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Comprehensive understanding of the thriving electrocatalytic nitrate/nitrite reduction to ammonia under ambient conditions

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Journal of Energy Chemistry 2024年第5期92卷 459-483页

作者： Xinying Zhao Yuzhuo Jiang Mengfan Wang Yunfei Huan Qiyang Cheng Yanzheng He Tao Qian Chenglin Yan Collaborative Innovation Center of Suzhou Nano Science and Technology College of EnergySoochow UniversitySuzhou 215006JiangsuChina School of Chemistry and Chemical Engineering Nantong UniversityNantong 226019JiangsuChina School of Petrochemical Engineering Changzhou UniversityChangzhou 213164JiangsuChina

Ammonia(NH_(3))is a multifunctional compound that is an important feedstock for the agricultural and pharmaceutical industries and attractive energy storage medium.At present,NH_(3)synthesis is highly dependent on the conventional Haber–Bosch process that operates under harsh conditions,which consumes large quantities of fossil fuels and releases a large amount of carbon dioxide.As an alternative,electrosynthesis is a prospective method for producing NH_(3)under normal temperature and pressure conditions.Although electrocatalytic nitrogen reduction to ammonia has attracted considerable attentions,the low solubility of N_(2)and high N≡N cracking energy render the achievements of high NH_(3) yield rate and Faradaic efficiency difficult.Nitrate and nitrite(NO_(x)^(-))are common N-containing pollutants.Due to their high solubilities and low dissociation energy of N=O,NO_(x)^(-)−are ideal raw materials for NH_(3) production.Therefore,electrocatalytic NO_(x)^(-)−reduction to NH_(3)(eNO_(x)RR)is a prospective strategy to simultaneously realise environmental protection and NH_(3) synthesis.This review offers a comprehensive understanding of the thriving eNO_(x)RR under ambient conditions.At first,the popular theory and mechanism of eNO_(x)RR and a summary of the measurement system and evaluation criteria are introduced.Thereafter,various strategies for developing NO_(x)−reduction catalysts are systematically presented and discussed.Finally,the challenges and possible prospects of electrocatalytic NO_(x)^(-1) reduction are outlined to facilitate energy-saving and environmentally friendly large-scale synthesis of NH_(3) in the future.

关键词： Electrocatalytic nitrate reduction Electrocatalytic nitrite reduction Ammonia synthesis Pollutant removal electrosynthesis

electrosynthesis of ^(15)N-labeled amino acids from ^(15)N-nitrite and ketonic acids

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Science China Chemistry 2023年第6期66卷 1854-1859页

作者： Yongmeng Wu Mengyang Li Tieliang Li Jinghui Zhao Ziyang Song Bin Zhang Department of Chemistry School of ScienceInstitute of Molecular PlusTianjin UniversityTianjin 300072China Tianjin Key Laboratory of Molecular Optoelectronic Science Key Laboratory of Systems Bioengineering(Ministry of Education)Tianjin UniversityTianjin 300072China

^(15)N isotope-labeled amino acids(^(15)N-amino acids)are crucial in the fields of biology,medicine,and chemistry.^(15)N-amino acids are conventionally synthesized through microbial fermentation and chemical reductive amination of ketonic acids methodologies,which usually require complicated procedures,high temperatures,or toxic cyanide usage,causing energy and environmental concerns.Here,we report a sustainable pathway to synthesize ^(15)N-amino acids from readily available ^(15)N-nitrite(^(15)NO_(2)-)and biomass-derived ketonic acids under ambient conditions driven by renewable electricity.A mechanistic study demonstrates a ^(15)N-nitrite→^(15)NH_(2)OH→^(15)N-pyruvate oxime→^(15)N-alanine reaction pathway for ^(15)N-alanine synthesis.Moreover,this electrochemical strategy can synthesize six ^(15)N-amino acids with 68%–95%yields.Furthermore,a ^(15)N-labeled drug of ^(15)N-tiopronin,the most commonly used hepatitis treatment drug,is fabricated using ^(15)N-glycine as the building block.Impressively,^(15)N sources can be recycled by the electrooxidation of ^(15)NH4^(+) to ^(15)NO_(2)-with a method economy.This work opens an avenue for the green synthesis of ^(15)N-labeled compounds or drugs.

关键词： green synthesis ^(15)N-labeled amino acids electrosynthesis C-N bond isotope labeling

electrosynthesis of hydroxylamine from nitrate reduction in water

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Science China Chemistry 2023年第6期66卷 1758-1762页

作者： Xianen Lan Chuanqi Cheng Chengying Guo Minghao Guo Tieliang Li Yongmeng Wu Yifu Yu Bin Zhang Institute of Molecular Plus Department of ChemistrySchool of ScienceTianjin UniversityTianjin 300072China Institute of New Energy Materials School of Materials Science and EngineeringTianjin UniversityTianjin 300072China Haihe Laboratory of Sustainable Chemical Transformations Tianjin 300192China

Hydroxylamine(NH_(2)OH),a vital but unstable industrial feedstock,is presently prepared under harsh conditions that cause environmental and energy concerns.Here,we report an electrochemical method to prepare oximes,which serve as precursors for NH_(2)OH after facile hydrolysis.The carbon-supported amorphous Mn electrocatalyst delivers a current density of~100 mA cm^(-2) with a Faradaic efficiency of 40.92%and a yield rate of 0.251 mmol cm^(-2)h^(-1) for formaldoxime(CH_(2)NOH)generation by using nitrate and formaldehyde as reactants.Formaldoxime can be easily released to produce NH_(2)OH via hydrolysis.Impressively,this method exhibits an economic advantage over conventional manufacturing based on techno-economic analysis.A series of control experiments,in situ characterizations,and theoretical simulations unveil the reaction mechanism via the spontaneous reaction between an aldehyde and*NH_(2)OH intermediate derived from nitrate electroreduction.The high activity of Mn originates from its inhibitory effects on the further reduction of key*NH_(2)OH intermediate.This strategy opens a sustainable and green way for NH_(2)OH synthesis under mild conditions using renewable energy.

关键词： electrosynthesis hydroxylamine nitrate reduction amorphous Mn reaction pathway

Coupling functional anodes with natural air-diffused cathodes enables highly efficient hydrogen peroxide electrosynthesis

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Journal of Zhejiang University-Science A(Applied Physics & Engineering) 2023年第4期24卷 377-386页

作者： Chen LING Aiping LIANG Chaolin LI Wenhui WANG School of Civil and Environmental Engineering Harbin Institute of TechnologyShenzhenShenzhen 518055China State Key Laboratory of Urban Water Resource and Environment School of EnvironmentHarbin Institute of TechnologyHarbin 150090 China

electrosynthesis of hydrogen peroxide(H_(2)O_(2))is a decentralized production method with excellent application prospects.Coupling anodes with cathodes can achieve highly efficient electrosynthesis of hydrogen peroxide.In this study,we prepared an anode for H_(2)O_(2) electrosynthesis via the two-electron water oxidation reaction(2e-WOR)by modifying carbon fiber paper with self-assembling monolayers.In addition,a natural air-diffused cathode loaded with polytetrafluoroethylene/carbon black using carbon cloth as substrate was prepared to combine with the modified anode to produce H_(2)O_(2) simultaneously.The total current efficiency of the anode and cathode reached 152.9%,and the H_(2)O_(2) production rate was as high as 38μmol/min at 2.8 V vs.reversible hydrogen electrodes(RHE)in a Nafion 117 membrane-separated electrolyzer.This work reported a novel carbon-based 2e-WOR catalyst and laid a theoretical foundation for the simultaneous electrosynthesis of H_(2)O_(2) with an anode and cathode.

关键词： Two-electron water oxidation Two-electron oxygen reduction Self-assembled membrane Hydrogen peroxide electrosynthesis

Recent developments in electrosynthesis of nitriles and electrocatalytic cyanations

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Journal of Energy Chemistry 2022年第7期31卷 542-575,I0014页

作者： Haiyan Hu Shanxuan Wu Fachao Yan Mohamed Makha Yuxia Sun Chen-Xia Du Yuehui Li State Key Laboratory for Oxo Synthesis and Selective Oxidation Suzhou Research Institute of LICPCenter for Excellence in Molecular SynthesisLanzhou Institute of Chemical Physics(LICP)Chinese Academy of SciencesLanzhou 730000GansuChina University of Chinese Academy of Sciences Zhengzhou 450001HenanChina College of Chemistry Zhengzhou UniversityBeijing 100049China

Nitrile compounds are a class of high-value chemicals and versatile intermediates which can easily be transformed into a variety of useful products bearing functional groups such as carboxyl, carbamoyl, aminomethyl, ketyl and heterocyclic derivatives. Various thermal catalytic cyanation procedures have been devised and scaled up industrially while developing alternative methods are actively pursued. The access to these classes of molecules electrochemically offers greener alternatives to their preparation. The development of electrochemical synthesis of cyano-containing compounds under mild conditions with low energy consumption will imminently become indispensable approaches for industrial production of nitriles. The electrochemical cyanation presents many challenges from the toxicity of cyanide to the development of catalysts and the design of electrochemical cells. Electrochemical cyanation reaction offers promise to conveniently accessing nitriles but still requires efficient electro-catalysts, safe protocols and scale up considerations. This review discusses recent progress in the field of electrochemical synthesis of nitrile compounds placing emphasis on electro-synthetic and electro-catalytic mechanism aspects while making reference to original works to highlight the progress in this area.

关键词： Cyano compounds Nitriles Cyanation electrosynthesis Electrocatalysis

Cobalt-iron oxide/black phosphorus nanosheet heterostructure:electrosynthesis and performance of(photo-)electrocatalytic oxygen evolution

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Nano Research 2023年第5期16卷 6057-6066页

作者： Man Zhao Xiaoru Cheng He Xiao Jianru Gao Shoufeng Xue Xiaoxia Wang Haishun Wu Jianfeng Jia Nianjun Yang Key Laboratory of Magnetic Molecules&Magnetic Information Materials Ministry of Education The School of Chemical and Material ScienceShanxi Normal UniversityTaiyuan 030000China Institute of Materials Engineering University of SiegenSiegen 57076Germany

Highly active,stable,and cut-price(photo-)electrocatalysts are desired to overwhelm high energy barriers for anodic oxygen evolution reaction processes.Herein,a heterostructure of cobalt-iron oxide/black phosphorus nanosheets is in-situ synthesized via a facile and novel three-electrode electrolysis method.Bulky black phosphorus is exfoliated into its nanosheets at the cathode while the CoFe oxide is derived directly from the metal wire anode during the electrolysis process.This heterostructure exhibits excellent electrocatalytic oxygen evolution reaction(OER)performance,and the overpotential at 10 mA·cm^(−2)is 51 mV lower than that of the commercial RuO_(2)catalyst.Its superior OER performance stems from the favorable adsorption behavior and an enlarged electrochemical active surface area of the catalyst.To reveal the origin of excellent OER performance from the point of adsorption strength of OH*,methanol oxidation reaction(MOR)test is applied under the identified OER operating conditions.Further introduction of light illumination enhances the OER activity of this heterostructure.The overpotential drops down to 280 mV,benefiting from pronounced photochemical response of black phosphorus nanosheets and iron oxide inside the heterostructure.This work develops a new electrochemical method to construct high performance and light-sensitive heterostructures from black phosphorus nanosheets for the OER.

关键词： electrosynthesis oxygen evolution reaction black phosphorus cobalt oxide iron oxide

Metal, iodine and oxidant-free electrosynthesis of substituted indoles from 1-(2-aminophenyl)alcohols

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Green Synthesis and Catalysis

Green Synthesis and Catalysis 2023年第4期4卷 311-315页

作者： Chengcheng Yuan Xiangxing Huang Yi Lu Zheng Fang Chengkou Liu Beining Chen Kai Guo College of Biotechnology and Pharmaceutical Engineering Nanjing Tech UniversityNanjing 211816China Department of Chemistry University of SheffieldSheffield S37HFUK State Key Laboratory of Materials-Oriented Chemical Engineering Nanjing Tech UniversityNanjing 211816China

A green and straightforward electrosynthesis of substituted indoles has been developed through dehydration and intramolecular dehydrogenative C–N bond-forming radical cross-coupling from 1-(2-aminophenyl)alcohols under metal,iodine and oxidant-free conditions.This electrochemical indole synthesis strategy has an excellent functional group,water and air tolerance.And,a possible cyclization process was proposed based on the radicaltrapping,intermediate verification,cyclic voltammetry,EPR and control experiments.

关键词： electrosynthesis Metal Iodine and oxidant-free C-N coupling Indoles N-centered radicals

electrosynthesis of Arylsulfonamides from Amines and Sodium Sulfinates Using H2O-Nal as the Electrolyte Solution at Room Temperature

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Chinese Journal of Chemistry 2016年第12期34卷 1277-1282页

作者： Chen Zhang Yibin Chen Gaoqing Yuan Key Laboratory of Functional Molecular Engineering of Guangdong Province School of Chemistry and Chemical Engineering South China University of Technolog) Guangzhou Guangdong 510640 China

With H2O as the solvent and NaI as the supporting electrolyte, a green and efficient electrochemical route has been developed to synthesize arylsulfonamides via I2 electrogenerated in situ at a graphite anode to promote the reaction of sodium sulfinates with aromatic or aliphatic primary and secondary amines. The target products could be obtained in good to excellent yields at room temperature.

关键词： sulfonamindes I2-promoted sodium sulfinates electrosynthesis

electrosynthesis of hierarchical NiLa-layered double hydroxide electrode for efficient oxygen evolution reaction

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Journal of Energy Chemistry 2019年第6期28卷 125-129页

作者： Shan Jiang Yunke Liu Wenfu Xie Mingfei Shao State Key Laboratory of Chemical Resource Engineering Beijing University of Chemical Technology

Oxygen evolution reaction(OER) is a key process for electrochemical water splitting due to its intrinsic large overpotential. Recently, layered double hydroxides(LDHs), especially Ni Fe-LDH, have been regarded as highly performed electrocatalysts for OER in alkaline condition. Here we first present a new class of Ni La-LDH electrocatalyst synthesized by an electrochemical process for efficient water splitting. The as-prepared NiL a-LDH nanosheet arrays(NSAs) give remarkable electrochemical activity and durability under alkaline environments, with a low overpotential of 209 mV for OER to deliver a current density of 10 mA cm^-2, surpassing most of previous reported LDHs eletrocatalysts. The presence of NiLa-LDH in this work extends the studies about LDHs-based electrocatalysts, which will benefit the development of electrochemical energy storage and conversion systems.

关键词： Layered double hydroxides Oxygen evolution reaction Lanthanides electrosynthesis