Paired Electrolysis for Inorganic Small Molecules Reduction Coupled with Alternative Oxidation Reactions

doi:10.6023/cjoc202312013

Abstract

Electrocatalytic reduction and oxidation processes offer an efficient and sustainable platform for synthesizing valuable chemicals. Particularly, coupling the cathodic reduction and anodic oxidation processes via paired electrolysis can efficiently lower the reaction overpotential as well as selectively synthesize various high-value chemicals, which has drawn ever-growing attention in recent years. Herein, the recent advancements in paired electrolysis are summarized, focusing on the reduction of inorganic small molecules including carbon dioxide, nitrogen-containing substances, and water coupled with alternative oxidation reactions. Additionally, major challenges as well as potential solutions of paired electrolysis are proposed in this review, which may provide some guidance for researchers in the future.

Key words: paired electrolysis, inorganic small molecules reduction, alternative oxidation reaction, coupling

Cite this article

Fangying Duan, Menglei Yuan, Jian Zhang. Paired Electrolysis for Inorganic Small Molecules Reduction Coupled with Alternative Oxidation Reactions[J]. Chinese Journal of Organic Chemistry, 2024, 44(3): 809-824.

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Fig. & Tab. 8

Figure 1. Three types of paired electrolysis with internal rela- tionships (A) parallel, (B) sequential, and (C) convergent electrochemical processes

Cathode reaction	Anode reaction	Electrocatalyst		Electrolyte	Product		FE (%) C/A	Ref.
Cathode reaction	Anode reaction	Cathode	Anode	Electrolyte	Cathode	Anode	FE (%) C/A	Ref.
CO₂RR	HMFOR	BiO_x	NiO NPs	CO₂-saturated 0.5 mol/L KHCO₃	HCOOH	FDCA	81/36	[48]
		PdO_x/ZIF-8	PdO	[Bmim]BF₄ (0.5 mol/L)/CH₃CN＋H₂SO₄ (0.5 mol/L)/CH₃CN (6.0 mol/L)	CO	Organic acid	97/84.3	[49]
		Bi-FDCA MOF	Ni(OH)₂	CO₂-saturated 0.1 mol/L KHCO₃＋0.1 mol/L KOH and 5 mmol/L HMF	HCOOH	FDAC	95.6/75	[51]
	GOR	InBi NP’s	Ni₃S₂	1 mol/L KOH＋1 mol/L KOH/0.05 mol/L C₃H₈O₃	HCOOH	HCOOH	98/83	[54]
	GOR	BiOBr	Ni_xB	1 mol/L KOH＋1 mol/L KOH/1 mol/L C₃H₈O₃	HCOOH	HCOOH	96/45	[55]
	MOR	SnO₂	CuO	1 mol/L KHCO₃＋1 mol/L KOH/1 mol/L CH₃OH	HCOOH	HCOOH	80.5/91.3	[61]
		CuSn alloy		CO₂-saturated 0.5 mol/L KHCO₃＋1 mol/L KOH/ 1 mol/L CH₃OH	HCOOH	HCOOH	93.7/96.7	[66]
		Sn-GDE	Pt/PtO_x	1 mol/L KHCO₃＋0.5 mol/L H₂SO₄/8 mol/L CH₃OH	HCOOH	HCOH	—	[69]
	FOR	BiOCl	Cu₂O	CO₂-saturated 0.5 mol/L KHCO₃＋1 mol/L KOH/ 0.1 mol/L HCOH	HCOOH	HCOOH	>180	[52]
	FOR	Cu@Sn NWs	MnO₂	0.5 mol/L KHCO₃＋0.1 mol/L Na₂SO₄/ 5 mmol/L HCOH	CO	HCOOH	93/—	[68]

Table 1. Summary of paired CO2RR with organic oxidation reactions recently reported.

Figure 2. (A) Paired electrolysis of CO2 and biomass. Reproduced with permission.[48] Copyright 2020, Journal of Physical Chemistry Letters. (B) The comparison between a traditional single reaction and paired electrolysis system. (C) Mechanism study of paired CO2RR and HMFOR. Reproduced with permission.[49] Copyright 2022, ACS Sustainable Chemistry & Engineering. (D) Diagrammatic sketch of the strategy employed in this work to construct paired electrolysis reactions with the inner relationship. (E) Product distribution after the electrolysis. Reproduced with permission.[51] Copyright 2022, ChemCatChem. (F) Product distribution of half-cell measurements for BiOBr cathode. (G) Obtained formate selectivity using the paired electrolyzer for the BiOBr-GDE cathode (blue) and NixB anode (yellow) FE at different current densities for 2.5 h. Reproduced with permission.[55] Copyright 2022, ChemSusChem

Figure 3. (A) Formate production rate for electrolysis experiments with 2.5 mol/L formate at the start and the theoretic formate production when 100% FE is assumed (red line). Reproduced with permission.[54] Copyright 2023, ChemPlusChem. (B) Stability test for CO2RR-MOR couple under a cell voltage of 3.2 V. Reproduced with permission.[66] Copyright 2022, Nano Energy. (C) Anodic current efficiency for methanol oxidation on Pt at a current density of 25 mA?cm－2 and (D) on PtOx at 75 mA?cm－2. (E) Comparison of the products formed per electrical energy input for the three paired processes. For each process two bars are shown, indicating the energy efficiency at the start (up to the first sample taken) and at the end of the experiment (up to the last sample taken). The total amount of products formed is divided into HCOOH produced at the cathode (light blue, hatched), as well as HCOOH and CH2O produced at the anode (light gray and dark gray, respectively). Reproduced with permission.[69] Copyright 2023, ACS Sustainable Chemistry & Engineering

Cathode substrate	Electrocatalyst		Innovation point	Ref.
Cathode substrate	Cathode	Anode	Innovation point	Ref.
$\mathrm{NO}_{3}^{-}$	Ni₃Se₄		Design of catalyst (paired with BOR)	[94]
	Porous foam iron	MMO	Mechanism analysis: intermediate	[99]
	A polytetrafluoroethylene film was coated with a CuO catalytic layer		A prototype electrified synchronous electrochemical reduction	[101]
	Pd Cu/GAC		EPBMR	[102]
	Cu₉Ni/C	Pt₉Ir/C	Symmetric square wave pulse technology, paired with AOR	[103]
NO_x	—	Graphite felt GDE (electrode)	A two-stage oxidation absorption technique	[109]
NO_x	AC (electrode)	DSA (electrode)	MLPE	[112]

Table 2. Summary of paired electrolysis with $\mathrm{NO}_{3}^{-}$ and NOx as cathode substrates in recent years.

Figure 4. (A) Digital photo of the actual paired electrolysis to co-upgrade nitrate and benzylamine to ammonium and benzonitrile. (B) Energy consumption per kg of NH3 produced. (C) Product value per kWh (green) and the cost of the reactant (blue) (color online). Reproduced with permission.[94] Copyright 2023, Science China Chemistry. (D) Mechanism of the electrocatalytic reduction of the iron catalyst on the cathode.Reproduced with permission.[99] Copyright 2021, Applied Catalysis B: Environmental. (E) The working diagram and major electrode reactions of the electrified membrane flow cell. (F) The evolution of various Nspecies over time of actual chemical industrial wastewater. Reproduced with permission.[101] Copyright 2022, Environmental Science & Technology. (G) Schematic diagram of the EPBMR for nitrate removal. Reproduced with permission.[102] Copyright 2022, Separation and Purification Technology. (H) Pulse electrolysis. (I) The concentration of ammonia and nitrate during the pulse electrolysis process. Reproduced with permission.[103] Copyright 2023, Journal of the Electrochemical Society

Figure 5. (A) Effect of time on NOx removal efficiency of different electrolysis systems. Reproduced with permission.[109] Copyright 2022, Separation and Purification Technology. (B) Conversion efficiency of complex NO in different electrolysis systems. Reproduced with permission.[112] Copyright 2022, Industrial & Engineering Chemistry Research. (C) Polarization curves of Ni-VN/NF couple in 1.0 mol/L KOH with/without 10×10－3 mol/L HMF. (D) Electron density difference plots of the NiOOH-VN and Ni-VN interface, respectively. Reproduced with permission.[116] Copyright 2023, Nano Micro Small. (E) Current density profile vs time and the FEs toward FDCA during continuous operation for 100 h. Reproduced with permission.[119] Copyright 2023, Journal of the American Chemical Society. (F) LSV of two NF@Mo-Ni0.85Se electrode coupling systems obtained in the absence (black) and presence (red) of 10 mmol/L HMF in 1.0 mol/L KOH (H-cell). Reproduced with permission.[122] Copyright 2021, Chemical Engineering Journal. (G) Energy diagrams of CoP-p and NFP before and after contact. Reproduced with permission.[124] Copyright 2023, ACS Applied Nano Materials. (H) Performance of the NiFe2O4/NF||NiFe2O4/NF catalytic electrodes for HER-SMOR electrolysis in seawater: I-t curves of at 2.0 V. Reproduced with permission.[126] Copyright 2023, Chemical Engineering Journal

Cathode reaction	Anode reaction	Electrocatalyst		Voltage @10 mA•cm^－2/V	Tafel slope/(mV•dec^－1)	Stability	Ref.
Cathode reaction	Anode reaction	Cathode	Anode	Voltage @10 mA•cm^－2/V	Tafel slope/(mV•dec^－1)	Stability	Ref.
HER	HMFOR	Ni-VN		1.426	45/25	10 cycle	[116]
		Rh-O₅/Ni (Fe)		1.32	31.5/55	>100 h	[119]
		Co-Ni_xP@C hybrid		1.4	140.6/—	6 cycle	[120]
		Co₄N/NC@CC		1.38	69.2/—	6 cycle	[121]
		NF@Mo-Ni_0.85Se		1.5 (@50 mA•cm^－2)	98.98/—	6 cycle	[122]
		NiMo₃S₄	NiMo₃S₄-R	1.414	28.8/36.5	6 cycle	[123]
	MOR	Co-Ni-P		1.45 (@100 mA•cm^－2)	67.7/22.2	20 h	[124]
	MOR	NiFe₂O₄		1.55	—/28.5	>48 h	[126]
	UOR	NiCoP	NiCo MOF	1.447	218/88	24 h	[135]
		Ni-MOF@Ni-NCNT		1.33	—/38.8	>20 h	[136]
		Ce-Ni₂P		1.51	78.4/53.7	>12 h	[137]
		Mo-NT@NF		1.57 (@50 mA•cm^－2)	89/—	90 h	[138]
		Fe-Co_0.85Se/FeCo LDH		1.57 (@300 mA•cm^－2)	43.9/40	>60 h	[141]
		CoNi@CN‐CoNiMoO		1.58 (@500 mA•cm^－2)	61/30	120 h	[142]
		NiFeSP		1.938 (@500 mA•cm^－2)	38.2/76.8	1000 h	[146]

Table 3. Summary of paired HER with organic oxidation reactions recently reported

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无机小分子还原耦合选择性氧化反应的成对电解