贫燃/富燃循环气氛下原位活化Pd负载钙钛矿催化剂促进NOx还原消除

doi:10.1016/S1872-2067(20)63694-4

催化学报 ›› 2021, Vol. 42 ›› Issue (5): 795-807.DOI: 10.1016/S1872-2067(20)63694-4

贫燃/富燃循环气氛下原位活化Pd负载钙钛矿催化剂促进NO_x还原消除

赵东越^a, 杨岳溪^a, 高中楠^a, 尹萌欣^a, 田野^a, 张静^b, 姜政^c, 于晓波^d, 李新刚^a^,^*()

^a天津大学化工学院, 天津化学化工协同创新中心, 化学工程联合国家重点实验室, 天津市应用催化科学与工程重点实验室, 天津300072
^b中国科学院高能物理研究所, 北京100049
^c中国科学院上海应用物理研究所上海同步辐射光源, 上海201800
^d吉林化工学院材料科学与工程学院, 吉林吉林132022

收稿日期:2020-04-26 接受日期:2020-04-26 出版日期:2021-05-18 发布日期:2021-01-29
通讯作者: 李新刚
基金资助:
国家自然科学基金项目(21878213);吉林省教育厅“十三五“科学研究规划项目(JJKH20180554KJ);高等学校学科创新引智计划项目(B06006)

Promoting NO_x reduction via in situ activation of perovskite supported Pd catalysts under alternating lean-burn/fuel-rich operating atmospheres

Dongyue Zhao^a, Yuexi Yang^a, Zhongnan Gao^a, Mengxin Yin^a, Ye Tian^a, Jing Zhang^b, Zheng Jiang^c, Xiaobo Yu^d, Xingang Li^a^,^*()

^aCollaborative Innovation Center of Chemical Science and Engineering (Tianjin), Tianjin Key Laboratory of Applied Catalysis Science and Technology, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China
^bInstitute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China
^cShanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China
^dCollege of Materials Science and Engineering, Jilin Institute of Chemical Technology, Jilin 132022, Jilin, China

Received:2020-04-26 Accepted:2020-04-26 Online:2021-05-18 Published:2021-01-29
Contact: Xingang Li
About author:^* E-mail: xingang_li@tju.edu.cn
Supported by:
National Natural Science Foundation of China(21878213);Scientific Research Project of Jilin Provincial Education Department(JJKH20180554KJ);Program of Introducing Talents of Disciplines to China Universities(B06006)

摘要/Abstract

摘要：

稀燃发动机通过提高空燃比来改善燃油经济性, 减少CO₂排放. 但由于空燃比较高, 稀燃发动机尾气中的NO_x无法通过传统的三效催化技术有效消除. 为了解决这一问题, 适用于稀燃条件的NO_x储存还原(NSR)技术得到了开发和应用. 传统的NSR催化剂以贵金属Pt作为其氧化还原活性中心. Pt基催化剂具有较高的NO_x消除活性, 然而热稳定性差, 高温下易团聚失活. 据报道, Pd具有比Pt更好的热稳定性和抗硫性, 且能够在更低的温度下活化还原剂, 促进NO_x还原. 但De-NO_x反应中的活性Pd物种至今仍无定论, 这对设计高效的Pd基NSR催化剂提出了挑战.

本文设计制备了具有高活性的Pd负载型钙钛矿催化剂(Pd-La_0.7Sr_0.3MnO₃). 其中钙钛矿组分的加入提高了Pd基催化剂的NO氧化能力和热稳定性, 并提供了可用于NO_x储存的碱性位点. 通过调节金属-载体相互作用, 使Pd催化剂在NSR反应气氛下发生了自活化现象, 活化后催化剂的NO_x消除活性由56.1%提高到90.1%, 同时副产物N₂O的选择性降低. XRD、XAFS和XPS等表征结果显示, 在反应气氛下催化剂中的Pd²⁺被部分还原为高活性的Pd⁰物种. 相较于Pd²⁺, Pd⁰表现出更强的活化C₃H₆的性能, 从而提高了催化剂在富燃阶段的NO_x还原效率. 结合XPS、CO化学吸附和动力学的实验结果, 计算得出Pd⁰位点的NO_x还原速率是Pd²⁺位点的8倍, 从实验现象和动力学计算两个角度分别证明Pd⁰物种具有更优异的NO_x还原活性.

然而, Pd⁰物种的生成需要适当强度的金属-载体相互作用. 通过与传统的Pd/BaO/Al₂O₃催化剂进行对比研究, 发现金属-载体相互作用过强时, 在富燃阶段Pd²⁺物种难以被还原, 且还原得到的Pd⁰物种并不稳定, 会在随后的贫燃阶段被快速重新氧化为Pd²⁺. 强相互作用虽然可以降低Pd物种粒径, 提高Pd的分散度, 但由于无法产生高活性的Pd⁰物种, 催化剂的NO_x消除性能显著降低. 此外, 相较于传统的Pd/BaO/Al₂O₃和Pt/BaO/Al₂O₃催化剂, Pd负载型钙钛矿催化剂具有更为优异的NO氧化能力, 且储存位碱性适中, 因而表现出更强的抗H₂O、CO₂和SO₂的性能, 具有良好的应用前景. 本文的结果说明了金属-载体相互作用对催化剂活性的显著影响, 同时也为理解和设计应用于动态氧化/还原气氛的金属催化剂提供了新的思路.

关键词: 贫燃, 氮氧化物还原, 金属-载体相互作用, 原位活化, 钯

Abstract:

Herein, we report the excellent De-NO_x performance of La_0.7Sr_0.3MnO₃ (LSM) perovskite-supported Pd catalysts (Pd-LSM) in alternating lean-burn/fuel-rich atmospheres using C₃H₆ as reductant and describe the in situ activation of the Pd catalysts via metal-support interaction (MSI) tuning. The NO_x reduction conversion of the Pd-LSM catalyst increased significantly from 56.1% to 90.1% and the production of N₂O was suppressed. Our results demonstrated that this behavior was mainly attributed to the in situ transformation of Pd²⁺ into Pd⁰ during the reaction. The generated Pd⁰ species could readily activate the C₃H₆ reductant and achieve an eight-fold higher turnover frequency than Pd²⁺ for the reduction of NO_x. Moreover, excessive MSIs inhibited the in situ generation of Pd⁰, and thereby, lowered the De-NO_x activity of the catalyst even at high Pd dispersion. In addition, the Pd-LSM catalysts exhibited much higher S tolerance than conventional Al₂O₃-supported catalysts. Our study provides a new approach for analyzing and designing highly active metal catalysts operated under dynamic alternating oxidizing/reducing atmospheric conditions.

Key words: Lean-burn, NO_x reduction, Metal-support interactions, In situ activation, Pd

赵东越, 杨岳溪, 高中楠, 尹萌欣, 田野, 张静, 姜政, 于晓波, 李新刚. 贫燃/富燃循环气氛下原位活化Pd负载钙钛矿催化剂促进NO_x还原消除[J]. 催化学报, 2021, 42(5): 795-807.

Dongyue Zhao, Yuexi Yang, Zhongnan Gao, Mengxin Yin, Ye Tian, Jing Zhang, Zheng Jiang, Xiaobo Yu, Xingang Li. Promoting NO_x reduction via in situ activation of perovskite supported Pd catalysts under alternating lean-burn/fuel-rich operating atmospheres[J]. Chinese Journal of Catalysis, 2021, 42(5): 795-807.

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图/表 15

Fig. 1. XRD patterns of the fresh La0.7Sr0.3MnO3 (1), fresh sol-gel-prepared La0.7Sr0.3MnO3-supported Pd (2), and fresh wet-impregnation-prepared La0.7Sr0.3MnO3-supported Pd (3) catalysts.

Table 1 Physicochemical properties and De-NOx activities of the catalysts at 350 °C.

Catalyst	Pd content ^a (wt%)	Specific surface area (m² g^-1)	NO_x storage efficiency ^b(%)	NO_x reducing efficiency ^b (%)	NO_x removal percentage ^b (%)	N₂O selectivity ^c (%)
LSM ^d	—	14.3	59.0	58.3	34.4	2.7
Pd-LSM-SG ^e	2.1	14.9	98.9	91.1	90.1	2.6
Pd-LSM-IM ^f	2.1	13.4	97.2	74.0	72.0	5.0

Fig. 2. Normalized Pd K-edge X-ray absorption near-edge structure spectra (a) and radial distribution function profiles (b) of the Pd-foil (1), PdO (2), fresh sol-gel-prepared La0.7Sr0.3MnO3-supported Pd (3), and fresh wet-impregnation-prepared La0.7Sr0.3MnO3-supported Pd (4) catalysts.

Fig. 3. Pd 3d (a) and Mn 2p (b) XPS profiles of the fresh sol-gel-prepared La0.7Sr0.3MnO3-supported Pd (1) and fresh wet-impregnation-prepared La0.7Sr0.3MnO3-supported Pd (2) catalysts.

Table 2 Chemical states of the Pd and Mn species in the fresh and activated catalysts determined from the XANES and XPS results.

Catalyst	XANES		XPS
Catalyst	Pd⁰ (%)	Pd²⁺ (%)	Pd⁰ (%)	Pd²⁺ (%)	Mn³⁺ (%)	Mn⁴⁺ (%)
Fresh Pd-LSM-SG	100	0	100	0	57.4	42.6
Fresh Pd-LSM-IM	100	0	100	0	66.5	33.5
Activated Pd-LSM-SG	53.0	47.0	43.6	56.4	58.0	42.0
Activated Pd-LSM-IM	6.0	94.0	0	100	67.1	32.9

Fig. 4. H2-TPR profiles (a) and magnified area marked with a dashed square (b) in (a). (1) PdO; (2) fresh pure La0.7Sr0.3MnO3; (3) fresh sol-gel-prepared La0.7Sr0.3MnO3-supported Pd; (4) fresh wet-impregnation-prepared La0.7Sr0.3MnO3-supported Pd catalysts.

Fig. 5. (a) De-NOx activity of La0.7Sr0.3MnO3 (LSM) (1), sol-gel-prepared La0.7Sr0.3MnO3-supported Pd (Pd-LSM-SG) (2), and wet-impregnation-prepared La0.7Sr0.3MnO3-supported Pd (Pd-LSM-IM) (3) at 200-450 °C. (b) Time evolution of the De-NOx activity of LSM (1), Pd-LSM-SG (2), Pd-LSM-IM (3), and pretreated Pd-LSM-SG (4) at 350 °C. Reaction conditions: lean-burn phase: 50 s, 400 ppm NO/5% O2/N2; fuel-rich phase: 10 s, 1000 ppm C3H6/N2; space velocity: 120 000 mL g-1 h-1.

Fig. 6. (a) XRD patterns of the fresh sol-gel-prepared Pd-LSM-SG (1), activated Pd-LSM-SG (2), fresh Pd-LSM-IM (3), and activated Pd-LSM-IM (4); Normalized Pd K-edge X-ray absorption near-edge structure spectra (b) and radial distribution functions (c) of Pd foil (1), PdO (2), activated Pd-LSM-SG (3), activated Pd-LSM-IM (4), and sample (3) oxidized under lean-burn atmosphere at 350 oC for 8 min (5).

Fig. 7. Pd 3d XPS profiles of fresh Pd/BaO/Al2O3 (1), activated Pd/BaO/Al2O3 (2), Pd/BaO/Al2O3 reduced in 1000 ppm C3H6/N2 at 350 °C for 3 min (3), and sample (3) after five NOx storage and reduction cycles (4).

Fig. 8. (a) C3H6 oxidation profiles of the fresh Pd-LSM-SG (1), activated Pd-LSM-SG (2), fresh Pd-LSM-IM (3), activated Pd-LSM-IM catalysts (4), and fresh pure La0.7Sr0.3MnO3 (5). (b) De-NOx reaction at 200 °C over the fresh Pd-LSM-SG (1), activated Pd-LSM-SG (2), fresh Pd-LSM-IM (3), and activated Pd-LSM-IM (4) catalysts.

Table 3 Surface Pd contents and kinetic results at 200 °C.

Catalyst	R(mol g^-1 s^-1 × 10^-8)	Exposed Pd atoms ^a(mol g^-1 s^-1 × 10^-5)	Pd dispersion (%)	Pd TOF(s^-1 × 10^-3)	Pd²⁺ TOF ^b (s^-1 × 10^-3)	Pd⁰ TOF ^b (s^-1 × 10^-3)
Fresh Pd-LSM-SG	3.0	2.3	12.1	1.3	1.3	—
Activated Pd-LSM-SG	12.6	2.3	11.9	5.3	1.3	10.6
Fresh Pd-LSM-IM	6.4	5.9	30.1	1.1	1.1	—
Activated Pd-LSM-IM	7.3	5.8	29.4	1.3	1.3	—

Fig. 9. De-NOx activity over the conventional and perovskite-based catalysts at 350 °C in the absence of H2O and CO2 (1) and in the presence of 5% H2O (2), 5% CO2 (3), and 5% H2O and 5% CO2 (4).

Fig. 10. De-NOx activity of the sol-gel-prepared La0.7Sr0.3MnO3-supported Pd (black lines) and wet-impregnation-prepared La0.7Sr0.3MnO3-supported Pd (red lines) in the absence (solid lines) and presence (dashed lines) of H2O and CO2 as function of the O2 concentration at 350 °C.

Fig. 11. De-NOx activities of the conventional Pd/BaO/Al2O3 (Pd/Ba/Al) and Pt/BaO/Al2O3 (Pt/Ba/Al) and perovskite-based catalysts at 350 °C in the absence of H2O, CO2 and SO2 (1), in the presence of 125 ppm SO2 (2), and 5% H2O, 5% CO2 and 125 ppm SO2 (3).

Fig. 12. Product selectivity of the fresh Pd-LSM-SG (a) and activated Pd-LSM-SG (b) catalysts at 350 °C: N2 (■), N2O (▼), NO (▲), NO2 (?), and C3H6 (●). Feeding gas: 1000 ppm C3H6, 5 vol% H2O, 5 vol% CO2 balanced with N2; space velocity: 120000 mL g-1 h-1.

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贫燃/富燃循环气氛下原位活化Pd负载钙钛矿催化剂促进NO_x还原消除

Promoting NO_x reduction via in situ activation of perovskite supported Pd catalysts under alternating lean-burn/fuel-rich operating atmospheres

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贫燃/富燃循环气氛下原位活化Pd负载钙钛矿催化剂促进NOx还原消除

Promoting NOx reduction via in situ activation of perovskite supported Pd catalysts under alternating lean-burn/fuel-rich operating atmospheres

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贫燃/富燃循环气氛下原位活化Pd负载钙钛矿催化剂促进NO_x还原消除

Promoting NO_x reduction via in situ activation of perovskite supported Pd catalysts under alternating lean-burn/fuel-rich operating atmospheres