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化学进展 2020, Vol. 32 Issue (1): 33-45 DOI: 10.7536/PC190606 前一篇   后一篇

所属专题： 电化学有机合成

• •

基于非贵金属催化剂常温常压电化学合成氨

郭芬岈1, 李宏伟1, 周孟哲2, 徐正其2, 郑岳青1, 黎挺挺1,**()   

  1. 1. 宁波大学化学合成与绿色应用研究所 材料科学与化学工程学院 宁波 315211
    2. 宁波大学医学院 宁波 315211
  • 收稿日期:2019-06-10 出版日期:2020-01-15 发布日期:2019-12-11
  • 通讯作者: 黎挺挺
  • 基金资助:
    国家自然科学基金项目资助(21603110)
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Electroreduction of Nitrogen to Ammonia Catalyzed by Non-Noble Metal Catalysts under Ambient Conditions

Fenya Guo1, Hongwei Li1, Mengzhe Zhou2, Zhengqi Xu2, Yueqing Zheng1, Tingting Li1,**()   

  1. 1. Chemistry Institute for Synthesis and Green Application, School of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211, China
    2. Medical School, Ningbo University, Ningbo 315211, China
  • Received:2019-06-10 Online:2020-01-15 Published:2019-12-11
  • Contact: Tingting Li
  • About author:
    ** E-mail:
  • Supported by:
    National Natural Science Foundation of China(21603110)

氨是一种重要的化工原料和能量载体,“哈伯反应”是工业上合成氨最主要的方法,但是该方法存在着能耗高,大量排放温室气体CO2以及转化率低等问题。近年来,常温常压下基于多相催化剂的电化学还原N2反应(NRR)来制备氨因其原料(N2 + H2O)易得,不依赖传统化石能源以及条件温和等原因而表现出巨大的应用潜能,并受到了科学家的广泛关注。然而目前NRR仍存在着如催化剂以贵金属材料为主,催化效率低和催化机理未明确等问题亟待解决。本综述主要总结了电催化NRR的最新研究成果,首先介绍了电催化NRR热力学和催化机理,接着重点列举了基于非贵金属催化剂的研究进展,包括过渡金属氧化物、氮化物、硫化物、非金属催化剂及单原子催化剂等,然后讨论了几种NRR电催化剂的改性方法,以及常见的产物氨的定性定量方法,最后,就目前该研究方向中仍待解决的问题进行了总结,并对下一步的研究进行了展望。

关键词： 电化学合成氨, 非贵金属催化剂, 催化机理, 催化剂改性, 氨的检测

Ammonia is an important chemical for producing fertilizer and also an important carbon-free energy carrier. Haber-Bosch process is the main method to synthesize ammonia. However, it suffers from some severe problems, such as the high energy consumption, the massive emission of greenhouse gas CO2 and the poor catalytic efficiency. Recently, ammonia synthesis based on electrocatalytic nitrogen reduction reaction (NRR) by using renewable energy under mild reaction conditions has attracted wide research attention. In addition, the raw materials (N2 + H2O) are earth abundant. Although great advances have been achieved in electrocatalytic NRR field, some challenges including the high-cost of noble metal based electrocatalysts, the low ammonia yield and unsatisfactory Faradaic efficiency, as well as the unexplored catalytic mechanism of NRR still exist. In this review, we summarize the recent advances in electrocatalytic NRR field based on heterogeneous catalysts. Firstly, we discuss the catalytic thermodynamics and reaction mechanisms towards NRR. Secondly, a range of recently reported non-noble metal included catalysts are surveyed, including transition metal oxides/nitrides/sulfides, metal-free materials and single-metal-atom catalysts. Then, some promising strategies to enhance the catalytic activity, selectivity and efficiency are proposed, and the main methods for the determination of ammonia are also mentioned. Finally, the challenges remaining to be solved are summarized, and future perspectives are also presented.

Key words: electrochemical ammonia synthesis, non-noble metal catalysts, catalytic mechanism, catalyst optimization, determination of ammonia
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图1 基于多相催化剂NRR机理图[10]
Fig. 1 The mechanism of electrochemical N2 reduction reaction based on heterogeneous catalysts[10]
图2 (a) Cr2O3微米球高分辨透射电镜图;(b) 不同电压下Cr2O3微米球的i~t曲线; (c) 施加不同电压后电解液所对应的UV-Vis光谱图; (d) 稳定性循环实验[56]
Fig. 2 (a) The HR-TEM image of Cr2O3 microspheres; (b) The i~t plots obtained from different applied potentials; (c) The corresponding UV-Vis spectra obtained after long-term tests; (d) The durability test for Cr2O3 microspheres[56]
图3 (a) VN纳米颗粒的扫描电镜图;(b )电催化NRR性能;(c) 电催化机理及失活路径[63]
Fig. 3 (a) The SEM image of VN nanoparticles; (b) The electrocatalytic NRR performance; (c) The electrocatalytic mechanism and corresponding deactivation pathway[63]
图4 (a) 富缺陷MoS2纳米花的扫描电镜图;(b) 施加不同电压后电解液所对应的UV-Vis光谱图;(c) 不同电压电解实验所对应的合成氨速率;(d) 基于富缺陷MoS2纳米花电催化NRR的自由能变化图[67]
Fig. 4 (a) SEM image for defect-rich MoS2 nanoflower; (b) The corresponding UV-Vis spectra obtained after long-term tests; (c) The corresponding NH3 yields under different potentials; (d) Calculated free energy profile for NRR process on MoS2 basal plane[67]
图5 (a) 基于B掺杂石墨烯电催化NRR结构示意图;(b) 不同B掺杂量的石墨烯;(c) B掺杂量对于石墨烯电催化法拉第效率的影响[76]
Fig. 5 (a) Schematic illustration of NRR over B-doped graphene; (b) Percentages of different B doping configurations in three B-doped graphene samples; (c) The Faradaic efficiency values of BG-1, BOG, BG-2 and G at different applied potentials[76]
图6 (a) Ru/N-C的制备方法;(b~e) Ru/N-C与Ru纳米颗粒的电催化NRR性能比较[84]
Fig. 6 (a) Scheme of the synthetic procedure for Ru/N-C; (b~e) Comparison of electrocatalytic NRR performance for Ru/N-C and Ru nanoparticles[84]
图7 (a) 二十四面体Au纳米棒的原子层表面结构;(b) Au纳米棒几何模型及暴露的{730}面;(c) 电化学反应池构成;(d) Au纳米棒不同电压下的电催化NRR表现[91]
Fig. 7 (a) Atomic level surface structures of Au THH NR; (b) Geometric models of an Au THH NR and exposed {730} facet; (c) Schematic for electrocatalytic NRR; (d) Yield rate of ammonia, hydrazine hydrate formation, and Faradic efficiency at each given potential[91]
图8 (a) 基于MoN纳米片阵列电化学反应池示意图;(b) MoN纳米片阵列扫描电镜图;(c,d) 不同电压下电催化NRR性能[92]
Fig. 8 (a) Schematic for electrocatalytic NRR based on MoN nanosheet array; (b) The corresponding SEM image; (c,d) The electrocatalytic performance under various applied potential[92]
图9 (a) 碳缺陷的碳纳米片(BCN)的扫描电镜图;(b) 基于理论模拟的BCN表面结构(灰(黑)、粉、红、黄和绿球分别代表C、B、O、N和H);(c) 不同催化剂对应的电催化NRR性能[97]
Fig. 9 (a) The SEM image for BCN materials; (b) Schematic of the computational models. Gray (black), pink, red, blue, and green balls represent C, B, O, N, and H atoms, respectively; (c) The corresponding electrocatalytic NRR performance based on different catalysts[97]
表1 电催化剂性能对比
Table 1 Summary of recently reported NRR electrocatalysts
Catalyst Electrolyte NH3 yield rate Faraday efficiency(%) Ref
Noble metalcatalyst Au nanocage 0.5 M LiClO4 3.9 μg·h-1·cm-2 (-0.5 V vs. RHE) 30.2 25
Au nanorod 0.1 M KOH 1.648 μg·h-1·cm-2 (-0.2 V vs. RHE) 4 91
Ru/C 2 M KOH 0.21 μg·h-1·cm-2 (-1.1 V vs. Ag/AgCl) 0.28 27
RuPt/C 18.36 μg·h-1·cm-2 (0.123 V vs. RHE) 13.2 28
Rh ultrathin nanosheet 0.1 M KOH 23.88 μg·h-1·m g cat - 1 (-0.2 V vs. RHE) 0.217 31
Pt/C H+/Li+/N H 4 + 47.2 μg·h-1·cm-2 (1.2 V) 0.83 32
Non-noble metal catalyst Fe2O3/CNT dilute KHCO3 solution 0.22 μg·h-1·cm-2 (-0.2 V vs. Ag/AgCl) 0.15 49
Fe2O3-rGO 0.5 M LiClO4 22.13 μg·h-1·m g cat - 1 (-0.50 V vs. RHE) 5.89 51
Fe2O3- x /CNT 0.1 M KOH 0.46 μg·h-1·cm-2 (-0.9 V vs. Ag/AgCl) 6.0 52
Fe3O4/Ti 0.1 M Na2SO4 5.6×10-11 mol·s-1·cm-2 (-0.4 V vs. RHE) 2.6 53
Hollow Cr2O3 mircometer
ball		 0.1 M Na2SO4 25.3 μg·h-1·m g cat - 1 (-0.9 V vs. RHE) 6.78 56
Mo2N 0.1 M HCl 78.4 μg·h-1·m g cat - 1 (-0.3 V vs. RHE) 4.5 62
VN 0.05 M H2SO4 20.2 μg·h-1·cm-2 (-0.1 V vs. RHE) 6 63
MoS2 0.1 M Na2SO4 8.08×10-11 mol·s-1·cm-2 (-0.5 V vs. RHE) 1.17 66
Defect-rich MoS2 nanoflower 0.1 M Na2SO4 29.28 μg·h-1·m g cat - 1 (-0.4 V vs. RHE) 8.34 67
MoS2/graphene 0.1 M LiClO4 24.82 μg·h-1·m g cat - 1 (-0.45 V vs. RHE) 4.58 68
CoS x /NS-G 0.05 M H2SO4 25.0 μg·h-1·m g cat - 1 (-0.2 V vs. RHE) 25.9
(-0.05 V vs.RHE)		 69
MoN nanosheet array 0.1 M HCl 3.01×10-10 mol·s-1·cm-2 (-0.3 V vs. RHE) 1.15 92
Bi nanosheet array 0.1 M HCl 6.89 × 10-11 mol·s-1·cm-2 (-0.5 V vs. RHE) 10.26 93
Bi4V2O11/CeO2 0.1 M HCl 23.21 μg·h-1·mg-1 (-0.2 V vs. RHE) 10.16 96
Metal-free catalyst Oxidized carbonnanotube 0.1 M LiClO4 32.33 μg·h-1·m g cat - 1 (-0.4 V vs. RHE) 12.50 73
N-doped Carbon 0.1 M KOH 3.4×10-6 mol·h-1·cm-2(-0.4 V vs. RHE) 10.2 75
B-doped graphene 0.05 M H2SO4 9.8 μg·h-1·cm-2 (-0.5 V vs. RHE) 10.8 76
N, P-codoped porous carbon 0.1 M HCl 0.97 μg·h-1·m g cat - 1 (-0.2 V vs. RHE) 4.2 77
BCN 0.1 M HCl 7.75 μg·h-1·mgcat.-1 (-0.2 V vs. RHE) 13.79 97
nitrogen-decifient polymeric carbon nitride 0.1 M HCl 8.09 μg·h-1·m g cat - 1 (-0.2 V vs. RHE) 11.59 98
S-CNS 0.1 M Na2SO4 19.07 μg·h-1·m g cat - 1 (-0.7 V vs. RHE) 7.47 99
single metal atom catalyst Au/C3N4 0.05 M H2SO4 1.3 mg·h-1·m g Au - 1 (-0.1 V vs. RHE) 11.1 83
Ru/N-C 0.05 M H2SO4 120.9 μg·h-1·mg-1 (-0.2 V vs. RHE) 29.6 84
Ru/N-C 0.1 M HCl 3.665 m g N H 3 ·h-1·m g Ru - 1 (-0.21 V) 21 (-0.11 V) 85
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