Novel Porous Melamine Foam Loaded with MnCe for Highly Selective Electrocatalytic CO2 to Formic Acid

doi:10.6023/A23120529

Abstract

A previously unreported CO₂ reduction electrocatalyst consisting of MnCe as the active site and melamine foam (MS) as the carrier precursor is proposed. The MS were prepared into carbonized melamine foam (CMS) and graphene oxide- activated melamine foam (GOMS) by activation, respectively. And Mn and Ce were impregnated on the above substrates to synthesize MnCe-CMS and MnCe-GOMS catalysts for the electrocatalytic CO₂ reduction to formic acid. It was found that MnCe-MS (MnCe-CMS and MnCe-GOMS) had a wide potential range (–0.2~–3 V vs. RHE) and better formic acid production ability. Among them, the Faraday efficiency of formic acid (FE_f) on MnCe-CMS was 63.04% at –0.4 V, and the yield rate of formic acid (Y_f) was 470.89 μg•h^–1•cm^–2 at –3.0 V. MnCe-GOMS showed better electrocatalytic activity, with a FE_f of 75.72% at –0.6 V (when the Y_f=661.99 μg•h^–1•cm^–2), and optimal Y_f of 746.9 μg•h^–1•cm^–2 at –0.8 V. In addition, no other products (e.g., acetic acid, methanol, ethanol, CO, methane) were detected during the reaction, suggesting that MnCe-MS has a good formic acid selectivity. Compared with the MnCe-CC, which are based on the commonly used carbon cloth (CC) as a carrier, the Y_f of MnCe-CMS and MnCe-GOMS were increased to 2.3 and 2.8 times, and the FE_f were increased to 2.3 and 2.5 times, respectively, at the optimal potential of MnCe-CC of –0.4 V. This is attributed to the rich pore structure and large electrochemical surface area of the MS material, which can easily form carbon defects during the preparation, thus favoring the adsorption of CO₂. Moreover, under the joint action of Mn and Ce, it effectively promotes electron transport, inhibits the competition reaction of hydrogen precipitation, and forms oxygen vacancies, which is conducive to the adsorption, activation and conversion of CO₂, thus promoting the formation of formic acid.

Key words: electrocatalytic CO₂ reduction reaction, formic acid, Mn, Ce, melamine foam, graphene oxide activation, high temperature carbonization

Cite this article

Yaru Lei, Tingkai Xiong, Xiangtao Yu, Xiubing Huang, Xiaolong Tang, Honghong Yi, Yuansong Zhou, Shunzheng Zhao, Long Sun, Fengyu Gao. Novel Porous Melamine Foam Loaded with MnCe for Highly Selective Electrocatalytic CO₂ to Formic Acid[J]. Acta Chimica Sinica, 2024, 82(4): 396-408.

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Catalysts	Onset potential (V vs. RHE)	exit potential (V vs. RHE)	Selection of experimental sites (V vs. RHE)	Maximum yield rate/ (μg•h^–1•cm^–2)	Optimum FE_f/%
MnCe-GOMS	–0.06	–2.99	–0.2, –0.4, –0,5, –0.6, –0.8, –1.0, –2.0, –2.5	746.92 (–0.8 V)	75.72 (–0.6 V)
MnCe-CMS	–0.13	–3.1	–0.2, –0.4, –1.0, –2.0, –3.0	470.89 (–3.0 V)	63.04 (–0.4 V)
MnCe-CC	0.58	–1.06	0.0, –0.2, –0.4, –0.8, –1.0	78.69 (–0.4 V)	64.14 (0 V)
MnCe-CF	0.65	–0.23	0.0, –0.1, –0.2	489.62 (–0.2 V)	11.67 (0 V)
MnCe-NF	0.43	–0.74	–0.4, –0.5, –0.6, –0.7	542.69 (–0.4 V)	41.47 (–0.4 V)

Catalysts	Onset potential (V vs. RHE)	exit potential (V vs. RHE)	Selection of experimental sites (V vs. RHE)	Maximum yield rate/ (μg•h^–1•cm^–2)	Optimum FE_f/%
MnCe-GOMS	–0.06	–2.99	–0.2, –0.4, –0,5, –0.6, –0.8, –1.0, –2.0, –2.5	746.92 (–0.8 V)	75.72 (–0.6 V)
MnCe-CMS	–0.13	–3.1	–0.2, –0.4, –1.0, –2.0, –3.0	470.89 (–3.0 V)	63.04 (–0.4 V)
MnCe-CC	0.58	–1.06	0.0, –0.2, –0.4, –0.8, –1.0	78.69 (–0.4 V)	64.14 (0 V)
MnCe-CF	0.65	–0.23	0.0, –0.1, –0.2	489.62 (–0.2 V)	11.67 (0 V)
MnCe-NF	0.43	–0.74	–0.4, –0.5, –0.6, –0.7	542.69 (–0.4 V)	41.47 (–0.4 V)

Adsorption site types		Weak adsorption		Medium adsorption		Strong adsorption	Amount
Adsorption site types		1# (30~180 ℃)	2# (180~350 ℃)	3# (350~430 ℃)	4# (400~600 ℃)	5# (600~800 ℃)	Amount
MnCe-CMS	Area	34.45	14.98	3.10	35.42	95.67	183.62
MnCe-CMS	Proportion%	18.76	8.16	1.69	19.29	52.10	100
MnCe-GOMS	Area	9.28	28.01	94.40	101.29	24.48	248.18
MnCe-GOMS	Proportion%	3.60	10.88	36.67	39.34	9.51	100

Adsorption site types		Weak adsorption		Medium adsorption		Strong adsorption	Amount
Adsorption site types		1# (30~180 ℃)	2# (180~350 ℃)	3# (350~430 ℃)	4# (400~600 ℃)	5# (600~800 ℃)	Amount
MnCe-CMS	Area	34.45	14.98	3.10	35.42	95.67	183.62
MnCe-CMS	Proportion%	18.76	8.16	1.69	19.29	52.10	100
MnCe-GOMS	Area	9.28	28.01	94.40	101.29	24.48	248.18
MnCe-GOMS	Proportion%	3.60	10.88	36.67	39.34	9.51	100

Catalysts	Element content/%					Atomic ratio/%
Catalysts	C	N	O	Mn	Ce	Mn³⁺/Mn	Ce³⁺/Ce	O_α/O	O_β/O
MnCe-CC	60.10	0.37	30.33	3.60	5.57	30.75	9.30	46.81	53.19
MnCe-CMS	38.00	1.20	46.55	8.67	5.58	32.29	11.09	37.69	26.81
MnCe-GOMS	55.87	4.49	33.22	4.68	4.49	40.45	24.92	48.62	11.76

新型多孔三聚氰胺负载MnCe用于高选择性电催化CO₂产甲酸

Novel Porous Melamine Foam Loaded with MnCe for Highly Selective Electrocatalytic CO₂ to Formic Acid

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Fig. & Tab. 17

References 57

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Parameters	MnCe-CC	MnCe-CMS	MnCe-GOMS
b/(mV•dec^–1)	–396	–1750	–1169
i₀/(mA•cm^–2)	0.042	0.783	0.575
k⁰/(cm•s^–1)	7.0×10^–6	1.23×10^–5	9.1×10^–6
α	–0.149	–0.034	–0.051

Catalysts	Carrier	Advantages	Disadvantages	Potentiostatic properties
MnCe-CMS	Melamine foam (MS)	High FE, high yield and low cost	Low conductivity and poor stability	Wider potential range (–0.2~–3 V)
MnCe-GOMS	Melamine foam (MS)	High FE, high yield and low cost	Low conductivity and poor stability	Wider potential range (–0.2~–3 V)
MnCe-CC	Carbon cloth (CC)	Higher FE	Low yield	Narrower potential range (0~–1 V)
MnCe-CF	Metal foams	High conductivity and higher yield	Low FE, severe HER competitive response and poor reproducibility	Narrow potential range (<–0.7 V)
MnCe-NF	Metal foams	High conductivity and higher yield		Narrow potential range (<–0.7 V)

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新型多孔三聚氰胺负载MnCe用于高选择性电催化CO2产甲酸