MFI介孔分子筛限域封装Co纳米颗粒选择性催化合成气转化为重质液态烃燃料

doi:10.1016/S1872-2067(24)60166-X

催化学报 ›› 2025, Vol. 68: 246-258.DOI: 10.1016/S1872-2067(24)60166-X

MFI介孔分子筛限域封装Co纳米颗粒选择性催化合成气转化为重质液态烃燃料

龚能^a^,¹, 邓权政^a^,¹, 王雨娇^b, 王自陶^c, 韩璐^a^,^*(), 吴鹏^d^,^*(), 车顺爱^e^,^*()

^a同济大学化学科学与工程学院, 上海 200092
^b重庆大学化学化工学院, 前沿交叉学科研究院, 跨尺度多孔材料研究中心, 重庆 400044
^c吉林大学无机合成与制备化学国家重点实验室, 吉林长春 130015
^d华东师范大学化学与分子工程学院, 上海市绿色化学与化工过程绿色化重点实验室, 石油化工分子转化与反应工程全国重点实验室, 上海 200062
^e上海交通大学化学化工学院, 变革性分子前沿科学中心, 金属基复合材料国家重点实验室, 上海市手性药物分子工程重点实验室, 上海 200240

收稿日期:2024-07-03 接受日期:2024-09-27 出版日期:2025-01-18 发布日期:2025-01-02
通讯作者: * 电子信箱: chesa@sjtu.edu.cn (车顺爱), pwu@chem.ecnu.edu.cn (吴鹏), luhan@tongji.edu.cn (韩璐).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(21931008);国家重点研发计划(2021YFA1200301);国家重点研发计划(2021YFA1501401)

Co nanoparticles confined in mesopores of MFI zeolite for selective syngas conversion to heavy liquid hydrocarbon fuels

Neng Gong^a^,¹, Quanzheng Deng^a^,¹, Yujiao Wang^b, Zitao Wang^c, Lu Han^a^,^*(), Peng Wu^d^,^*(), Shun’ai Che^e^,^*()

^aSchool of Chemical Science and Engineering, Tongji University, Shanghai 200092, China
^bMulti-scale Porous Materials Center, Institute of Advanced Interdisciplinary Studies & School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400044, China
^cState Key Laboratory of Inorganic Synthesis & Preparative Chemistry, Jilin University, Changchun 130015, Jilin, China
^dShanghai Key Laboratory of Green Chemistry and Chemical Processes, State Key Laboratory of Petroleum Molecular & Process Engineering, School of Chemistry and Molecular Engineering, East China Normal University, Shanghai 200062, China
^eSchool of Chemistry and Chemical Engineering, Frontiers Science Center for Transformative Molecules, State Key Laboratory of Metal Matrix Composites, Shanghai Key Laboratory for Molecular Engineering of Chiral Drugs, Shanghai Jiao Tong University, Shanghai 200240, China

Received:2024-07-03 Accepted:2024-09-27 Online:2025-01-18 Published:2025-01-02
Contact: * E-mail: chesa@sjtu.edu.cn (S. Che), pwu@chem.ecnu.edu.cn (P. Wu), luhan@tongji.edu.cn (L. Han).
About author:
¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(21931008);National Key R&D Program of China(2021YFA1200301);National Key R&D Program of China(2021YFA1501401)

摘要/Abstract

摘要：

费托合成(FTS)能有效地将非石油基碳资源衍生的合成气(CO/H₂)转化为清洁液态烃燃料. 目前FTS主要的活性金属组分是Fe, Ru和Co, 其中, Co基催化剂具有适宜的长链烃生长能力和价格低廉等优点. 采用介孔ZSM-5或者Y分子筛作为Co金属纳米颗粒(NPs)的载体, 利用分子筛固有的酸性位点, 增强传质能力和择形选择性, 将固体蜡C₂₁₊裂解为中间馏分液体燃料. 由于重质的液态烃过度裂解和氢解, 这些催化剂合成的液态产物通常是汽油烃(C₅-C₁₁). 本文通过调控Co NPs在介孔MFI分子筛中的位置分布, 抑制重质烃产物的C-C键过度裂解和氢解, 以实现煤油(C₈-C₁₆)和柴油(C₁₀-C₂₀)的高选择性生成.
本文采用浸渍法将Co NPs选择性地封装到有序介孔MFI分子筛(OMMZ)的微孔和介孔孔道中, 通过调控不同尺寸孔道中催化活性位点的位置, 实现了FTS产物中碳数分布的控制. 设计了醋酸盐配位Co(Co-acet) (9.4×4.2×2.5 Å)和2,2'-联吡啶配位Co(Co-bpy) (9.5×8.7×7.9 Å)两种比MFI结构的10元环孔道(5.5 Å)尺寸更小和更大的Co前驱体, 使得Co分别进入OMMZ的微孔(Co-acet/OMMZ)和介孔孔道(Co-bpy/OMMZ). X射线衍射和高分辨扫描透射电镜结果表明, 在Co-acet/OMMZ中, Co NPs主要以亚纳米纤维状限域在微孔孔道里, 直径约为0.9 nm; 在Co-bpy/OMMZ中, Co NPs主要以纳米颗粒状限域在介孔孔道中, 尺寸约为2.5 nm. 合成气转化反应结果表明, Co NPs限域在微孔和介孔孔道中的弱酸性Na型Co-acet/Na-OMMZ和Co-bpy/Na-OMMZ催化剂分别显示出66.5%的煤油选择性和65.3%的柴油选择性. Co NPs限域在具有Brönsted酸位点的H型Co-acet/H-OMMZ和Co-bpy/H-OMMZ催化剂时, 分别显示了76.7%的汽油选择性和70.8%的煤油选择性. 催化结果表明, 在Co NPs位于OMMZ有序介孔中的Co-bpy/OMMZ上形成的烃类产物碳数比位于微孔中的Co-acet/OMMZ上形成的产物碳数高, 意味着介孔中均匀分布的Co NPs可以缓解重质烃的C-C裂解, 而且Co-bpy/OMMZ的CH₄选择性低于Co-acet/OMMZ, 表明介孔中的Co NPs上重质烃的氢解作用受到抑制. 几乎不含Brönsted酸的Co/Na-OMMZ有效抑制了重质烃的裂解, 其产物碳数比Co/H-OMMZ更大.
综上, 本文通过选择不同尺寸的Co前驱体, 成功地调控了有序介孔MFI分子筛中Co金属颗粒的尺寸和位置分布, 从而抑制长链烃的C-C裂解, 实现了液态烃燃料在特定碳数范围的可控分布. 该工作为设计合成直接生产重质烃燃料的FTS催化剂提供了一条有效的策略.

关键词: 费托合成, 重质液态烃燃料, Co纳米颗粒, 有序介孔MFI分子筛, C-C裂解

Abstract:

Designing Fischer-Tropsch synthesis (FTS) catalysts to selectively produce liquid hydrocarbon fuels is a crucial challenge. Herein, we selectively introduced Co nanoparticles (NPs) into the micropores and mesopores of an ordered mesoporous MFI zeolite (OMMZ) through impregnation, which controlled the carbon number distribution in the FTS products by tuning the position of catalytic active sites in differently sized pores. The Co precursors coordinated by acetate with a size of 9.4 × 4.2 × 2.5 Å and by 2,2'-bipyridine with a size of 9.5 × 8.7 × 7.9 Å, smaller and larger than the micropores (ca. 5.5 Å) of MFI, made the Co species incorporated in OMMZ's micropores and mesopores, respectively. The carbon number products synthesized with the Co NPs confined in mesopores were larger than that in micropores. The high jet and diesel selectivities of 66.5% and 65.3% were achieved with Co NPs confined in micropores and mesopores of less acidic Na-type OMMZ, respectively. Gasoline and jet selectivities of 76.7% and 70.8% were achieved with Co NPs confined in micropores and mesopores of H-type OMMZ with Brönsted acid sites, respectively. A series of characterizations revealed that the selective production of diesel and jet fuels was due to the C-C cleavage suppressing of heavier hydrocarbons by the Co NPs located in mesopores.

Key words: Fischer-Tropsch synthesis, Heavy liquid hydrocarbon fuel, Co nanoparticle, Ordered mesoporous MFI zeolite, C-C cleavage

龚能, 邓权政, 王雨娇, 王自陶, 韩璐, 吴鹏, 车顺爱. MFI介孔分子筛限域封装Co纳米颗粒选择性催化合成气转化为重质液态烃燃料[J]. 催化学报, 2025, 68: 246-258.

Neng Gong, Quanzheng Deng, Yujiao Wang, Zitao Wang, Lu Han, Peng Wu, Shun’ai Che. Co nanoparticles confined in mesopores of MFI zeolite for selective syngas conversion to heavy liquid hydrocarbon fuels[J]. Chinese Journal of Catalysis, 2025, 68: 246-258.

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图/表 12

Fig. 1 Strategy for confining the Co NPs in micropores and mesopores of OMMZ for selective FTS of liquid fuels with controlled carbon number distribution, which would be realized by impregnation with smaller precursor of Co-acet (9.4 × 4.2 × 2.5 ?) and larger precursor of Co-bpy (9.5 × 8.7 × 7.9 ?) than the 10-MR micropores (ca. 5.5 ?) of MFI, respectively. (a) shows the low- and high-angle XRD patterns of Na-OMMZ, Co-acet/Na-OMMZ and Co-bpy/Na-OMMZ. Na-OMMZ show well-resolved diffraction peaks centered at 2θ = 1.50° due to the presence of ordered mesostructure with a d-spacing of 5.9 nm. The mesostructured-related peaks are invisible in Co-acet/Na-OMMZ and Co-bpy/Na-OMMZ (Fig. 1(a1)), which is possibly due to that the mesopores are partially occupied by Co NPs. The high-angle XRD patterns indicate all samples possess the pure MFI

Fig. 1. Morphology and structure of Na-OMMZ, Co-acet/Na-OMMZ and Co-bpy/Na-OMMZ. Low- and high-angle XRD patterns (a1,2), N2 adsorption-desorption isotherms and pore size distributions (b1,2). SEM images, HAADF-STEM images, elemental mappings and structural models of Na-OMMZ (c1-4), Co-acet/Na-OMMZ (d1-4) and Co-bpy/Na-OMMZ (e1-4).

Table 1 Textural properties, element composition and acidity amounts of different zeolites before and after Co loading.

Sample	A_BET^a (m² g^-1)	A_ext^b (m² g^-1)	Pore size^c (nm)	V_micro^d (cm³ g^-1)	V_total^e (cm³ g^-1)	Si/Al ratio^f	Loading Co^f (wt%)	Amounts of acid sites^g
Sample	A_BET^a (m² g^-1)	A_ext^b (m² g^-1)	Pore size^c (nm)	V_micro^d (cm³ g^-1)	V_total^e (cm³ g^-1)	Si/Al ratio^f	Loading Co^f (wt%)	B (μmol g^-1)	L (μmol g^-1)
Na-bulky ZSM-5	362	37	3.2	0.15	0.44	112	—	—	102.2
Na-meso-ZSM-5	388	168	3.5	0.09	0.46	111	—	—	106.0
Na-OMMZ	856	505	3.6	0.21	0.67	90	—	—	112.4
H-bulky ZSM-5	366	49	3.4	0.15	0.41	109	—	65.8	40.5
H-meso-ZSM-5	408	165	3.5	0.09	0.49	110	—	50.4	50.9
H-OMMZ	863	503	3.6	0.21	0.70	98	—	22.0	73.8
Co-acet/Na-bulky ZSM-5	317	63	3.5	0.12	0.38	105	9.9	—	84.4
Co-acet/Na-meso-ZSM-5	371	126	3.5	0.13	0.46	111	9.4	—	74.0
Co-bpy/Na-meso-ZSM-5	370	136	3.5	0.10	0.44	112	9.3	—	76.3
Co-acet/Na-OMMZ	508	334	4.3	0.12	0.50	81	9.1	—	79.8
Co-bpy/Na-OMMZ	574	388	4.4	0.12	0.55	84	8.8	—	78.3
Co-acet/H-bulky ZSM-5	355	81	3.5	0.13	0.36	102	9.6	25.8	48.3
Co-acet/H-meso-ZSM-5	369	131	3.7	0.11	0.47	116	9.6	22.3	48.9
Co-bpy/H-meso-ZSM-5	345	154	3.5	0.09	0.47	115	9.5	28.1	52.2
Co-acet/H-OMMZ	534	345	4.1	0.14	0.54	104	9.5	18.2	56.4
Co-bpy/H-OMMZ	585	391	4.2	0.12	0.54	106	9.3	15.1	60.4

Table 2 Chemical adsorptions and Co sizes of various samples of zeolites supported Co NPs.

Sample	H₂ consumption^a (mmol g^-1)	Reduction degree^a (%)	Adsorbed H₂^b (cm³ g^-1)	Dispersity^b (%)	Mean Co size^c (nm)
Sample	H₂ consumption^a (mmol g^-1)	Reduction degree^a (%)	Adsorbed H₂^b (cm³ g^-1)	Dispersity^b (%)	fresh	used^e
Co-acet/Na-bulky ZSM-5	3.7	83.1	1.7	9.0	18.4	23.3
Co-acet/Na-meso-ZSM-5	3.4	80.6	4.2	23.5	13.6	19.3
Co-bpy/Na-meso-ZSM-5	3.6	84.6	5.2	29.4	10.6	14.3
Co-acet/Na-OMMZ	1.5	35.9	0.3	1.7	0.9^d	3.6(3.8)
Co-bpy/Na-OMMZ	1.6	39.7	0.9	5.4	2.5^d	3.8(4.0)
Co-acet/H-bulky ZSM-5	3.6	83.2	4.3	23.5	17.9	22.7
Co-acet/H-meso-ZSM-5	3.8	87.4	4.0	21.9	9.0	13.6
Co-bpy/H-mes-ZSM-5	3.8	87.2	5.0	27.7	6.5	10.2
Co-acet/H-OMMZ	1.4	33.4	0.3	1.7	—	3.4(3.5)
Co-bpy/H-OMMZ	1.2	27.7	0.2	1.1	—	3.6(3.8)

Fig. 2. Co 2p XPS spectra of Co catalysts supported on Na-type MFI (a) and H-type MFI zeolites (b). H2-TPR of Co based catalysts supported on Na-type MFI (c) and H-type MFI zeolites (d).

Fig. 3. Acidity of Na-MFI and H-MFI zeolites and Co based catalysts measured by NH3-TPD profiles (a1?a3) and pyridine-IR spectra (b1?b3).

Fig. 4. FTS performance over Co-based catalysts with Na- and H-type MFI zeolites supports. CO Conversion and selectivity of gasoline (C5-C11), jet (C8-C16) and diesel (C10-C20) (a); and distributions of carbon number in the products on different Na-(b1,2) and H-type MFI zeolites supports (c1,2). Co loading = 10 wt%, Si/Al = 100. Reaction conditions: T = 513?K, P = 2.0?MPa, H2/CO = 1.0, flow rate = 20 mL min-1, GHSV = 3600 mL gcat-1 h-1, time on stream = 10?h. The hydrocarbon selectivity was calculated by the weight fraction of target product with respect to the total hydrocarbons.

Fig. 5. Catalytic performance syngas conversion on Co-bpy/Na-OMMZ (8.8 wt% Co) at different reaction temperature (a) and different GHSVs (b). Reaction conditions: H2/CO = 1, P = 2.0 MPa; (a) GHSV = 3600 mL gcat-1 h-1; (b) T = 513 K; time on stream = 10 h.

Table 3 Catalytic performances of Co based catalysts supported on different MFI zeolites.

Catalyst	CO conv.^a (%)	Hydrocarbon selectivity (%)				C_iso/C_n^a	C_olefins^b (%)	CO₂	Alcohols	CTY (mol_CO kg_Co^-1 h^-1)
Catalyst	CO conv.^a (%)	CH₄	C₂-C₄	C₅-C₂₀	C₂₁₊	C_iso/C_n^a	C_olefins^b (%)	(%)	(%)	CTY (mol_CO kg_Co^-1 h^-1)
Co-acet/Na-bulky ZSM-5	10.1	5.2	13.1	66.3	15.4	0.3	27.7	4.3	7.6	78
Co-acet/Na-meso-ZSM-5	21.9	3.1	6.4	64.7	25.8	0.1	30.8	6.5	4.6	178
Co-bpy/Na-meso-ZSM-5	22.5	2.6	4.9	65.9	26.6	0.04	28.0	4.1	4.5	185
Co-acet/Na-OMMZ	35.9	7.5	6.9	80.4	5.2	1.1	32.7	2.1	1.0	301
Co-bpy/Na-OMMZ	38.2	5.8	5.1	77.3	11.8	0.6	28.0	3.6	0.9	331
Co-acet/H-bulky ZSM-5	29.7	10.2	7.7	70.3	11.8	0.4	35.6	2.4	1.4	236
Co-acet/H-meso-ZSM-5	35.1	8.5	7.9	76.4	7.2	1.1	38.0	5.5	0.7	279
Co-bpy/H-meso-ZSM-5	37.7	7.6	7.7	77.3	7.4	0.9	31.3	1.6	0.7	303
Co-acet/H-OMMZ	34.0	7.1	6.4	86.5	—	3.0	35.2	1.5	0.1	273
Co-bpy/H-OMMZ	31.5	5.7	5.5	88.8	—	3.8	22.1	0.6	0.1	258

Fig. 6. Time on stream (a) and products distribution (b) of Co based catalysts supported on OMMZ after 120 h. Reaction conditions: H2/CO = 1, P = 2.0 MPa, T = 513 K, GHSV = 3600 mL gcat-1 h-1, time on stream = 120 h.

Fig. 7. HAADF-SETM images of used Co based catalysts for syngas conversion. Used Co-acet/Na-OMMZ after 10 h (a1) and 120 h (a2), used Co-bpy/Na-OMMZ after 10 h (b1) and 120 h (b2).

Fig. 8. XRD patterns (a1,b1) and Co 2p XPS spectra (a2,b2) of used Co based catalysts supported on Na-OMMZ and H-OMMZ for syngas conversion after 10 and 120 h.

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MFI介孔分子筛限域封装Co纳米颗粒选择性催化合成气转化为重质液态烃燃料

Co nanoparticles confined in mesopores of MFI zeolite for selective syngas conversion to heavy liquid hydrocarbon fuels

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