获得理想的FA产率. 其中, 高度羟基化的NiCo₂O₄纳米片(311)-OH*晶面上具有最低的吉布斯自由能, 能显著提升反应过程动力学. 在理论分析的基础上, 通过简易的电沉积方法精准制备了超薄NiCo₂O₄纳米片 (~1.7 nm), 并采用X射线吸收精细结构谱和高分辨透射电镜对催化剂进行了结构分析. 结果表明, NiCo₂O₄纳米片中四面体(A_Td)和八面体(B_Oh)配位具有内角共享的A_Td-O-B_Oh和边共享的B_Oh-O-B_Oh构型, 金属间的协同作用有效改善了材料的电子效应, 有利于提供更多的吸附位点并促进EGOR过程中的电荷转移. NiCo₂O₄纳米片在EGOR中的电荷转移电阻仅为0.94 Ω, 电化学活性表面积高达10.25 cm². 相比较电催化析氧反应, NiCo₂O₄纳米片表现出了较好的EGOR性能, 在10 mA cm^-2的电流密度下阳极功耗降低了320 mV, 在100 mA cm^-2的电流密度时的阳极电势仅为1.46 V_RHE. 此外, 在120 h的稳定性测试中, 甘油的转化率和FA的选择性可分别保持在89%和70%. 多电位步骤实验、原位电化学阻抗谱和电子顺磁共振谱结果表明, NiCo₂O₄纳米片上原位产生的OH*物种是EGOR过程中的直接活性中心, 有利于将RDS从甘油酸脱氢裂解转化为甘油醛的脱氢步骤, 并进一步促进C-C键的裂解. 进一步结合理论预测, 证实了OH*物种是EGOR过程中的直接活性中心.

综上, 采用绿色高效的电催化手段促进甘油生产高附加值化学品是生物质链升级的重要举措, 有效避免了传统的高温高压, 以水为介质, 原位利用OH*. 本文为新型催化剂的未来设计和理解生物质基原料电氧化升级反应机制提供了新思路.

关键词: 密度泛函理论预测, 活性羟基, 电化学氧化, 甘油, NiCo₂O₄纳米片

Abstract:

Electrocatalytic refinery of low-value biomass-based glycerol into value-added chemicals formic acid (FA) is an attractive alternative to traditional thermochemical refineries. However, constructing non-precious catalysts with abundant active hydroxyl (OH*) is the main obstacle to the electrocatalytic glycerol oxidation reaction (EGOR). Herein, we combine density functional theory (DFT) and experiments to investigate EGOR over the finely constructed NiCo₂O₄ nanosheets. DFT results firstly indicate that the NiCo₂O₄ nanosheets exhibit the highly hydroxylated (311)-OH* surface with the lowest Gibbs free energy, which significantly improves the electrochemical reaction kinetics and can achieve desirable FA yield by adjusting the adsorption energy of the adsorption intermediate. Following the theoretical prediction, ultrathin NiCo₂O₄ nanosheets (~1.70 nm) are fabricated by a facile electrodeposition method with sufficient OH* on the surface. The charge-transfer resistance of NiCo₂O₄ nanosheets in EGOR is only 0.94 Ω and the anode power consumption can be reduced by up to 320 mV at 10 mA cm^-2, keeping the high glycerol conversion (89%) and FA selectivity (70%) during the 120-h stability test. DFT calculations and experimental tools (e.g., multi-potential step experiments, operational electrochemical impedance spectroscopy) confirm that OH* in-situ generated on the thin nanosheets structure is essential in facilitating charge transfer between catalysts and adsorbed molecules to enhance C-C bond cleavage. This work offers a guideline for the rational design of robust catalysts for the selective upgrading of biomass-derived chemicals.

Key words: Density functional theory prediction, active hydroxyl, Electrochemical oxidation, Glycerol, NiCo₂O₄ nanosheets

段妍, 薛米风, 刘彬, 张曼, 王宇辰, 王宝俊, 章日光, 严凯. 理论和实验相结合研究NiCo₂O₄纳米片用于甘油电氧化反应机制[J]. 催化学报, 2024, 57: 68-79.

Yan Duan, Mifeng Xue, Bin Liu, Man Zhang, Yuchen Wang, Baojun Wang, Riguang Zhang, Kai Yan. Integration of theory prediction and experimental electrooxidation of glycerol on NiCo₂O₄ nanosheets[J]. Chinese Journal of Catalysis, 2024, 57: 68-79.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64585-1

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Fig. 1. (a) The top view and side views of NiCo2O4 (220) and NiCo2O4 (311) surface. (b) Gibbs free-energy diagram of the EGOR process over NiCo2O4 (220) and NiCo2O4 (311) surfaces and the corresponding structures are shown in Fig. S3. The Gibbs free-energy diagram of the EGOR and OER processes over NiCo2O4 (311) (c) and NiCo2O4 (311)-OH* (d) surface and the corresponding structure of intermediates are shown in Figs. S4 and S5.

Fig. 2. Synthesis process and morphological characterization of NiCo2O4 catalyst: (a) Schematic diagram; (b) SEM; (c) the corresponding EDX mapping; (d) AFM; (e) TEM; (f) HR-TEM; (g) SAED.

Fig. 3. Internal atomic structure analysis of NiCo2O4 nanosheets catalyst: XPS spectra of Ni 2p (a) and Co 2p (b). XANES spectra of Ni K-edge (c) and Co K-edge (d). Fourier-transformed EXAFS spectra of Ni R-space (e) and Co R-space (f). (g) Wavelet-EXAFS maps of the Ni atom environment with the standard substrate of NiO and the Co atom environment with the standard substrate of Co2O3, deeper color meant greater intensity.

Fig. 4. Electrochemical characterization analysis of NiCo2O4 nanosheets electrode: (a) Comparison of the LSV curves without (OER) and within (EGOR) 0.1 mol L-1 glycerol in 1.0 mol L-1 KOH solution at a scan rate of 5 mV s?1 with 60% iR-corrected. (b) The corresponding Tafel slope. (c) Nyquist plots of impedances. (d) The comparison of electric double layer capacitance (Cdl) values corresponding to CV curves with different scan rates (2-20 mV s-1) in OER and EGOR. (e) Ring current on an RRDE at the ring potential of 0.40 VRHE in OER and EGOR. Hold 200 s at 0 μA current and 200 s at 200 μA current. (f) The comparison at 10 mA cm-2 between this work and previously reported data.

Fig. 5. Products analysis and cycle stability testing. (a) The evolution of product concentration and glycerol conversion as a function of electrolysis time at 1.42 VRHE in 0.1 mol L-1 glycerol-KOH mixture. (b) The selectivity of different products after electrolyzing as a function of electrolysis time and the overall Faradaic efficiency. (c) Stability test for EGOR at the potential of 1.42 VRHE for 5 cycles. After each test, replace the electrode surface with deionized water and a new electrolyte (0.1 mol L-1 glycerol-KOH mixture). (d) Glycerol conversion rate and overall Faradaic efficiency of each cycle test.

Fig. 6. Mechanism analysis. (a) Multi-potential step experimental results. (b) EPR spectroscopic analysis of NiCo2O4 nanosheets electrode in 0 and 0.1 mol L-1 glycerol-KOH mixture at 1.42 VRHE. Bode plots of OER (c) and EGOR (d). (e) The scheme of the relationship between structure-activity-potential.

Fig. 7. Schematic diagram of the main reaction pathways for glycerol oxidation to FA on a simplified model of NiCo2O4.

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理论和实验相结合研究NiCo₂O₄纳米片用于甘油电氧化反应机制

Integration of theory prediction and experimental electrooxidation of glycerol on NiCo₂O₄ nanosheets

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