强化脱氢动力学实现超低电池电压和大电流密度下抗坏血酸电氧化

doi:10.1016/S1872-2067(23)64446-8

催化学报 ›› 2023, Vol. 50: 372-380.DOI: 10.1016/S1872-2067(23)64446-8

• 论文 • 上一篇

强化脱氢动力学实现超低电池电压和大电流密度下抗坏血酸电氧化

周波^a^,¹, 石建巧^a^,¹, 姜一民^a^,¹, 肖磊^b, 逯宇轩^a, 董帆^b, 陈晨^a, 王特华^a^,^c, 王双印^a, 邹雨芹^a^,^*()

^a湖南大学生物传感与化学计量学国家重点实验室, 教育部先进催化工程中心, 湖南长沙 410082
^b电子科技大学基础与前沿科学研究所, 环境与能源催化研究中心, 四川成都 611700
^c湖南大学深圳学院, 广东深圳 518057

收稿日期:2023-04-21 接受日期:2023-05-07 出版日期:2023-07-18 发布日期:2023-07-25
通讯作者: *电子信箱: yuqin_zou@hnu.edu.cn (邹雨芹).
作者简介:
¹共同第一作者.
基金资助:
国家重点研发计划(2020YFA0710000);国家重点研发计划(2021YFA1500900);国家自然科学基金(22122901);国家自然科学基金(U19A2017);国家自然科学基金(21972164);湖南省自然科学基金(2021JJ0008);湖南省自然科学基金(2021JJ20024);湖南省自然科学基金(2021RC3054);湖南省自然科学基金(2020JJ5045);深圳市科技计划项目(JCYJ20210324140610028)

Enhanced dehydrogenation kinetics for ascorbic acid electrooxidation with ultra-low cell voltage and large current density

Bo Zhou^a^,¹, Jianqiao Shi^a^,¹, Yimin Jiang^a^,¹, Lei Xiao^b, Yuxuan Lu^a, Fan Dong^b, Chen Chen^a, Tehua Wang^a^,^c, Shuangyin Wang^a, Yuqin Zou^a^,^*()

^aState Key Laboratory of Chemo/Bio-Sensing and Chemometrics, College of Chemistry and Chemical Engineering, Advanced Catalytic Engineering Research Center of the Ministry of Education, Hunan University, Changsha 410082, Hunan, China
^bResearch Center for Environmental and Energy Catalysis, Institute of Fundamental and Frontier Sciences, University of Electronic Science and Technology of China, Chengdu 611700, Sichuan, China
^cShenzhen Institute of Hunan University, Shenzhen 518057, Guangdong, China

Received:2023-04-21 Accepted:2023-05-07 Online:2023-07-18 Published:2023-07-25
Contact: *E-mail: yuqin_zou@hnu.edu.cn (Y. Zou).
About author:
¹ Contributed equally to this work.
Supported by:
National Key R&D Program of China(2020YFA0710000);National Key R&D Program of China(2021YFA1500900);National Natural Science Foundation of China(22122901);National Natural Science Foundation of China(U19A2017);National Natural Science Foundation of China(21972164);Natural Science Foundation of Hunan Province(2021JJ0008);Natural Science Foundation of Hunan Province(2021JJ20024);Natural Science Foundation of Hunan Province(2021RC3054);Natural Science Foundation of Hunan Province(2020JJ5045);Shenzhen Science and Technology Program(JCYJ20210324140610028)

摘要/Abstract

摘要：

当今社会日益严峻的能源危机进一步加速了生物质资源多层次转化利用的发展, 现代生物质能源技术已成为研究热点. 抗坏血酸是生物质平台分子之一, 脱氢抗坏血酸作为抗坏血酸的氧化产物, 不仅与抗坏血酸一起组成了生物抗氧化系统, 而且还发挥着重要的生物医学功能, 例如人体抗癌、抗病毒和抗衰老等. 在众多的脱氢抗坏血酸制备方法中, 抗坏血酸的电催化氧化提供了在常温常压条件下使用水作为氧化剂和电能作为能量输入生产脱氢抗坏血酸的机会. 另一方面, 在水体系内, 较低的抗坏血酸理论氧化电位(E_理论 = 0.390 V)使得抗坏血酸氧化反应/氢析出反应(AAOR/HER)电对可以在低电池电压下工作, 降低了因高电压带来的能源消耗和设备要求等成本, 实现低能耗条件下的化学品转化和制氢.

本课题组通过简单的氧气等离子体在碳材料表面引入含氧官能团(OCGs), 并揭示了OCGs和抗坏血酸分子脱氢动力学之间的关系, 利用提升反应动力学的策略提高AAOR的电催化活性. 得益于OCGs对抗坏血酸分子脱氢动力学的调控作用, 所设计的氧气等离子体处理碳纸电极(P_O-CP)可以在0.65 V_RHE下驱动100 mA cm^-2的电流密度, 明显优于原始碳纸(CP)和其他金属基电催化剂. 此外, 在P_O-CP电极表面抗坏血酸制备脱氢抗坏血酸的法拉第效率超过90%, 并且具备较好的稳定性(20 h). X射线光电子能谱(XPS)结果表明, 随着等离子体处理时间的延长, 碳表面的含氧量增加, 最终呈现饱和状态. 进一步利用氢气退火作为对照组去除表面的OCGs, 发现退火过程中所有类型的OCGs含量都明显下降, 其中羧基和羰基的含量变化明显, 说明退火处理可显著去除碳表面的C=O键, 进而影响其AAOR性能. 电化学测试表明, OCGs的引入提升了碳材料的AAOR本征活性, 氢气退火对照组性能急剧下降, 进一步表明了碳表面的含氧官能团对AAOR性能的提升至关重要. 结合XPS结果, 分析其中C=O键可能对AAOR本征活性的提升发挥重要作用. 为降低三维电极带来的传质影响及等离子体处理对碳表面清洁影响等, 进一步选用商业碳粉(XC 72)作为模型材料并在玻碳电极表面探究OCGs的影响, 同时选择氧气等离子体刻蚀和电化学氧化方法作为OCGs修饰策略. 电化学测试表明, XC 72表面的电化学性能规律和碳纸表面类似, 进一步表明了碳表面的OCGs对AAOR的性能提升至关重要. 最后, 通过密度泛函理论来对AAOR的各基元步骤的吉布斯自由能(G_ads)进行了研究. 结果表明, OCGs修饰后, 虽然AAOR的决速步骤没有发生变化(第一步脱氢过程), 但是ΔG_ads变化明显. 相比于原始碳晶格(G_ads(C) = 1.36 eV), 不同含氧官能团修饰下的碳表面的吉布斯自由能变化为ΔG_ads(-OH) = 1.33 eV, ΔG_ads(C=O) = 1.55 eV, ΔG_ads(-COOH) = 1.24 eV. 由此可见, 含氧官能团特别是羧基的引入, 可以显著降低AAOR过程中脱氢能垒, 通过增强脱氢动力学来实现高效的抗坏血酸转化.

此外, 还将AAOR和HER集成到质子交换膜型电解槽中, 当P_O-CP阳极和Pt/C阴极组装时, 在0.98 V (80 ^oC)的超低电池电压下获得了1.00 A cm^-2的电流, 这是目前电催化有机物转化反应的一个非常有优势的数据. 而且系统每产生1 m³的氢气只需要1.54 kWh的电能, 几乎是传统电解水(4.95 kWh)的三分之一. 综上, 基于抗坏血酸在P_O-CP表面高效率的电化学转化, 这项工作为电化学生物质转化升级和制氢提供了更环保更经济的策略，并为适应规模化生产的电极设计提供了参考。

关键词: 电催化, 抗坏血酸电化学氧化, 氧等离子体, 制氢, 无金属电催化剂, 脱氢动力学

Abstract:

Dehydroascorbic acid (DHA) production from ascorbic acid electrochemical oxidation (AAOR) can be used to upgrade biomass derivatives and hydrogen production with low energy consumption. Carbon materials are a promising class of nonmetal AAOR electrocatalysts; however, their performance does not meet the requirements for practical applications. In this study, an oxygen-containing group (OCG)-modified carbon electrocatalyst was prepared via oxygen plasma treatment. It could drive a current density of 100 mA cm^-2 at only 0.65 V_RHE and realize a Faradaic efficiency of over 90% for DHA production with long-term stability of 20 h. A proton exchange membrane-type electrolyzer integrating the anodic AAOR and the cathodic hydrogen evolution reaction (HER) was assessed. It only requires a cell voltage input of 0.98 V to deliver a current density of 1000 mA cm^-2, which is superior to most reported organic upgrading reactions. Moreover, it only needs 1.54 kWh to produce normal cubic H₂, which is one-third of that of traditional water electrolysis. Importantly, the contribution of each type of OCG was investigated by combining electrochemical measurements and theoretical calculations. It was revealed that the OCGs, especially the carboxyl groups (-COOH) of carbon materials, could enhance the dehydrogenation kinetics of the AAOR, thereby boosting the electrocatalytic activity. This study presents a low-energy and eco-friendly strategy for electrochemical biomass upgrading and hydrogen production, provides an in-depth understanding of the role of oxygen-containing functional groups in the AAOR, and guides the design of carbon-based electrocatalysts for AAOR.

Key words: Electrocatalysis, L-ascorbic acid electro-oxidation, Oxygen plasma, Hydrogen production, Metal-free electrocatalyst, Dehydrogenation kinetics

周波, 石建巧, 姜一民, 肖磊, 逯宇轩, 董帆, 陈晨, 王特华, 王双印, 邹雨芹. 强化脱氢动力学实现超低电池电压和大电流密度下抗坏血酸电氧化[J]. 催化学报, 2023, 50: 372-380.

Bo Zhou, Jianqiao Shi, Yimin Jiang, Lei Xiao, Yuxuan Lu, Fan Dong, Chen Chen, Tehua Wang, Shuangyin Wang, Yuqin Zou. Enhanced dehydrogenation kinetics for ascorbic acid electrooxidation with ultra-low cell voltage and large current density[J]. Chinese Journal of Catalysis, 2023, 50: 372-380.

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Fig. 1. Physical and chemical characterization of electrocatalysts and electrocatalytic activity towards AAOR in 0.5 mol L?1 H2SO4 and 0.1 mol L?1 AA electrolyte. High-resolution XPS spectra of C 1s (a) and O 1s (b) for CP, Po-CP, and Po-CP-H2. (c) Content of various oxygenated groups at CP, Po-CP, and Po-CP-H2 surface. The content of different structures equals the content of total oxygen from wide XPS spectra times the ratio of the typical structure obtained from high-resolution XPS of O 1s spectra; (d) LSV curves for PO-CP with and without 0.1 mol L?1 AA in 0.5 mol L?1 H2SO4. (e) LSV curves for CP, Po-CP, and Po-CP-H2. (f) Tafel slopes of AAOR at CP, Po-CP, and Po-CP-H2 electrodes. (g) Conversion of AA and Faraday efficiencies of DHA at different potentials. (h) Long-term stability of electrocatalytic AA oxidation at 50 mA cm-2 in 0.5 mol L?1 H2SO4 with 0.1 mol L?1 AA; the inset is the SEM images of PO-CP before and after AAOR for 20 h. (i) Content of various oxygenated groups at the Po-CP surface before and after the 20-h electrolysis test. The content of different OCGs equals the content of total oxygen from wide XPS spectra times the ratio of typical OCGs obtained from the high-resolution XPS of O 1s spectra.

Fig. 2. Oxygen-enhanced dehydrogenation kinetics. (a) High-resolution XPS of C 1s of XC 72, PO-XC 72, PO-XC 72-H2. (b,c) LSV curves of AAOR at XC 72 with different treatments. (d) Most stable configurations of the intermediates on the carbon surface. (e) Corresponding free-energy diagram for the AAOR on different OCG-decorated surfaces.

Fig. 3. Evaluation of hydrogen production capacity. (a) Comparison of the cell voltage to obtain a specific current density of prior works about H2 production based on organic oxidation; inset presents the catalysts couple. (b) Polarization curves for AAOR/HER in the electrolyzer. (c) Measured H2 production compared with theoretically calculated H2 quantity at 0.6 to 1.0 V. (d) Comparative analysis of the calculated electricity consumption for hydrogen production via our system and conventional water electrolysis. (e) Durability measurement of PO-CP || Pt/C couple for DHA and hydrogen production at 30 °C.

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强化脱氢动力学实现超低电池电压和大电流密度下抗坏血酸电氧化

Enhanced dehydrogenation kinetics for ascorbic acid electrooxidation with ultra-low cell voltage and large current density

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[1]	唐小龙, 李锋, 李方, 江燕斌, 余长林. 单原子催化剂在光催化和电催化合成过氧化氢中的研究进展[J]. 催化学报, 2023, 52(9): 79-98.
[2]	张季, 俞爱民, 孙成华. 非金属掺杂石墨烯异核双原子催化剂氮还原特性研究[J]. 催化学报, 2023, 52(9): 263-270.
[3]	胡金念, 田玲婵, 王海燕, 孟洋, 梁锦霞, 朱纯, 李隽. MXene负载3d金属单原子高效氮还原电催化剂的理论筛选[J]. 催化学报, 2023, 52(9): 252-262.
[4]	洪岩, 王琦, 阚子旺, 张禹烁, 郭晶, 李思琦, 刘松, 李斌. 电化学氮还原氨反应催化剂的最新研究进展[J]. 催化学报, 2023, 52(9): 50-78.
[5]	刘勇, 赵晓丽, 隆昶, 王晓艳, 邓邦为, 李康璐, 孙艳娟, 董帆. 原位构筑动态Cu/Ce(OH)_x界面用于高活性、高选择性和高稳定性硝酸盐还原合成氨[J]. 催化学报, 2023, 52(9): 196-206.
[6]	高晖, 张恭, 程东方, 王永涛, 赵静, 李晓芝, 杜晓伟, 赵志坚, 王拓, 张鹏, 巩金龙. 构建Cu台阶位促进电催化CO₂还原制醇类化学品的研究[J]. 催化学报, 2023, 52(9): 187-195.
[7]	王思恺, 闵祥婷, 乔波涛, 颜宁, 张涛. 单原子催化: 追寻催化领域的“圣杯”[J]. 催化学报, 2023, 52(9): 1-13.
[8]	邹心仪, 顾均. 酸性条件下二氧化碳高效电还原策略[J]. 催化学报, 2023, 52(9): 14-31.
[9]	乔蔚, 于立策, 常进法, 杨甫林, 冯立纲. MoSe₂纳米片耦合Pt纳米颗粒用于高效双功能催化甲醇辅助水电解制氢[J]. 催化学报, 2023, 51(8): 113-123.
[10]	王元男, 王立娜, 张可新, 徐靖尧, 武倩楠, 谢周兵, 安伟, 梁宵, 邹晓新. 钙钛矿氧化物在水裂解反应中的电催化研究[J]. 催化学报, 2023, 50(7): 109-125.
[11]	周纳, 王家志, 张宁, 王志, 王恒国, 黄岗, 鲍迪, 钟海霞, 张新波. 富含缺陷的Cu@CuTCNQ复合材料增强电催化硝酸盐还原成氨[J]. 催化学报, 2023, 50(7): 324-333.
[12]	李轩, 蒋兴星, 孔艳, 孙建桔, 胡琪, 柴晓燕, 杨恒攀, 何传新. GaN/In₂O₃的界面工程用于高效电催化CO₂还原制备甲酸[J]. 催化学报, 2023, 50(7): 314-323.
[13]	Sang Eon Jun, Sungkyun Choi, Jaehyun Kim, Ki Chang Kwon, Sun Hwa Park, Ho Won Jang. 用于电化学能量转换反应的非贵金属单原子催化剂[J]. 催化学报, 2023, 50(7): 195-214.
[14]	牛青, 米林华, 陈玮, 李秋军, 钟升红, 于岩, 李留义. 基于共价有机框架的单位点光(电)催化材料的研究进展[J]. 催化学报, 2023, 50(7): 45-82.
[15]	欧阳玲, 梁杰, 罗永嵩, 郑冬冬, 孙圣钧, 刘倩, Mohamed S. Hamdy, 孙旭平, 应斌武. 电催化合成氨的研究进展[J]. 催化学报, 2023, 50(7): 6-44.