可批量合成的FeNi@纳米多孔碳电催化剂用于高效尿素合成

doi:10.1016/S1872-2067(24)60111-7

催化学报 ›› 2024, Vol. 65: 153-162.DOI: 10.1016/S1872-2067(24)60111-7

可批量合成的FeNi@纳米多孔碳电催化剂用于高效尿素合成

孙作淑^a^,¹, 向雪艳^a^,¹, 赵秋平^a, 唐朝^a, 姜诗译^a, 鲁统部^a, 张志明^a, 王白帆^b^,^*(), 尹华卿^a^,^*()

^a天津理工大学材料科学与工程学院, 新能源材料与低碳技术研究院, 天津300384
^b南开大学化学学院, 元素有机化学国家重点实验室, 天津300071

收稿日期:2024-05-27 接受日期:2024-07-31 出版日期:2024-10-18 发布日期:2024-10-15
通讯作者: *电子信箱: hqyin@email.tjut.edu.cn (尹华卿), baifan_wang@outlook.com (王白帆).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(22104110);国家自然科学基金(22071180);国家自然科学基金(92161103);天津市自然科学基金(18JCJQJC47700)

Efficient electrocatalytic urea synthesis from CO₂ and nitrate over the scale-up produced FeNi alloy-decorated nanoporous carbon

Zuo-Shu Sun^a^,¹, Xue-Yan Xiang^a^,¹, Qiu-Ping Zhao^a, Zhao Tang^a, Shi-Yi Jiang^a, Tong-Bu Lu^a, Zhi-Ming Zhang^a, Baifan Wang^b^,^*(), Hua-Qing Yin^a^,^*()

^aInstitute for New Energy Materials and Low Carbon Technologies, School of Materials Science & Engineering, Tianjin University of Technology, Tianjin 300384, China
^bState Key Laboratory of Elemento-Organic Chemistry, College of Chemistry, Nankai University, Tianjin 300071, China

Received:2024-05-27 Accepted:2024-07-31 Online:2024-10-18 Published:2024-10-15
Contact: *E-mail: hqyin@email.tjut.edu.cn (H.-Q. Yin), baifan_wang@outlook.com (B. Wang).
About author:¹ These authors contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22104110);National Natural Science Foundation of China(22071180);National Natural Science Foundation of China(92161103);Natural Science Foundation of Tianjin City of China(18JCJQJC47700)

摘要/Abstract

摘要：

尿素在农业、工业合成和医药产品等领域有着广泛的应用. 传统的尿素合成通常使用NH₃和CO₂制得, 然而这一过程需要苛刻的条件(150‒250 bar, 150‒200 °C)及复杂的设备, 且消耗大量的NH₃. 而NH₃的合成是通过Haber-Bosch工艺实现的, 会消耗大量化石能源并伴随着大量温室气体的排放. 近几十年来, 科研工作者致力于利用CO₂和含氮小分子(N₂, NO₂^-和NO₃^-)的电催化共还原策略实现尿素合成. 其中, 由于NO₃^-的N=O解离能(204 kJ mol^-1)相对较低, 直接合成尿素的效率更高. 此外, 利用硝酸盐作为尿素合成的原料, 能够缓解水体中硝酸盐积累导致的富营养化问题. 因此, 在温和条件下电催化耦合CO₂和NO₃^-合成尿素, 被认为是一种环境友好的绿色合成策略. 尽管非贵金属催化剂已被广泛应用于尿素电催化合成, 但合成具有工业前景的电催化剂的大规模生产仍具有挑战性. 同时, 在利用CO₂和NO₃^-合成尿素的过程中, C-N偶联反应的高势垒仍然限制着其催化效率的提升.

本文采用简单浸渍-煅烧法批量合成了以纳米多孔碳为载体的廉价金属FeNi@nC-T复合材料(n代表纳米多孔碳的含量, 分别为1, 3, 5, 7, 9 g; T代表煅烧温度, 分别为900, 950, 1000, 1100 °C), 并用于电催化CO₂和NO₃^-高效共还原合成尿素. 纳米多孔碳不仅为CO₂和NO₃^-的吸附提供了较大的比表面积, 而且促进了FeNi合金纳米颗粒的均匀分布, 使CO₂和NO₃^-的共还原反应分别在Ni及Fe位点上高效进行. 实验结果显示, FeNi@7C-1000表现出较好的尿素合成效率, 在‒1.2 V vs. RHE电压下电解2 h, 尿素产率可达1041.33 mmol h^-1 g_FeNi^-1, 法拉第效率(FE)为15.56%, 显著高于Fe@7C-1000 (374.26 mmol h^-1 g_Fe^-1, FE 8.00%)和Ni@7C-1000 (495.43 mmol h^-1 g_Ni^-1, FE 10.75%). 此外, FeNi@7C-1000还具备良好的电催化稳定性和可循环利用性. 值得一提的是, 本研究成功实现了电催化剂(以FeNi@7C-950-S为例)的批量制备(每批次100 g), 且催化剂在相同条件下仍能维持高效的尿素电催化性能(1034.42 mmol h^-1 g_FeNi^-1, FE 10.44%)及良好的稳定性. 通过系统实验和密度泛函理论计算进一步阐明了CO₂和NO₃^-还原同时发生在Ni和Fe位点上, 且中间产物*CO和*N偶联显著降低了C-N偶联反应势垒, 从而实现了尿素的高效合成.

综上所述, 本文以降低电催化尿素合成过程中的C-N偶联的能垒为切入点, 理性设计出了可批量合成的FeNi@nC-T复合催化体系, 为实现高效的电催化合成尿素, 缓解能源和环境危机, 提供了一种有效策略.

关键词: 尿素合成, 电催化, FeNi合金, 批量合成, C-N耦合

Abstract:

Electrocatalytic urea synthesis provides a favorable strategy for conventional energy-consuming urea synthesis, but achieving large-scale catalyst synthesis with high catalytic efficiency remains challenging. Herein, we developed a simple method for the preparation of a series of FeNi-alloy-based catalysts, named FeNi@nC-T (n represents the content of nanoporous carbon as 1, 3, 5, 7 or 9 g and T = 900, 950, 1000 or 1100 °C), for highly performed urea synthesis via NO₃^- and CO₂ co-reduction. The FeNi@7C-1000 achieved a high urea yield of 1041.33 mmol h^-1 g_FeNi^-1 with a Faradaic efficiency of 15.56% at -1.2 V vs. RHE. Moreover, the scale-up synthesized FeNi@7C-950-S (over 140 g per batch) was achieved with its high catalytic performance and high stability maintained. Mechanism investigation illuminated that the Ni and Fe sites catalyze and stabilize the key *CO and *N intermediates and minimize the C-N coupling reaction barriers for highly efficient urea synthesis.

Key words: Urea synthesis, Electrocatalysis, FeNi alloy, Scale-up synthesis, C-N coupling

孙作淑, 向雪艳, 赵秋平, 唐朝, 姜诗译, 鲁统部, 张志明, 王白帆, 尹华卿. 可批量合成的FeNi@纳米多孔碳电催化剂用于高效尿素合成[J]. 催化学报, 2024, 65: 153-162.

Zuo-Shu Sun, Xue-Yan Xiang, Qiu-Ping Zhao, Zhao Tang, Shi-Yi Jiang, Tong-Bu Lu, Zhi-Ming Zhang, Baifan Wang, Hua-Qing Yin. Efficient electrocatalytic urea synthesis from CO₂ and nitrate over the scale-up produced FeNi alloy-decorated nanoporous carbon[J]. Chinese Journal of Catalysis, 2024, 65: 153-162.

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https://www.cjcatal.com/CN/Y2024/V65/I10/153

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Fig. 1. (a) HRTEM and (b) enlarged TEM images of FeNi@7C-1000 (inset is a crystal lattice of FeNi@7C-1000). (c) The line scan intensity profile of FeNi@7C-1000. (d) HAADF-STEM images and the corresponding EDX elemental mapping images of FeNi@7C-1000.

Fig. 2. (a) The experimental PXRD patterns of FeNi@nC-1000 (n = 1, 3, 5, 7, 9) and the simulated PXRD signal of FeNi alloy. The high-resolution XPS spectra of Fe 2p (b) and Ni 2p (c) of the FeNi@7C-1000. (d) The nitrogen adsorption-desorption isotherms of the nanoporous carbon before and after FeNi alloy anchoring (inset is the pore size distribution).

Fig. 3. (a) LSV curves of FeNi@7C-1000 in the Ar/KNO3, CO2/KNO3, and CO2/K2SO4 systems. Electrocatalytic performance over FeNi@7C-1000 under different applying potentials (b) and FeNi@nC-1000 under -1.2 V vs. RHE (c). (d) The urea yield over FeNi@7C-1000, FeNi@7C-950 and FeNi@7C-950-S. (e) Recycle experiments and (f) current intensity stability of FeNi@7C-1000.

Fig. 4. DFT calculations. (a) Free-energy diagram for urea production on the FeNi alloy. (b) Corresponding atomic configurations for each step.

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可批量合成的FeNi@纳米多孔碳电催化剂用于高效尿素合成

Efficient electrocatalytic urea synthesis from CO₂ and nitrate over the scale-up produced FeNi alloy-decorated nanoporous carbon

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可批量合成的FeNi@纳米多孔碳电催化剂用于高效尿素合成

Efficient electrocatalytic urea synthesis from CO2 and nitrate over the scale-up produced FeNi alloy-decorated nanoporous carbon

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Efficient electrocatalytic urea synthesis from CO₂ and nitrate over the scale-up produced FeNi alloy-decorated nanoporous carbon