Silicalite-1中CoOx物种在反应诱导下的重构机制以调控丙烷非氧化脱氢选择性

doi:10.1016/S1872-2067(25)64724-3

催化学报 ›› 2025, Vol. 74: 108-119.DOI: 10.1016/S1872-2067(25)64724-3

Silicalite-1中CoO_x物种在反应诱导下的重构机制以调控丙烷非氧化脱氢选择性

张启扬^a^,^*(), Vita A. Kondratenko^a, 丁湘浓^a, Jana Weiss^a, Stephan Bartling^a, Elizaveta Fedorova^a, 赵丹^a^,^b^,^c, Dmitry E. Doronkin^b, 王东旭^d, Christoph Kubis^a, Evgenii V. Kondratenko^a^,^*()

^a莱布尼茨催化研究所, 罗斯托克, 德国
^b卡尔斯鲁厄理工学院化学技术与高分子化学研究所, 催化研究与技术研究所, 卡尔斯鲁厄, 德国
^c中国科学院大连化学物理研究所, 甲醇制烯烃国家工程实验室, 清洁能源国家实验室, 能源材料化学协同创新中心(iChEM), 辽宁大连 116023, 中国
^d马克斯·普朗克微结构物理研究所, 哈勒, 德国

收稿日期:2025-01-28 接受日期:2025-03-08 出版日期:2025-07-18 发布日期:2025-07-20
通讯作者: *电子信箱: Qiyang.Zhang@catalysis.de (张启扬),Evgenii.kondratenko@catalysis.de (E. V. Kondratenko).

Understanding the reaction-induced restructuring of CoO_x species in silicalite-1 to control selectivity in non-oxidative dehydrogenation of propane

Qiyang Zhang^a^,^*(), Vita A. Kondratenko^a, Xiangnong Ding^a, Jana Weiss^a, Stephan Bartling^a, Elizaveta Fedorova^a, Dan Zhao^a^,^b^,^c, Dmitry E. Doronkin^b, Dongxu Wang^d, Christoph Kubis^a, Evgenii V. Kondratenko^a^,^*()

^aLeibniz-Institut für Katalyse e.V., D-18059 Rostock, Germany
^bInstitute for Chemical Technology and Polymer Chemistry, and Institute of Catalysis Research and Technology, Karlsruhe Institute of Technology, D-76131, Karlsruhe, Germany
^cNational Engineering Laboratory for Methanol to Olefins, Dalian National Laboratory for Clean Energy, iChEM (Collaborative Innovation Center of Chemistry for Energy Materials), Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^dMax Planck Institute of Microstructure Physics, 06120 Halle, Germany

Received:2025-01-28 Accepted:2025-03-08 Online:2025-07-18 Published:2025-07-20
Contact: *E-mail: Qiyang.Zhang@catalysis.de (Q. Zhang), Evgenii.kondratenko@catalysis.de (E. V. Kondratenko).

摘要/Abstract

摘要：

丙烷非氧化脱氢(PDH)是大规模定向生产丙烯的重要途径. 尽管钴基催化剂有望替代当前使用的铂基或氧化铬基催化剂, 但由于对目标反应和副反应中活性位点种类的不确定性, 其进一步发展受到限制. 因此, 本文系统研究了基于Silicalite-1分子筛负载的具有不同氧化还原特性的CoO_x物种中氧化态CoO_x和金属态Co⁰物种在PDH反应中的作用. 通过亚毫秒级和秒级时间分辨的丙烷脉冲实验(脉冲量分别约13和2200 nmol), 并结合深度的催化剂表征及不同丙烷转化率下的PDH测试, 揭示了反应诱导的CoO_x还原对产物选择性的影响机制. 研究结果表明, 丙烷可快速与CoO_x反应生成丙烯、碳氧化物和水; 生成的Co⁰物种在结焦和裂解反应中表现出高活性; 但当此类物种尺寸小于2 nm时, 由于碳物种对活性位点的覆盖显著抑制了这些副反应的发生; 未被覆盖的表面钴位点可选择性催化丙烷脱氢生成丙烯. 性能最优的催化剂展现出高于商用K-CrO_x/Al₂O₃催化剂的活性, 并在工业条件下的10次脱氢/再生循环中保持稳定运行. 在550 °C、平衡丙烷转化率52%和丙烯选择性95%的条件下, 生成丙烯的时空产率达到0.97 kg·h^-1·kg-cat^-1.

关键词: 丙烷, 脱氢, 丙烯, 钴, 反应机理

Abstract:

Non-oxidative dehydrogenation of propane (PDH) is an important route for large-scale on purpose propene production. Although cobalt-based catalysts are promising alternatives to currently used platinum- or chromium oxide-based catalysts, their further developments are hindered by the uncertainties related to the kind of the active sites involved in the desired and side reactions. To contribute to closing such a gap, we systematically investigate the role of oxidized CoO_x and metallic Co⁰ species in the PDH reaction over catalysts based in Silicalite-1 with supported CoO_x species differing in their redox properties. C₃H₈ pulse experiments with sub-millisecond and second resolution at pulse sizes of about 13 and 2200 nmol, respectively, combined with in-depth catalyst characterization and PDH tests at different propane conversions enabled us to understand how the reaction-induced reduction of CoO_x affects product selectivity. Propane readily reacts with CoO_x to yield propene, carbon oxides and water. The formed Co⁰ species show high activity to coking and cracking reactions. However, if the size of such species is below 2 nm, these undesired reactions are significantly hindered due to the coverage of the active sites by carbon-containing species. The remaining uncovered surface Co⁰ sites selectively dehydrogenate propane to propene. The best-performing catalyst showed higher activity than a commercial-like K-CrO_x/Al₂O₃ and operated durable in a series of 10 dehydrogenation/regeneration cycles under industrial relevant conditions. The space time yield of propene formation of 0.97 kg·h^-1·kg_cat^-1 was achieved at 550 °C, 52% equilibrium propane conversion and 95% propene selectivity.

Key words: Propane, Dehydrogenation, Propene, Cobalt, Mechanism

张启扬, Vita A. Kondratenko, 丁湘浓, Jana Weiss, Stephan Bartling, Elizaveta Fedorova, 赵丹, Dmitry E. Doronkin, 王东旭, Christoph Kubis, Evgenii V. Kondratenko. Silicalite-1中CoO_x物种在反应诱导下的重构机制以调控丙烷非氧化脱氢选择性[J]. 催化学报, 2025, 74: 108-119.

Qiyang Zhang, Vita A. Kondratenko, Xiangnong Ding, Jana Weiss, Stephan Bartling, Elizaveta Fedorova, Dan Zhao, Dmitry E. Doronkin, Dongxu Wang, Christoph Kubis, Evgenii V. Kondratenko. Understanding the reaction-induced restructuring of CoO_x species in silicalite-1 to control selectivity in non-oxidative dehydrogenation of propane[J]. Chinese Journal of Catalysis, 2025, 74: 108-119.

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https://www.cjcatal.com/CN/Y2025/V74/I7/108

图/表 10

Fig. 1. HAADF-STEM images of as-prepared 0.6Co/S-1 (a), 1Co/S-1 (b), 3Co/S-1 (c), and 5Co/S-1 (d).

Fig. 2. UV-vis spectra (a) and Co K-edge XANES (b) of the fresh catalysts and reference samples (Co3O4 and Co foil). The corresponding k2-weighted Fourier transform spectra are shown in (c).

Fig. 3. (a) H2-TPR profiles of xCo/S-1. (b) Quasi in situ XPS spectra of 1Co/S-1 after treatment at 550 °C with 20 vol% O2/Ar or 40 vol% H2/Ar. (c) In situ UV-vis spectra of 1Co/S-1 after treatment at 550 °C with 40 vol% H2/Ar.

Fig. 4. (a) The rate of propene formation over xCo/S-1. Temperature-resolved m/z values of 42 (C3H6) (b), 16 (CH4) (c) and 18 (H2O) (d) collected during temperature-programmed surface reaction of C3H8 with xCo/S-1 between 300 and 600 °C. (e) Arrhenius plots of the propene formation rate over xCo/S-1 as well as the respective apparent activation energy (Ea). (f) Ea versus the size of CoOx NP determined by HAADF-STEM (Fig. 1).

Fig. 5. The selectivity-conversion relationships for propene (a), C1-C2 hydrocarbons (b) and coke (c) formed over 0.6Co/S-1, 1Co/S-1 and 3Co/S-1. Proposed reaction pathways for propane dehydrogenation over 0.6Co/S-1 and 1Co/S-1 (d) as well as 3Co/S-1 (e). Reaction conditions: T = 550 °C, C3H8:N2 = 2:3, WHSV(C3H8) = 2.4-14.1 h-1.

Fig. 6. The normalized transient responses recorded upon pulsing a C3H8:Ar = 1:1 mixture at 550 °C over oxidized 1Co/S-1 (a) and 5Co/S-1 (d). C3H6 (b,e) and H2 (c,f) response recorded at 550 °C after pulsing (1mL) of a C3H8/Ar = 1:19 mixture over oxidized 1Co/S-1 (b,c) and 5Co/S-1 (e,f). Before the C3H8 pulses, the catalysts were exposed to a flow of O2/Ar = 1:4 (10 mL·min-1) at 550 °C for 30 min and then flushed with Ar for 20 min.

Fig. 7. The normalized transient responses recorded upon pulsing of a C3H8:Ar = 1:1 mixture at 550 °C over reduced 1Co/S-1 (a) and 5Co/S-1 (d). C3H6 (b,e) and H2 (c,f) response recorded at 550 °C after pulsing (1mL) of an C3H8/Ar = 1:19 mixture over reduced 1Co/S-1 (b,c) and 5Co/S-1 (e,f). Before the C3H8 pulses, the catalysts were exposed to a flow of H2/Ar=1:4 (10 mL/min) at 550°C for 30 min and then flushed with Ar for 20 min.

Fig. 8. (a) Operando UV-vis spectra of 1Co/S-1 during the C3H8 pulses (1mL pulse size) at 550 °C using a feed with 5 vol% C3H8 in Ar. (b) Operando Raman spectra of 1Co/S-1 collected during exposure to a feed with 40 vol% C3H8 in N2 at 550 °C.

Fig. 9. (a) Time-on-stream profiles of propane conversion and propene selectivity over tested samples. (b) Space time yield of propene formation (STY(C3H6)) determined over 1Co/S-1 and previously reported Co-based catalysts (Table S4) versus X(C3H8)exp/X(C3H8)eq. Reaction conditions: T = 550 °C, catalyst amount = 100 mg, WHSV(C3H8) = 4.7 h-1, C3H8:N2 = 2:3.

Fig. 10. Propane conversion and propene selectivity over 1Co/S-1 in 10 PDH/ regeneration cycles. Reaction conditions: T = 550 °C, catalyst amount = 100 mg, WHSV(C3H8) = 4.7 h-1, C3H8:N2 = 2:3. Each cycle consisted of a PDH stage lasted for 120 min and a regeneration stage lasted for 30 min.

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Silicalite-1中CoO_x物种在反应诱导下的重构机制以调控丙烷非氧化脱氢选择性

Understanding the reaction-induced restructuring of CoO_x species in silicalite-1 to control selectivity in non-oxidative dehydrogenation of propane

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Silicalite-1中CoOx物种在反应诱导下的重构机制以调控丙烷非氧化脱氢选择性

Understanding the reaction-induced restructuring of CoOx species in silicalite-1 to control selectivity in non-oxidative dehydrogenation of propane

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Silicalite-1中CoO_x物种在反应诱导下的重构机制以调控丙烷非氧化脱氢选择性

Understanding the reaction-induced restructuring of CoO_x species in silicalite-1 to control selectivity in non-oxidative dehydrogenation of propane