Sn1Pt单原子合金催化剂在丙烷脱氢反应中的应用

doi:10.1016/S1872-2067(23)64402-X

催化学报 ›› 2023, Vol. 48: 164-174.DOI: 10.1016/S1872-2067(23)64402-X

Sn₁Pt单原子合金催化剂在丙烷脱氢反应中的应用

邢亚楠^a^,^b^,¹, 康磊磊^a^,¹, 马静远^d, 蒋齐可^a, 苏杨^a, 张盛鑫^a^,^b, 徐晓燕^a, 李林^a, 王爱琴^a, 刘智攀^c^,^e, 马思聪^c^,^*(), 刘晓艳^a^,^*(), 张涛^a^,^b

^a中国科学院大连化学物理研究所, 中国科学院应用催化科学技术重点实验室, 辽宁大连116023
^b中国科学院大学, 北京100049
^c中国科学院上海有机化学研究所, 有机功能分子合成与自组装化学重点实验室, 上海200032
^d中国科学院上海高等研究院, 上海同步辐射光源, 上海201204
^e复旦大学化学系, 计算物理科学重点实验室, 分子催化与创新材料上海重点实验室, 上海200433

收稿日期:2022-11-27 接受日期:2023-02-03 出版日期:2023-05-18 发布日期:2023-03-15
通讯作者: * 电子信箱: scma@mail.sioc.ac.cn (马思聪), xyliu2003@dicp.ac.cn (刘晓艳).
作者简介:第一联系人：
¹共同第一作者
基金资助:
国家自然科学基金(22102180);中国科学院洁净能源创新研究院合作基金(DNL202002);辽宁省“兴辽英才计划”项目(XLYC2007070);中央高校基本科研业务费专项资金(20720220009)

Sn₁Pt single-atom alloy evolved stable PtSn/nano-Al₂O₃ catalyst for propane dehydrogenation

Yanan Xing^a^,^b^,¹, Leilei Kang^a^,¹, Jingyuan Ma^d, Qike Jiang^a, Yang Su^a, Shengxin Zhang^a^,^b, Xiaoyan Xu^a, Lin Li^a, Aiqin Wang^a, Zhi-Pan Liu^c^,^e, Sicong Ma^c^,^*(), Xiao Yan Liu^a^,^*(), Tao Zhang^a^,^b

^aCAS Key Laboratory of Science and Technology on Applied Catalysis, iChEM, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bUniversity of Chinese Academy of Sciences, Beijing 100049, China
^cKey Laboratory of Synthetic and Self-Assembly Chemistry for Organic Functional Molecules, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai 200032, China
^dShanghai Synchrotron Radiation Facility, Shanghai Advanced Research Institute, Chinese Academy of Sciences, Shanghai 201204, China
^eShanghai Key Laboratory of Molecular Catalysis and Innovative Materials, Key Laboratory of Computational Physical Science, Department of Chemistry, Fudan University, Shanghai 200433, China

Received:2022-11-27 Accepted:2023-02-03 Online:2023-05-18 Published:2023-03-15
Contact: * E-mail: scma@mail.sioc.ac.cn (S. Ma), xyliu2003@dicp.ac.cn (X. Y. Liu).
About author:First author contact:
¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22102180);DNL Cooperation Fund, CAS(DNL202002);Key Research Program of Frontier Sciences, CAS(ZDBS-LY-7012);LiaoNing Revitalization Talents Program(XLYC2007070);Fundamental Research Funds for the Central Universities(20720220009)

摘要/Abstract

摘要：

丙烯是生产聚丙烯、各类丙烷氧化物、丙烯腈的重要化工原料. 近年来, 随着丙烯需求量日益增长, 作为一种专产丙烯的生产方式, 丙烷脱氢(PDH)受到了越来越多的关注. PtSn/Al₂O₃是一种典型的工业丙烷脱氢催化剂, 其特征是催化活性会随反应时间的推移而下降, 因此需要反复再生以保证丙烯产率. 提高PtSn催化剂的稳定性, 需要明确反应状态下PtSn的催化性能与其结构之间的关系. 然而, Pt和Sn的价态及其相互作用, 对制备方法、预还原条件、载体类型等因素非常敏感, 此外, 从Pt-Sn二元相图来看, 二者在高温(~600 °C)还原性反应气氛下可形成多种合金结构, 因此, PtSn在丙烷脱氢中的活性位结构的认识颇具挑战, 目前文献报道结果仍存在争议.
本文选用商业化的纳米级γ-Al₂O₃作为载体, 通过利用纳米载体上只能担载有限数量的金属原子和加入过量的第二金属Sn稀释活性金属Pt的方式, 得到高分散的PtSn/nano-Al₂O₃催化剂. 当Pt和Sn的负载量分别为0.1 wt%和1 wt%时, 其初始丙烯产率可达到47.6 mol_C3H6 g_Pt^-1 h^-1, 高于文献已报道的PtSn双金属催化剂, 该催化剂经3-10 h活性快速下降期(k_d-3h: 0.11 h^-1)后, 表现出较好的稳定性(k_d-10~40h: 0.0026 h^-1). 球差电镜(AC-HAADF-STEM)表征结果显示, 该催化剂经500 °C焙烧后, Pt及Sn在Al₂O₃载体上均呈单原子分散状态; 经600 °C氢气还原后, Pt团聚为平均直径约0.85 nm的纳米颗粒; 通过对其进行能谱点扫分析, 发现Pt纳米颗粒上分布有少量的Sn原子, 而剩余大量的Sn原子则继续以单原子形式分布在载体上. 进一步原位X射线光电子能谱和原位X射线吸收能谱结果证明, 该催化剂中纳米颗粒的具体组成为Sn单原子分散在Pt纳米颗粒表面, 形成Sn₁Pt表面单原子合金结构. 密度泛函理论理论计算证明了Sn₁Pt表面单原子合金结构的稳定性及其在丙烷脱氢中的高活性. 最后结合原位CO吸附的漫反射红外光谱等表征, 揭示了催化剂反应初期活性下降及后期高稳定性的内在原因: 催化剂经还原后形成了高活性的Sn₁Pt表面单原子合金结构, 在反应过程中, 该结构演变为纯相Pt₃Sn金属间化合物, 其与周围呈单分散的SnO_x物种协同作用, 抑制和转移在活性中心上的积碳, 进而实现了高稳定性. 这种通过单原子表面合金演变得到的Pt₃Sn金属间化合物, 与传统Pt与Pt₃Sn等金属化合物混相共存的工业催化剂相比, 可以避免丙烯在催化剂表面单金属Pt平台位点上的深度脱氢和积碳, 进而提高了催化剂稳定性. 综上, 本文从原子水平上为PDH反应中PtSn/Al₂O₃催化剂的活性位结构及其演化过程提供了新的见解, 并为工业催化剂的设计制备提供了理论参考.

关键词: 丙烷脱氢, 丙烯, Pt-Sn催化剂, 结构重构, 单原子合金

Abstract:

The PtSn/Al₂O₃ is a prototypical industrial catalyst for propane dehydrogenation (PDH). However, the local structures of the active sites are still inconclusive under the operation conditions. Herein, the evolutions of the Pt-Sn active centers supported on nano-Al₂O₃ are definitely discerned at the atomic level during PDH reaction. By combining complementary in situ characterizations and theoretical calculations, we demonstrate that a highly productive Sn₁Pt single-atom alloy (47.6 mol_C3H6 g_Pt^-1 h^-1) forms after the reduction, and thereby self-assembles to the Pt₃Sn intermetallic compound during the reaction, which exhibits a rather stable performance (k_d-10~40h: 0.0026 h^-1). Intriguingly, the results of in situ diffuse reflectance infrared Fourier-transform spectroscopy further corroborate that the adjacent Pt atoms with terrace sites aggravating the coke deposition can be circumvented through this single-atom alloy mediated reconstruction. Our findings depict an unprecedented evolution process of the active sites of the PtSn/Al₂O₃, and afford an effectual nanostructure engineering pathway for stable PDH catalysts.

Key words: Propane dehydrogenation, Propylene, Pt-Sn catalyst, Reconstruction, Single-atom alloy

邢亚楠, 康磊磊, 马静远, 蒋齐可, 苏杨, 张盛鑫, 徐晓燕, 李林, 王爱琴, 刘智攀, 马思聪, 刘晓艳, 张涛. Sn₁Pt单原子合金催化剂在丙烷脱氢反应中的应用[J]. 催化学报, 2023, 48: 164-174.

Yanan Xing, Leilei Kang, Jingyuan Ma, Qike Jiang, Yang Su, Shengxin Zhang, Xiaoyan Xu, Lin Li, Aiqin Wang, Zhi-Pan Liu, Sicong Ma, Xiao Yan Liu, Tao Zhang. Sn₁Pt single-atom alloy evolved stable PtSn/nano-Al₂O₃ catalyst for propane dehydrogenation[J]. Chinese Journal of Catalysis, 2023, 48: 164-174.

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图/表 6

Fig. 1. (a) Propane conversion (solid) and propylene selectivity (hollow) with time on stream for the 0.1Pt/nano-Al2O3 (green triangle), 0.1Pt1Sn/nano-Al2O3 (blue circle) and 0.5Pt1Sn/nano-Al2O3 (red square) catalysts. (b) The productivities and deactivation rate constants (kd) of the 0.1Pt1Sn/nano-Al2O3 and 0.5Pt1Sn/nano-Al2O3 at different stages in Fig. 1(a). (c) Initial productivity for representative PtSn-based PDH catalysts studied in the literatures. Numbers in brackets are corresponding to the row numbers in Table S2.

Fig. 2. AC-HAADF-STEM images of the 0.1Pt1Sn/nano-Al2O3 after the calcination (a), reduction (b) and PDH reaction (c). The insets are the corresponding size distribution of the metal nanoparticles. The EDS mappings of the 0.1Pt1Sn/nano-Al2O3 after the reduction (d-f) and PDH reaction (g-i) for 12 h.

Fig. 3. In situ XPS spectra of Sn 3d5/2 of the 0.1Pt1Sn/nano-Al2O3 (a) and the 0.5Pt1Sn/nano-Al2O3 (b) under 20 vol% H2/Ar at 600 °C for 2 h reduction. Normalized in situ XANES spectra at the Pt L3-edge (c) and Sn K-edge (e), as well as the corresponding k2-weighted Fourier transform spectra at the Pt L3-edge (d) and Sn K-edge (f) (without phase correction) of the 0.1Pt1Sn/nano-Al2O3 during PDH reaction. The Pt foil, Sn foil, SnO and SnO2 were provided as references.

Table 1 Fitting results of the EXAFS data of the 0.1Pt1Sn/nano-Al2O3 catalyst and the references.

Sample	Shell	N	R (Å)	σ² (×10^-2 Å²)	ΔE₀ (eV)	R-factor (%)
Pt foil	Pt-Pt	12.0	2.76	0.4	6.8	0.3
Sn foil	Sn-Sn	8.0	3.01	1.2	2.2	0.1
0.1Pt1Sn-reduction	Pt-O	0.4	1.94	0.3	1.0	3.1
	Pt-Pt	3.9	2.75	0.6	1.0	—
	Pt-Sn	1.4	2.66	0.7	1.0	—
	Sn-O	1.4	2.12	1.4	2.1	3.6
	Sn-Pt	1.4	2.66	0.8	-19.5	—
0.1Pt1Sn-reaction 3 h	Pt-O	0.7	2.12	0.3	15.4	0.1
	Pt-Pt	4.0	2.75	1.3	7.7	—
	Pt-Sn	1.7	2.81	1.3	7.7	—
0.1Pt1Sn-reaction17.5 h	Pt-O	0.6	2.06	0.3	9.5	0.6
	Pt-Pt	4.6	2.76	1.1	5.6	—
	Pt-Sn	1.6	2.80	1.2	5.6	—

Fig. 4. The DFT results of PDH reaction on PtSn/Al2O3. (a) The energy variation trajectory during SSW-DFT simulation for Pt6Sn3 cluster global optimization on Al2O3 (110) surface. Gibbs free energy profiles (b) and the corresponding structures (c) of the transition states during the PDH process. (d) The variation of reaction rate during microkinetics simulation for PDH reaction on Sn1Pt SAA and Pt3Sn (111) surface at 873 K and 1 bar 14 vol% C3H8 and 14 vol% H2 pressure. The asterisk indicates the adsorption state. The reaction snapshots are shown with the Pt, Sn, Al, O, C and H in cyan, light gray, pink, red, grey and white colours, respectively.

Fig. 5. In situ CO-DRIFTS of the 0.1Pt1Sn/nano-Al2O3 (a), and 0.5Pt1Sn/nano-Al2O3 (b). As a comparison, the corresponding monometallic counterparts were used as references. (c) Schematic illustration of the evolution of PtSn/nano-Al2O3 catalysts during PDH reaction.

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Sn₁Pt单原子合金催化剂在丙烷脱氢反应中的应用

Sn₁Pt single-atom alloy evolved stable PtSn/nano-Al₂O₃ catalyst for propane dehydrogenation

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[1]	孙嘉辰, 陈赛, 付东龙, 王伟, 王显辉, 孙国栋, 裴春雷, 赵志坚, 巩金龙. 氧扩散与表面反应在VO_x-Ce_1‒_xZr_xO₂催化丙烷脱氢反应中的影响[J]. 催化学报, 2023, 52(9): 217-227.
[2]	张龙康, 马跃, 刘昌呈, 万志鹏, 翟承伟, 王新, 徐浩, 关业军, 吴鹏. 脱金属-还原策略诱导创制高分散PtZn合金催化剂用于丙烷脱氢反应[J]. 催化学报, 2023, 55(12): 241-252.
[3]	王冶, 韩晶峰, 王男, 李冰, 杨淼, 吴一墨, 江子潇, 魏迎旭, 田鹏, 刘中民. SAPO-14催化的甲醇制丙烯反应: 反应机理与失活[J]. 催化学报, 2022, 43(8): 2259-2269.
[4]	尹金鹏, 金鑫, 徐浩, 关业军, 彭如斯, 陈丽, 蒋金刚, 吴鹏. 富硅壳层结构的无粘结剂MWW钛硅分子筛用作高选择性、高稳定性的丙烯环氧化[J]. 催化学报, 2021, 42(9): 1561-1575.
[5]	任栎, 王博文, 陆琨, 彭如斯, 关业军, 蒋金刚, 徐浩, 吴鹏. 脱铝丝光分子筛应用于MTP反应: Al的落位和晶体形貌的影响[J]. 催化学报, 2021, 42(7): 1147-1159.
[6]	郭玲玲, 虞静, 王伟伟, 刘家旭, 郭洪臣, 马超, 贾春江, 陈俊翔, 司锐. 负载于二氧化硅上的小尺寸氧化亚铜物种促进丙烯选择性氧化生成丙烯醛[J]. 催化学报, 2021, 42(2): 320-333.
[7]	郑仁垟, 谢在库. 多相催化时空演变的全生命周期表征策略[J]. 催化学报, 2021, 42(12): 2141-2148.
[8]	刘怡, 张光辉, 王建洋, 朱杰, 张新宝, Jeffrey T. Miller, 宋春山, 郭新闻. CO₂消除镓氢物种提升Ga₂O₃/SiO₂丙烷脱氢反应性能[J]. 催化学报, 2021, 42(12): 2225-2233.
[9]	纪中海, 苗登云, 高丽君, 潘秀莲, 包信和. B修饰的ZrO₂及其制备pH值对PtSn/B-ZrO₂丙烷脱氢反应性能的影响[J]. 催化学报, 2020, 41(4): 719-729.
[10]	陈冲, 孙明磊, 胡忠攀, 刘玉萍, 张守民, 袁忠勇. SiBeta负载的VO_x催化剂在丙烷直接脱氢制丙烯中的活性位[J]. 催化学报, 2020, 41(2): 276-285.
[11]	孙林林, 周亚举, 李鑫, 李金择, 沈东, 尹世康, 王会琴, 霍鹏伟, 闫永胜. 热响应型PNIPAM@Ag/Ag₃PO₄/CN复合光催化剂的制备及性能[J]. 催化学报, 2020, 41(10): 1573-1588.
[12]	胡忠攀, 任金涛, 杨丹丹, 王政, 袁忠勇. 介孔碳作为非金属丙烷脱氢催化剂:孔道结构和表面性质的影响[J]. 催化学报, 2019, 40(9): 1385-1394.
[13]	胡忠攀, 杨丹丹, 王政, 袁忠勇. 丙烷直接脱氢催化剂的研究进展[J]. 催化学报, 2019, 40(9): 1233-1254.
[14]	郭美玲, 刘雪斌, Amorelli Angelo. 镨掺杂氧化铈材料在小分子活化中的应用[J]. 催化学报, 2019, 40(11): 1800-1809.
[15]	黄昶, 王志强, 龚学庆. VO₃/CeO₂(111)催化剂上丙烷氧化脱氢反应活性和选择性的密度泛函理论研究[J]. 催化学报, 2018, 39(9): 1520-1526.