K-Fe3O4/Ni-AlMCM-41串联催化CO2加氢制高碳烃

高新华; 卢鹏飞; 陈国辉; 郭新雨; 梁洁; 马清祥; 张建利; 范素兵; 赵天生

doi:10.19906/j.cnki.JFCT.2021024

K-Fe₃O₄/Ni-AlMCM-41串联催化CO₂加氢制高碳烃

doi: 10.19906/j.cnki.JFCT.2021024

宁夏大学省部共建煤炭高效利用与绿色化工国家重点实验室，宁夏银川 750021

基金项目: 宁夏自然科学基金（2018AAC02002），国家自然科学基金（21965029, 21968025），第四批宁夏青年科技人才托举工程（TJGC2019022）和中国科学院“西部之光”（XAB2019AW02）项目资助

详细信息

通讯作者:
Tel: 0951-2062323, Fax: 0951-2062323, E-mail: gxh@nxu.edu.cn

zhangjl@nxu.edu.cn

中图分类号: O643
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出版历程
- 收稿日期: 2020-11-05
- 修回日期: 2020-11-30
- 网络出版日期: 2021-03-30
- 刊出日期: 2021-04-10

Performance of K-Fe₃O₄/Ni-AlMCM-41 tandem catalyst for CO₂ hydrogenation to long-chain hydrocarbons

State Key Laboratory of High-efficiency Utilization of Coal and Green Chemical Engineering, Ningxia University, Yinchuan 750021, China

Funds: The project was supported by the Natural Science Foundation of Ningxia (2018AAC02002), the National Natural Science Foundation of China (21965029, 21968025), the Fourth Batch of Ningxia Youth Talents Supporting Program (TJGC2019022) and West Light Foundation of the Chinese Academy of Sciences (XAB2019AW02)

摘要

摘要: 分别采用溶剂热法和离子交换法制备了K-Fe₃O₄与Ni-AlMCM-41介孔材料，串联后用于催化CO₂加氢制高碳烃，采用XRD、SEM、TEM、NH₃-TPD、烯烃-TPD、ICP-OES、XRF和XPS等手段对催化剂进行了表征，研究了钾含量和Si/Al比对Fe₃O₄/Ni-AlMCM-41串联催化CO₂加氢性能影响。结果表明，Fe₃O₄为400−800 nm的球形颗粒，Ni-AlMCM-41是以弱酸为主的介孔材料；CO₂首先在K-Fe₃O₄上生成富含低碳烯烃的混合气，然后在Ni-AlMCM-41酸性位点发生聚合、加氢等反应转化为高碳烃。适当的钾含量，可以提高一段反应CO₂转化率及低碳烯烃选择性。当0.5%K-Fe₃O₄与Ni-AlMCM-41（Si/Al = 50）相串联时，两段反应器温度分别为320和250 °C，在2 MPa、空速为1000 h⁻¹和H₂/CO₂物质的量比为3的条件下，CO₂转化率达32.9%，CH₄选择性为10.9%，高碳烃选择性为49.8%，远高于单一0.5%K-Fe₃O₄催化剂上的12.2%。
- CO₂加氢 /
- 串联催化 /
- 高碳烃 /
- Ni-AlMCM-41
Abstract: The K-Fe₃O₄ and Ni-AlMCM-41 catalysts were first prepared by a solvothermal and ion-exchange methods, respectively; they are then assembled to K-Fe₃O₄/Ni-AlMCM-41 tandem catalyst for CO₂ hydrogenation to long-chain hydrocarbons. The catalyst samples were characterized in detail by means of XRD, SEM, TEM, NH₃-TPD, olefin-TPD, ICP-OES, XRF and XPS; the effect of potassium modification and Si/Al ratio on the performance of Fe₃O₄/Ni-AlMCM-41 tandem catalyst in the hydrogenation of CO₂ was investigated. The results illustrate that the Fe₃O₄ component has a uniform spherical particles in the size range of 400–800 nm, whilst the Ni-AlMCM-41 component displays mesoporous structure, dominantly with weak acid sites on the surface. CO₂ is first converted to gaseous products rich in light olefins over the K-Fe₃O₄ catalyst and the light olefins is then transformed to long-chain hydrocarbons by a series of oligomerization and hydrogenation reactions over the acid sites of Ni-AlMCM-41. Appropriate content of potassium can improve the selectivity to light olefins over the Fe₃O₄ catalyst in the first stage. In particular, for CO₂ hydrogenation under 2 MPa and with a space velocity of 1000 h⁻¹ and a H₂/CO₂ ratio of 3, when 0.5%K-Fe₃O₄ (320 °C) is connected with Ni-AlMCM-41(Si/Al = 50) (250 °C), the conversion of CO₂ reaches 32.9% and the selectivities to CO, CH₄, and long-chain hydrocarbons are 7.1%, 10.9% and 49.8%, respectively. That is, the selectivity to long-chain hydrocarbons over the K-Fe₃O₄/Ni-AlMCM-41 catalyst (49.8%) is much higher than that over the single K-Fe₃O₄ catalyst (12.2%).
- CO₂ hydrogenation /
- tandem catalysis /
- long-chain hydrocarbon /
- Ni-AlMCM-41

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FIG. 614. FIG. 614.

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图 1 K-Fe₃O₄样品的XRD谱图

Figure 1 XRD patterns of the K-Fe₃O₄ samples

a: Fe₃O₄; b: 0.5% K-Fe₃O₄; c: 1.0% K-Fe₃O₄; d: 1.5% K-Fe₃O₄

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图 2 Ni-AlMCM-41催化剂的XRD谱图

Figure 2 Small-angle (a) and wide-angle (b) XRD patterns of the Ni-AlMCM-41 catalysts

a: Ni-AlMCM-41(25); b: Ni-AlMCM-41(50); c: Ni-AlMCM-41(75)

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图 3 催化剂的SEM和TEM照片

Figure 3 SEM image of Fe₃O₄ (a) and TEM image of Ni-AlMCM-41(50) (b)

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图 4 Ni-AlMCM-41样品N₂吸附-脱附等温曲线

Figure 4 N₂ adsorption-desorption isotherms of the Ni-AlMCM-41 samples

a: Ni-AlMCM-41(25); b: Ni-AlMCM-41(50); c: Ni-AlMCM-41(75)

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图 5 Ni-AlMCM-41样品的NH₃-TPD谱图

Figure 5 NH₃-TPD profiles of the Ni-AlMCM-41 samples

a: Ni-AlMCM-41(25); b: Ni-AlMCM-41(50); c: Ni-AlMCM-41(75)

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图 6 Ni-AlMCM-41样品的XPS谱图

Figure 6 XPS spectra of various Ni-AlMCM-41 samples

(a): Ni-AlMCM-41(25); (b): Ni-AlMCM-41(50); (c): Ni-AlMCM-41(75)

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图 7 Ni-AlMCM-41(50)的烯烃-TPD-Mass谱图

Figure 7 Olefin-TPD profiles of the Ni-AlMCM-4(50)

(a): C₂H₄-TPD profiles of Ni-AlMCM-41(50), a: C₃H₆; b: C₃H₈; c: C₄H₈; d: C₅H₁₀; e: C₆H₁₀; f: C₇H₁₄; g: C₈H₁₆(b): sample gas-TPD-Mass profiles of Ni-AlMCM-41(50) (sample gas: CH₄/C₂H₄/C₂H₆/C₃H₆/C₃H₈/C₄H₈/C₄H₁₀/C₅H₁₂/CO/CO₂/H₂/N₂ = 11.1/3.3/3.0/4.1/1.0/2.1/0.5/0.5/12.0/12.1/49.3/1.0), a: C₅H₁₀; b: C₆H₁₂; c: C₇H₁₄; d: C₈H₁₆; e: C₉H₁₈; f: C₁₀H₂₀; g: C₁₁H₂₂

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图 8 催化剂的CO₂加氢反应性能

Figure 8 Performance of the Fe₃O₄/Ni-AlMCM-41 tandem catalysts in the hydrogenation of CO₂

reaction conditions: K-Fe₃O₄ (320 ℃), Ni-AlMCM-41(250 ℃), H₂/CO₂ = 3/1, GHSV=1000 h⁻¹, 2 MPa a: 0.5% K-Fe₃O₄; b: 1.0% K-Fe₃O₄; c: 1.5% K-Fe₃O₄; d: K-Fe/Ni-AlMCM-41(75); e: K-Fe/Ni-AlMCM-41(50); f: K-Fe/Ni-AlMCM-41(25)

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表 1 Ni-AlMCM-41样品织构性质

Table 1 Texture properties of the Ni-AlMCM-41 samples

Catalyst	S_BET/(m²·g⁻¹)	v_total/(cm³·g⁻¹)	d/nm
Ni-AlMCM-41(25)	469.43	0.57	4.75
Ni-AlMCM-41(50)	488.63	0.58	4.77
Ni-AlMCM-41(75)	530.24	0.60	4.76

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表 2 Ni-AlMCM-41样品的元素含量

Table 2 Element content of Ni-AlMCM-41 samples

Catalyst	Atomic percentage^a/%			Si/Al^a	Si/Al^b
Catalyst	Si	Al	Ni	Si/Al^a	Si/Al^b
Ni-AlMCM-41(25)	93.34	3.68	2.98	25.36	25.34
Ni-AlMCM-41(50)	96.15	1.95	1.9	49.31	49.40
Ni-AlMCM-41(75)	97.01	1.41	1.57	68.80	68.59
^a: calculated from ICP-OES; ^b: calculated from XRF

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表 3 Ni-AlMCM-41样品的酸中心分布及酸量

Table 3 Distribution of acid sites on the Ni-AlMCM-41 samples

Catalyst	Weak acid		Middle acid		Total amount/ (mmol·g⁻¹)
Catalyst	temperature/℃	acid amount/(mmol·g⁻¹)	temperature/℃	acid amount/(mmol·g⁻¹)	Total amount/ (mmol·g⁻¹)
Ni-AlMCM-41(25)	212	0.341	382	0.058	0.398
Ni-AlMCM-41(50)	209	0.323	381	0.056	0.379
Ni-AlMCM-41(75)	208	0.194	371	0.030	0.224
calculated from NH₃-TPD

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表 4 催化剂表面Ni 2p结合能和Ni²⁺/Ni^{δ +}比

Table 4 Binding energy of Ni 2p and the atomic ratio of Ni²⁺/Ni^δ+ on catalyst surface

Catalyst	Binding energy/eV		Area/%		Ni²⁺/Ni^δ+
Catalyst	Ni^δ+	Ni²⁺	Ni^δ+	Ni²⁺	Ni²⁺/Ni^δ+
Ni-AlMCM-41(25)	853.7	857.0	10.1	89.9	8.9
Ni-AlMCM-41(50)	853.7	857.4	13.8	86.2	6.2
Ni-AlMCM-41(75)	853.7	857.0	20.1	79.9	4.0
Calculated from XPS

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K-Fe₃O₄/Ni-AlMCM-41串联催化CO₂加氢制高碳烃

doi: 10.19906/j.cnki.JFCT.2021024

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Tel: 0951-2062323, Fax: 0951-2062323, E-mail: gxh@nxu.edu.cn

zhangjl@nxu.edu.cn

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Performance of K-Fe₃O₄/Ni-AlMCM-41 tandem catalyst for CO₂ hydrogenation to long-chain hydrocarbons

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2023年《燃料化学学报（中英文）》评优结果公布！

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