用于氨电氧化反应生成硝酸盐/亚硝酸盐的金属基电催化剂：过去、现在和未来

doi:10.1016/S1872-2067(23)64576-0

催化学报 ›› 2024, Vol. 56: 25-50.DOI: 10.1016/S1872-2067(23)64576-0

用于氨电氧化反应生成硝酸盐/亚硝酸盐的金属基电催化剂：过去、现在和未来

田芸睿^a, 谭皓天^a, 李霞^a, 贾晶晶^a, 毛子贤^a, 刘健^b, 梁骥^a^,^*()

^a天津大学材料科学与工程学院, 先进陶瓷与机械加工技术教育部重点实验室, 天津300350
^b内蒙古大学化学化工学院, 内蒙古呼和浩特010021

收稿日期:2023-08-29 接受日期:2023-11-24 出版日期:2024-01-18 发布日期:2024-01-10
通讯作者: *电子信箱: liangji@tju.edu.cn (梁骥).
基金资助:
国家自然科学基金(22179093);国家自然科学基金(21905202)

Metal-based electrocatalysts for ammonia electro-oxidation reaction to nitrate/nitrite: Past, present, and future

Yunrui Tian^a, Haotian Tan^a, Xia Li^a, Jingjing Jia^a, Zixian Mao^a, Jian Liu^b, Ji Liang^a^,^*()

^aKey Laboratory of Advanced Ceramics and Machining Technology, Ministry of Education, School of Materials Science and Engineering, Tianjin University, Tianjin 300350, China
^bCollege of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021, Inner Mongolia, China

Received:2023-08-29 Accepted:2023-11-24 Online:2024-01-18 Published:2024-01-10
About author:Prof. Ji Liang received his Ph.D. degree from the University of Adelaide in 2014. After a T. S. Ke Fellowship and an ARC DECRA fellowship, he joined the School of Materials Science and Engineering, Tianjin University. His research interests are the design of functional carbon-based materials for electrochemical catalysis and energy storage applications.
Supported by:
National Natural Science Foundation of China(22179093);National Natural Science Foundation of China(21905202)

摘要/Abstract

摘要：

亚硝酸盐和硝酸盐(统称为NO_2/3⁻)是工业、农业和食品工程中的重要物质. 目前通过Ostwald氧化法制备亚硝酸盐和硝酸盐过程常常伴随着大量的能源消耗和温室气体排放. 氨的电催化氧化是一种低排放和节能的低温工艺过程, 可以持续生产NO_2/3⁻, 避免了有害的N₂O的形成, 并且可以完全由可再生电力供电. 目前对氨氧化反应的研究大多集中在氨裂解制氢和直接氨燃料电池上, 而对氨转化为NO_2/3⁻的研究关注较少. 因此, 本文在总结近年来氨电催化工作的基础上, 对催化剂的反应机理和设计思路进行了综述.

本文从电催化氨氧化反应(AOR)可能的反应机理入手, 介绍了AOR的反应条件、检测方法、原位表征方法以及理论计算的研究成果, 在总结了影响AOR催化剂催化性能因素的基础上提出了近年来电催化剂的设计策略以及合成方法, 并对未来氨领域的发展提出展望. 首先, 基于反应原理以及反应中间体的吸附路径等方面讨论了AOR的关键难点. 然后, 系统性总结了AOR的测试要求以及原位拉曼、原位红外、原位电化学质谱和原位X射线吸收光谱等技术在AOR机理研究中的重要作用, 讨论了密度泛函理论对于研究AOR催化过程中的反应能垒和催化剂电子轨道分布的贡献. 催化剂合金设计、界面工程、非晶化处理、单原子或双原子调制等可控策略有助于抑制副反应的进行以及电解过程中产生的腐蚀性物质对电极的破坏. 最后, 介绍了氨氧化在光、热以及生物催化领域的应用进展, 提出了当前AOR所面临的挑战和解决策略, 如将先进的材料设计与理论计算相结合, 有助于寻找新的高性能AOR电催化剂. 催化体系的改进和反应器的优化将加速大规模绿色、高效、低能耗电催化制备NO_2/3⁻的产业化.

综上所述, AOR领域取得的进展说明氨电氧化制备NO_2/3⁻用于工业生产具有可行性, 这为满足不断增长的NO_2/3⁻供应需求带来了新的机遇. 尽管AOR仍面临性能不高、工艺不成熟等难题, 但随着理论与实验研究的结合, 原位表征技术不断地开发利用, 未来高效、稳定的AOR催化剂会不断的出现. 本文也为生成NO_2/3⁻的催化剂的研发提供理论参考.

关键词: 氨氧化反应, 硝酸盐, 亚硝酸盐, 非贵金属催化剂, 氨

Abstract:

abstract: Electrocatalytic oxidation of ammonia is an appealing, low-temperature process for the sustainable production of nitrites/nitrates that avoids the formation of pernicious N₂O and can be fully powered by renewable electricity. However, the number of known efficient catalysts for this purpose is limited. In this review, based on the possible reaction mechanism of electrocatalytic ammonia oxidation reaction (AOR), the control of catalyst performance by hybrid composite design, microstructure construction, and surface modification is reviewed, and the prospects of AOR catalysts for photocatalysis, thermocatalysis, and biocatalysis are proposed. Notably, a rational and rigorous AOR experimental protocol is suggested. We hope that the research community will jointly focus on the sensible testing of AOR products and eventually develop a more realistic evaluation system. Finally, a techno-economic analysis of AOR electrocatalysis was carried out, and a more economical carbon-free cycle system based on the AOR process was proposed.

Key words: Ammonia oxidation reaction, Nitrite, Nitrate, Non-noble metal catalyst, Ammonia

田芸睿, 谭皓天, 李霞, 贾晶晶, 毛子贤, 刘健, 梁骥. 用于氨电氧化反应生成硝酸盐/亚硝酸盐的金属基电催化剂：过去、现在和未来[J]. 催化学报, 2024, 56: 25-50.

Yunrui Tian, Haotian Tan, Xia Li, Jingjing Jia, Zixian Mao, Jian Liu, Ji Liang. Metal-based electrocatalysts for ammonia electro-oxidation reaction to nitrate/nitrite: Past, present, and future[J]. Chinese Journal of Catalysis, 2024, 56: 25-50.

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图/表 37

Fig. 1. The first-generation nitrate synthesis pathway (B-E process).

Fig. 2. The second-generation NO2/3? synthesis pathway: Ostwald process (a) and AOR process (b).

Fig. 3. The progress of AOR-NO2/3? mechanism.

Fig. 4. Design solutions for non-precious metal-based AOR catalysts.

Fig. 5. Ammonia oxidation upon O-S (a) and G-M (b) mechanism.

Fig. 6. Ammonia oxidation for the preparation of NO2- (a) and NO3- (b) mechanisms.

Fig. 7. (a) Schematic illustration of the AOR reaction mechanism. CV measurement with 1 mol L?1 KOH (b) and 1 mol L?1 KOH + 0.5 mol L?1 NH4OH (c) electrolyte. Schematic representation of two proposed pathways for the copper-catalyzed AOR. Reprinted with permission from Ref. [32]. Copyright 2023, Elsevier Ltd.

Fig. 8. (a) Homogeneous electrocatalytic (mediated) oxidation, where the primary product is NO2-. (b) Direct heterogeneous electrocatalytic oxidation of NH3, where the primary product is NO3-. Reprinted with permission from Ref. [2]. Copyright 2021, Wiley-VCH.

Fig. 9. The proposed scheme strictly measures electrocatalytic AOR.

Fig. 11. Top: Free energy diagrams of NO3? formation from ammonia via Nads (a) and NHOHads (b) intermediates at equilibrium (red trace) and limiting (blue trace) potentials computed using the computational hydrogen electrode at pH 11. (c) Bottom, top and side views of the lowest energy configurations for AOR intermediates in the path toward NO3?; Reprinted with permission from Ref. [46]. Copyright 2021, Wiley-VCH.

Fig. 12. (a) CV for NiCuBO/NF at 5 mV s?1. (b) In-situ electrochemical Raman spectra during forward scan from low to high potential. (c) From high to low potential for NiCuBO/NF. Reprinted with permission from Ref. [49]. Copyright 2023, Elsevier Ltd. (d) Cyclic voltammograms collected on the Ir film electrode. (e) ATR-SEIRA spectra obtained on Ir surface as applied potential positive scanning from 0 to 1.2?V, taken the single-beam spectrum at 1.2? and 0 V as the reference spectrum, respectively. (f) Potential-dependent intensity variation of Ir-Hads, N2Hx+y,ads, NOads, NO2? and NO3?; Reprinted with permission from Ref. [52]. Copyright 2021, Elsevier Ltd.

Table 1 Comparing ammonia electrochemical oxidation rates.

Electrode	pH	Potential (V vs. RHE)	Current density (mA cm^-2)	Net yield reaction rate (mmol L^-1 h^-1 cm^-2)	NO₂^- selectivity (%)	Ref.
Ru-Ir/TiO₂	6.5	—	9	—	1	[53]
Ni(OH)₂	13	1.51	—	—	26.4	[54]
Ni/Ni(OH)₂	11	—	20	0.14	47	[55]
Ni(OH)₂/Ni	11	1.64	—	—	80	[4]

Fig. 13. Factors affecting the performance of electrocatalysts.

Fig. 14. Percentage of Pt(111) and Pt(100) sites for Typea, b, and c nanoparticles and ammonia oxidation on Pt nanoparticles of type c (solidline), type b (dashed line), and type a (dotted line) in 0.2 mol L?1 NaOH and 0.1 mol L?1 NH3. The sweep rate is 10 mV s?1. Reprinted with permission from Ref. [56]. Copyright 2004, American Chemical Society.

Fig. 15. SEM images of the surface morphologies of Pt particles electrodeposited on the ITO substrates at current densities of 0.2 (a), 0.5 (b), 1 (c) mA cm?2. Reprinted with permission from Ref. [57]. Copyright 2012, Elsevier Ltd.

Table 2 Summarize the exemplary results as well as the catalytic performance of different electrocatalyst substrates in the literature.

Electrocatalyst	Carrier material	Ref.
CNT/NCNT@MOF	carbon paper	[59]
1-Cu’	carbon paper	[27]
CuO-Cu₂O	glassy carbon	[60]
Pt/glassy carbon	nickel foam	[61]
Ni(OH)₂-decorated Pt NCs/C	glassy carbon	[62]
(Mn, Fe, Co, Ni, Cu)₃O₄	carbon fiber paper	[63]
NiCo₂N	carbon fiber paper	[64]

Fig. 16. STEM images of the NiCu/CP electrode before (a) and after (b) ammonia electrolysis tests. (c) The LSVs data of NiCu anode and Pt/C anode. Reprinted with permission from Ref. [41]. Copyright 2018, Elsevier Ltd. (d) CV curves in Ar-saturated 0.1 mol L?1 NH3 + 1.0 mol L?1 KOH at 5 mV s?1 (inset is TEM images and corresponding 3D models of PtIrCu HCOND). Reprinted with permission from Ref. [18]. Copyright 2021, Elsevier Ltd.

Fig. 17. SEM (a) and TEM (b) images of Cu@Pt/PGE at various magnifications. Reprinted with permission from Ref. [73]. Copyright 2021, The Royal Society of Chemistry. (c) Schematic of Ni(OH)2-Cu2O@CuO with dual-interface structure. Reprinted with permission from Ref. [61]. Copyright 2020, American Chemical Society.

Fig. 19. (a) A schematic illustration of selective NH3-to-N2 oxidation over Cu/NCNT via the i-SCR mechanism. (b) XPS Cu 2p3/2 spectra for Cu/NCNT catalysts with different surface N contents (Cu 2 wt% for all the catalysts). (c) Concentrations of the reactants and products in NH3-SCO over Cu/NCNT with different concentrations of NO in the reaction mixture at 120 °C. Reprinted with permission from Ref. [77]. Copyright 2022, American Chemical Society.

Fig. 20. (a) HRTEM images of Ce-NR. (b) NH3-TPD profiles of the as-synthesized catalysts. (c) Corresponding peak intensity ratios of I1226/I1117 and the amounts of relevant desorbed-NH3 species (peak β + γ) over the Cu/Ce-NR and Cu/Ce-NC catalysts. Reprinted with permission from Ref. [81]. Copyright 2023, American Chemical Society.

Fig. 21. (a) CV curves at the potential range from 0 to 0.6 V vs. Hg/HgO. (b) Atomic structures of CuO with oxygen vacancies. (c) Free energy diagrams of oxidation on the Vo-free and Vo-rich CuO(111) surface. Reprinted with permission from Ref. [42].Copyright 2022, Springer-Verlag.

Fig. 22. (a) Preparation and evolution of the host-guest Cu catalyst through metal ion deposition and in situ clustering routes. (b) In situ XANES. (c) FE-EXAFS at the Cu K-edge for 1-Cu. Reprinted with permission from Ref. [27] Copyright 2022, American Chemical Society.

Table 3 Summarizes the exemplary results of electrodeposition in the literature for the preparation of electrocatalysts, as well as their structural features and catalytic performance.

Electrocatalyst	Structural characteristics	Test environment	Performancea (Peak current density)	Ref.
Pt-Rh/carbon fiber	continuous Pt-Rh layer on carbon fibers	1.03 mmol L^-1 NH₃ + 0.1 mol L^-1 KOH	15 mA cm^-2 (10 mV s^-1)	[58] [100]
Pt/graphite	Pt layer consisting of aggregates	0.1 mol L^-1 NH₃ + 0.2 mol L^-1 NaOH	32 mA (20 mV s^-1)	[58] [100]
Pt/Ni	submicron-sized Pt particles	0.1 mol L^-1 NH₃ + 0.2 mol L^-1 NaOH	1 mA cm^-2 (5 mV s^-1)	[101]
Pt/glassy carbon	Pt nanoparticles/Pt nanosheetsata	0.075-1.5mmol L^-1 NH₃ + 1 mol L^-1 KOH	4.6 mA (10 mV s^-1)	[102]
Pt-Ir/Pt or Au	Fcc Pt70Ir30 alloy	0.005 mmol L^-1 NH₃ + 0.1 mmol L^-1 KOH	25mA cm^-2 (10 mV s^-1)	[103]
Pt black	Pt film	0.1 mol L^-1 NH₃+1 mol L^-1 NaClO₄	22.5 mA (5 mV s^-1)	[104]
Pt	coral-like Pt nanowires	0.05 mol L^-1 (NH₄)₂SO₄ + 1 mol L^-1 KOH	72 mA cm^-2 (10 mV s^-1)	[105]
NiCu@NiCuOOH	core-shell NiCu@NiCuOOH	0.5 mol L^-1 NaOH + 0.015 mol L^-1 NH₄Cl	—	[99]
NiCu-S/DSA	particulate metal oxides	0.5 mol L^-1 NaOH + 0.015 mol L^-1 NH₄Cl	—	[106]

Fig. 24. (a) The formation diagram of NiCu@NiCuOOH-NF core-shell electrode. (b) SEM images of NiCu@NiCuOOH-NF. (c) The comparison of i-t curves at 0.6 V vs. SCE between 2 mol L?1 NaOH + 0.4 NH4Cl and 2 mol L?1 NaOH. Reprinted with permission from Ref. [99]. Copyright 2022, Elsevier Ltd.

Fig. 25. (a) Magnified TEM image. (b) Size distribution histogram. (c) Chronoamperometry curves of Pt-NCs and Pt-NPs-JM in 1 mol L?1 KOH solution containing 0.1 mol L?1 NH4OH at 0.6 V potential. Reprinted with permission from Ref. [107]. Copyright 2020, Elsevier Ltd.

Fig. 26. Schematic representation of the relative orientation of (003), (012), and (100) facets for CuFeO2 (a) and (012), (104), and (212?1) facets for CuFeO2-NH3 (b). (c) Calculated free energy profile for AOR processes on CuFeO2 (212?1) and CuFeO2 (212?1) @Cu-FeOOH (adsorption sites*). The inset is the charge density difference of *NH3 models. Isosurface is 0.003 e ??1. Reprinted with permission from Ref. [108]. Copyright 2023, Wiley-VCH.

Fig. 27. (a) HAADF-STEM images of individual PtIrCu RDNF-HNDs-2, and corresponding 3D models of respectively. (b) CV curves in Ar-saturated 0.1 mol L?1 NH3 and 1.0 mol L?1 KOH at 5 mV s?1. (c) Free energy diagrams of NH3 dehydrogenation at 0.3 V vs. RHE. Reprinted with permission from Ref. [109]. Copyright 2023, Elsevier Ltd.

Fig. 28. (a) TEM pictures of colloidal Pt nanoparticles. (b) Cyclic voltammograms of voltammetric profiles of Pt(100), Pt(110), Pt(111) and polyoriented Pt single crystal in 0.1 mol L?1 NaOH and 10?3 mol L?1 NH3. Scan rate 10 mV s?1. (c) Ammonia oxidation on hydrazine-Pt, borohydride-Pt, and colloidal Pt nanoparticles and polyoriented platinum in 0.2 mol L?1 NaOH and 0.1 mol L?1 NH3. Scan rate 10 mV s?1. Reprinted with permission from Ref. [110]. Copyright 2004, Elsevier Ltd.

Fig. 29. (a) Preparation schematic diagram of PtZn-P-300. (b) Cyclic voltammograms of HRTEM false color images of PtZn-P-300. (c) CV curves in 1.0 mol L?1 KOH with 0.1 mol L?1 NH3·H2O solution at 10 mV s?1. Reprinted with permission from Ref. [111]. Copyright 2023, Elsevier Ltd.

Fig. 30. The effect of NH3 concentration on the AOR. (a) LSV curves of α-Fe2O3 in the 0.1 mol L?1 NaClO4 electrolytes with different NH3 concentrations. (b) The FEs and the average current density at 1.3 V. Reprinted with permission from Ref. [118]. Copyright 2022, Wiley-VCH.

Fig. 31. The Classification of AOR research hotspots.

Fig. 32. Schematic illustration of the natural nitrogen cycle network dominated by NO2/3? prepared by AOR.

Table 4 Assessment of several waste-ammonia-to-fertilizer recovery strategies [6]. a

Strategy	Reaction	α_in ($)	Produced fertilizer	N-P-K-(S) ratio	α_out ($)	δ ($)
Acid-base reaction	2NH₃ (0.3 mol L^-1) + H₂SO₄ (0.15 mol L^-1) → (NH₄)₂SO₄ (0.15 mol L^-1)	0.4	(NH₄)₂SO₄	21-0-0-(24)	1.7	1.3
Acid-base reaction	NH₃ (0.3 mol L^-1) + HNO₃ (0.3 mol L^-1) → NH₄NO₃ (0.3 mol L^-1)	1.7	NH₄NO₃	35-0-0-(0)	2.1	0.3
Electrolysis in 0.1 mol L^-1 K₂SO₄	2NH₃ (0.3 mol L^-1) + 3H₂O → NH₄NO₃ (0.15 mol L^-1) + 4H₂	3.6	NH₄NO₃ + K₂SO₄ (3:2)	14-0-32-(11)	4.6	1.0
Electrolysis in 0.1 mol L^-1 K₂HPO₄	2NH₃ (0.3 mol L^-1) + 3H₂O → NH₄NO₃ (0.15 mol L^-1) + 4H₂	6.7	NH₄NO₃ + K₂HPO₄ (3:2)	14-24-32-(0)	7.7	1.0

Table 5 Assessment of several waste-ammonia-to-fertilizer recovery strategies [6].

Strategy	Reaction	α_in ($)	Produced fertilizer	N-P-K-(S) ratio	α_out ($)
Acid-base reaction	2NH₃ (0.3 mol L^-1) + H₂SO₄ (0.15 mol L^-1) → (NH₄)₂SO₄ (0.15 mol L^-1)	0.15	(NH₄)₂SO₄	21-0-0-(24)	0.66	0.51
Acid-base reaction	NH₃ (0.3 mol L^-1) + HNO₃ (0.3 mol L^-1) → NH₄NO₃ (0.3 mol L^-1)	1.00	NH₄NO₃	35-0-0-(0)	1.18	0.18
Electrolysis in 0.1 mol L^-1 K₂SO₄	2NH₃ (0.3 mol L^-1) + 3H₂O → NH₄NO₃ (0.15 mol L^-1) + 4H₂	1.90	NH₄NO₃ + K₂SO₄ (3:2)	14-0-32-(11)	2.49	0.59

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用于氨电氧化反应生成硝酸盐/亚硝酸盐的金属基电催化剂：过去、现在和未来

Metal-based electrocatalysts for ammonia electro-oxidation reaction to nitrate/nitrite: Past, present, and future

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