不互溶Ag提高Co/YSZ高压甲烷干重整催化剂稳定性研究

doi:10.1016/S1872-2067(25)64677-8

催化学报 ›› 2025, Vol. 74: 82-96.DOI: 10.1016/S1872-2067(25)64677-8

不互溶Ag提高Co/YSZ高压甲烷干重整催化剂稳定性研究

李士宁^a^,¹, 姚俊韬^a^,¹, 庞淑馨^a^,¹, 张景彭^a, 李诗颖^b, 刘志成^c, 韩璐^d, 樊卫斌^b^,^*(), 朱卡克^a^,^*(), 朱贻安^a^,^*()

^a华东理工大学化工学院, 上海 200237
^b中国科学院山西煤炭化学研究所, 国家煤炭转化重点实验室, 山西太原 030001
^c中石化上海石油化工研究院, 上海 201208
^d同济大学化学科学与工程学院, 上海 200092

收稿日期:2025-01-14 接受日期:2025-03-03 出版日期:2025-07-18 发布日期:2025-07-20
通讯作者: *电子信箱: fanwb@sxicc.ac.cn (樊卫斌),kakezhu@ecust.edu.cn (朱卡克),yanzhu@ecust.edu.cn (朱贻安).
作者简介:¹共同第一作者.
基金资助:
国家重点研发计划(2024YFA1509901);国家自然科学基金(22178111);中国石化与上海石油化工研究院有限公司的联合研究项目(222215)

Co particles separated by immiscible Ag on yttria-stabilized zirconia as durable methane dry reforming catalyst under pressurized conditions

Shi-Ning Li^a^,¹, Juntao Yao^a^,¹, Shuxin Pang^a^,¹, Jing-Peng Zhang^a, Shiying Li^b, Zhicheng Liu^c, Lu Han^d, Weibin Fan^b^,^*(), Kake Zhu^a^,^*(), Yi-An Zhu^a^,^*()

^aUNILAB, State Key Laboratory of Green Chemical Engineering and Industrial Catalysis, School of Chemical Engineering, East China University of Science and Technology, Shanghai 200237, China
^bState Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Science, Taiyuan 030001, Shanxi, China
^cShanghai Research Institute of Petrochemical Technology, Shanghai 201208, China
^dSchool of Chemical Science & Engineering, Tongji University, Shanghai 200092, China

Received:2025-01-14 Accepted:2025-03-03 Online:2025-07-18 Published:2025-07-20
Contact: *E-mail: fanwb@sxicc.ac.cn (W. Fan), kakezhu@ecust.edu.cn (K. Zhu), yanzhu@ecust.edu.cn (Y.-A. Zhu).
About author:¹Contributed equally to this work.
Supported by:
National Key Research and Development Program of China(2024YFA1509901);National Natural Science Foundation of China(22178111);SINOPEC joint research project with Shanghai Research Institute of Petrochemical Technology(222215)

摘要/Abstract

摘要：

甲烷-二氧化碳重整, 也称甲烷干重整, 可将两种温室气体转化为具有广泛用途的合成气, 是二氧化碳利用的一条重要途径. 该反应在接近工业高压条件下更具经济性, 但该苛刻操作条件对抗积碳催化剂设计提出了挑战.

本文以氧化钇稳定氧化锆(YSZ)为载体, 分别制备了接触不互溶型的Ag₁-Co₁/YSZ、表面合金型的Ag_0.03-Co₁/YSZ和不加助剂Ag的Co/YSZ催化剂样品, 对其在1123 K, 1-20 bar, 化学计量比进料苛刻条件下的稳定性进行了对比评价, 其中Ag₁-Co₁/YSZ最为稳定. X射线衍射(XRD)、透射电镜(TEM)和准原位X-射线光电子能谱分析表明, Ag₁-Co₁/YSZ主要由不互溶、彼此接触的Ag和Co颗粒构成, 与反应气氛接触后, 主要以金属态存在. 对反应后样品分析, 发现Ag₁-Co₁/YSZ上未生成XRD可观测石墨型积碳, 也未发现TEM可视胡须状积碳, 这也被Raman表征所证实. 对积碳在连续CO₂和空气气氛下的热重分析表明, Ag₁-Co₁/YSZ催化剂上仅生成可被CO₂氧化的碳物种, 且积碳总量大幅下降. Ag对Co表面的钝化作用也被程序升温表面反应证实, 起活温度在加入Ag后显著上升, 并且Ag₁-Co₁/YSZ温度最高. 紫外光电子谱对表面功函数的测量发现, Co/YSZ为3.63 eV, 而Ag₁-Co₁/YSZ则为4.38 eV, 高于银钴合金的4.13 eV. 动力学实验发现各个催化剂上均有同一个动力学方程, 即仅对甲烷呈现一级反应, 而与其他反应物或产物为零级反应; 不同之处仅在于活化能从单独Co的124 kJ mol^-1升高到Ag₁-Co₁/YSZ的175 kJ mol^-1. 基于密度泛函理论(DFT)计算和微观动力学分析, 发现在单独Co表面, CH₄依次解离为表面CH*或C*原子, CH*和表面O*的耦联是主要消碳路径; 而在加入Ag后, C*与O*的耦联成为Ag-Co表面的主要消碳反应, 且表面最丰物种(MARI)为表面O*, 该MARI不易受到温度和压力的影响, 说明其表面C*浓度较低. 对表面C*的成核、生长过程进行了模拟计算, 发现在表面C*经由碳岛生成石墨型碳的过程中, Ag团簇的修饰作用可将碳岛的临界尺寸由Co(111)上21个碳原子提高到Ag-Co(111)表面的648个碳原子. DFT所构建的动力学方程和实验结果一致, 所预测的活化能变化趋势也与实验结果定性相符. Ag颗粒的助剂作用可总结为: (1) 通过表面钝化作用, 减缓了高压下的积碳沉积速率, 在动力学上部分对冲了温度、压力上升对积碳过程影响, 有利于积碳-消碳实现动态平衡; (2) Ag颗粒的存在下, 表面MARI为O*, 而非C*; 且降低了表面C*在成核过程中形成碳岛的稳定性, 抑制了表面吸附C*通过成核和生长转化为石墨型碳.

当两种不互溶金属发生界面接触时, 其对金属颗粒的电子结构和催化性能的影响比常见的金属-载体作用更为显著. 这种不互溶金属间的接触会引发体系功函数变化, 为优化金属催化性能提供了具有一定普适性的调控策略.

关键词: 甲烷干重整, 二氧化碳, 多相催化, Co, Ag

Abstract:

It is economical to perform methane and carbon dioxide reforming (DRM) under industrially relevant high-pressure conditions, but the harsh operation condition poses a grand challenge for coke-resistant catalyst design. Here, we propose to boost the coke- tolerance of Co catalyst by applying a contact potential introduced by immiscible Ag clusters. We demonstrate that Co clusters separated by neighboring Ag on Yttria-stabilized zirconia (YSZ) support can serve as a coke- and sintering-resistant DRM catalyst under diluent gas-free, stoichiometric CH₄ and CO₂ feeding, 1123 K and 20 bar. Since immiscible metals are ubiquitous and metal contact influences surface work function in general, this new design concept may have general implications for tailoring catalytic properties of metals.

Key words: Methane dry reforming, Carbon dioxide, Heterogeneous catalysis, Co, Ag

李士宁, 姚俊韬, 庞淑馨, 张景彭, 李诗颖, 刘志成, 韩璐, 樊卫斌, 朱卡克, 朱贻安. 不互溶Ag提高Co/YSZ高压甲烷干重整催化剂稳定性研究[J]. 催化学报, 2025, 74: 82-96.

Shi-Ning Li, Juntao Yao, Shuxin Pang, Jing-Peng Zhang, Shiying Li, Zhicheng Liu, Lu Han, Weibin Fan, Kake Zhu, Yi-An Zhu. Co particles separated by immiscible Ag on yttria-stabilized zirconia as durable methane dry reforming catalyst under pressurized conditions[J]. Chinese Journal of Catalysis, 2025, 74: 82-96.

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https://www.cjcatal.com/CN/Y2025/V74/I7/82

图/表 13

Scheme 1. Simplified DRM mechanism and formation mechanism of various carbon species on catalyst surfaces.

Fig. 1. XRD patterns for fresh Co/YSZ, Ag0.03-Co1/YSZ, Ag1-Co1/YSZ catalysts and Ag/YSZ (a) and TEM image (b) and elemental mappings (c-f) for Ag1-Co1/YSZ. A structure model of Ag1-Co1/YSZ is presented in (g).

Table 1 Physicochemical properties of Ag-Co/YSZ catalysts.

Catalyst	Metal Loading				S_BET m² g^-1	H₂-chemisorption (q) Mmol g^-1	Work function eV
Catalyst	Ag wt%	Co wt%	Ag mol%	Co mol%	S_BET m² g^-1	H₂-chemisorption (q) Mmol g^-1	Work function eV
YSZ					41
Ag₉-Co₁/YSZ	18.1	1.2	16.7	2.0	27	3.01
Ag₃-Co₁/YSZ	14.4	2.8	13.0	4.8	28	6.30
Ag_1.5-Co₁/YSZ	12.2	4.5	11.1	7.6	22	8.38
Ag₁-Co₁/YSZ	10.0	6.2	9.2	10.5	23	9.26	4.38^a (4.90^b)
Ag_0.25-Co₁/YSZ	3.1	7.5	4.2	18.7	26
Ag_0.03-Co₁/YSZ	0.4	9.3	0.6	23.1	27		4.13
Co/YSZ	0	14	0	23.7	20	5.36	3.63 (4.62)

Fig. 2. Semi in situ XPS spectra of Co 2p (a), Ag 3d (b), O 1s (c), and C 1s (d) for representative Co/YSZ and Ag1-Co1/YSZ after exposing to H2 at 1073 K for 3 min and mixture gas feed of CH4, CO2 at 1073 K for 10 min. (e) A structure cartoon for the surface structure is diagrammatically illustrated in (d).

Table 2 Surface composition(mol%) of fresh Ag-Co/YSZ catalysts determined by semi in situ XPS at H2 atmosphere.

Catalyst	Ag⁰	Co⁰	Co²⁺	C
Catalyst	Ag⁰	Co⁰	Co²⁺	C-C	C-O	C=O
Co/YSZ	—	0.070	0.068	0.039	0.050	0.013
Ag_0.03-Co₁/YSZ	0.05	0.06	0.077	0.038	0.041	0.014
Ag₁-Co₁/YSZ	0.071	0.090	0.072	0.034	0.032	0.018

Fig. 3. Catalytic stability for Ag1-Co1/YSZ, Ag0.03-Co1/YSZ and Co/YSZ catalysts, displayed for CH4 conversion (a), CO2 conversion (b) and the corresponding H2/CO ratio variations (c) as a function of TOS at 1123 K and pressures from 1.0 to 20.0 bar with a space velocity of 3636 mL h-1 g-cat-1. The dashed line in (a) indicates the equilibrium conversion of CH4.

Fig. 4. (a) XRD patterns of spent Ag-Co/YSZ. TEM micrographs (b-f) and nanoparticle dispersion (g) of Co for spent Ag1-Co1/YSZ.

Fig. 5. CO2-TGA (a), air-TGA (b), quantity of coke detected on typical samples (c) and Raman pattern (d) for typical spent Co/YSZ, Ag0.03-Co1/YSZ and Ag1-Co1/YSZ catalysts.

Fig. 6. TPSR plots of Co/YSZ, Ag0.03-Co1/YSZ and Ag1-Co1/YSZ, conducted under ambient pressure, CH4= CO2 = 15 mL min-1, T = 323-1173 K.

Fig. 7. (a) Activation energy and TOF value of Co/YSZ, Ag0.03-Co1/YSZ and Ag1-Co1/YSZ. (b-e) relationship among CH4 turnover rate and gas partial pressure (CH4, CO2, H2, CO). (f) TOF value and Ea for Co/YSZ, Ag0.03-Co1/YSZ and Ag1-Co1/YSZ

Fig. 8. Potential energy profiles along the reaction coordinate for DRM on representative fcc- Co(111) and Ag-Co(111) surfaces.

Fig. 9. (a) Gibbs free energy diagrams for DRM over Co (111) through CH+O path, Ag-Co(111) through C+O path at 1123 K. Flux analysis of DRM under experimental reactor inlet conditions (1123 K, 20 bar of total pressure, with a gas composition of 50% CH4, 50% CO2, 0% CO, 0% H2, and 0% H2O) over Ag-Co(111) (b), Co(111) (c). The arrows, which are labeled with the percentage of the total reaction flux, show the direction the reversible elementary steps actually proceed. The percentage of the reaction flux was calculated as the absolute value of the net rate for that elementary step divided by the rate for methane consumption.

Fig. 10. (a) The model of graphene island is semi-hexagonal and attached to a step edge. The total energy (E) of a graphene island, the edge and bulk energies on Co (b), and Ag-Co (c) as a function of number of C atoms Ntot. The dotted lines are bulk energy, the dashed lines are the edge energy, and the full lines are the total energy of the island. The red line indicates the critical island size.

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不互溶Ag提高Co/YSZ高压甲烷干重整催化剂稳定性研究

Co particles separated by immiscible Ag on yttria-stabilized zirconia as durable methane dry reforming catalyst under pressurized conditions

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