CO优先氧化反应MnCu/Ce催化剂的制备及性能

武嘉欣; 韩蛟; 李学; 邢月; 张财顺; 刘道胜; 侯晓宁; 刘雅杰; 张磊; 高志贤

doi:10.19906/j.cnki.JFCT.2023080

CO优先氧化反应MnCu/Ce催化剂的制备及性能

doi: 10.19906/j.cnki.JFCT.2023080

武嘉欣^1,,
韩蛟^1,,
李学^2,,
邢月^1,,
张财顺^1,,
刘道胜^1,,
侯晓宁^3,,
刘雅杰^4,,
张磊^1, ,,
高志贤^1, ,

1.
辽宁石油化工大学石油化工学院, 辽宁抚顺 113001
2.
中石油天津天然气管道有限公司, 天津 300457
3.
山西师范大学化学与材料科学学院, 山西太原 030032
4.
晋中学院化学化工系, 山西晋中 030619

基金项目: 国家自然科学基金（22379059），辽宁省应用基础研究计划项目（2023JH2/101300224），辽宁省教育厅服务地方项目（揭榜挂帅）（LJKFZ20220201），辽宁省教育厅面上项目（LJKMZ20220728），山西省应用基础研究青年基金项目（20210302124338）和辽宁石油化工大学引进人才科研启动基金资助项目（2019-XJJL-028）

详细信息

通讯作者:
E-mail: lnpuzhanglei@163.com

gaozx@lnpu.edu.cn

中图分类号: O643
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- 被引次数: 0
出版历程
- 收稿日期: 2023-08-22
- 修回日期: 2023-11-23
- 录用日期: 2023-11-23
- 网络出版日期: 2023-12-13
- 刊出日期: 2024-04-03

Preparation and properties of MnCu/Ce catalyst for CO preferential oxidation reaction

WU Jiaxin^1
,,
HAN Jiao^1
,,
LI Xue^2
,,
XING Yue^1
,,
ZHANG Caishun^1
,,
LIU Daosheng^1
,,
HOU Xiaoning^3
,,
LIU Yajie^4
,,
ZHANG Lei^{1
, ,},
GAO Zhixian^{1
, ,}

1.
School of Petrochemical Engineering, Liaoning Petrochemical University, Fushun 113001, China
2.
Petrochina Tianjin Gas Pipeline Co., LTD., Petrochina, Tianjin 300457, China
3.
School of Chemistry and Materials Science, Shanxi Normal University, Taiyuan 030032, China
4.
Department of Chemistry and Chemical Engineering, Jinzhong University, Jinzhong 030619, China

Funds: The project was supported by National Natural Science Foundation of China (22379059), Applied Basic Research Program Project of Liaoning Province (2023JH2/101300224), Service Local Project of the Education Department of Liaoning Province (Enlisting and Leading) (LJKFZ20220201), General Project of the Educational Department of Liaoning Province (LJKMZ20220728), Fundamental Research Program (Free Exploration) of Shanxi Province (20210302124338), Supported by Talent Scientific Research Fund of Liaoning Petrochemical University (2019-XJJL-028)

摘要

摘要: 采用共浸渍法制备较低Cu含量的MnCu/Ce催化剂，通过XRD、BET、H₂-TPR、XPS和CO₂-TPD等表征手段对催化剂进行表征，考察催化剂焙烧温度对催化剂结构、性质及其在含有CO₂的富氢气氛下对CO优先氧化性能的影响。结果表明，MnCu/Ce催化剂均有Cu/Mn-O-Ce固溶体形成，其中，在焙烧温度600 ℃制备的催化剂中，Mn与Cu、Ce之间相互作用较强，形成较多三元氧化物固溶体，氧空位/Ce³⁺含量高，具备良好的CO-Prox活性。此外，对反应条件的考察发现，添加不同分压Ar对催化剂的CO-Prox活性影响较小，气体空速和氧过量系数对催化剂活性影响较大，且反应原料气中CO₂的存在对CO-Prox反应有负面影响。氧过量系数为1.2、空速范围为20266−30400 mL/(g·h)时，CO转化率最高，达到94.7%。
- 低含量铜 /
- 焙烧温度 /
- 氧化铈 /
- CO₂/H₂气氛 /
- 反应条件
Abstract: The MnCu/Ce catalyst with a lower Cu content was prepared by co-impregnation method, and then was characterized by XRD, BET, H₂-TPR, XPS and CO₂-TPD. The effects of calcination temperature on the structure and properties of the catalyst and the preferential oxidation of CO in a hydrogen-rich atmosphere containing CO₂ were investigated. The results indicated that Cu/Mn-O-Ce solid solution was formed in all MnCu/Ce catalysts. Of theses sample, the one calcined at 600 ℃ had strong interaction among Mn, Cu and Ce, formed more ternary oxide solid solution with more oxygen vacancies/Ce³⁺, and revealed good CO-Prox activity. In addition, it was found that the addition of different percentage of Ar had little effects on the CO-Prox activity of the catalyst, while the space velocity and oxygen excess coefficient had great effects on the catalytic performance, and the presence of CO₂ in the reaction feedstock gas had a negative effect on the CO-Prox reaction. At an oxygen excess coefficient of 1.2 and the space velocity of 20266−30400 mL/(g·h), the highest CO conversion rate reached 94.7%.
- low content copper /
- roasting temperature /
- cerium oxide /
- CO₂/H₂ atmosphere /
- reaction condition

HTML全文

FIG. 3080. FIG. 3080.

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图 1 (a) CeO₂和MnCu/Ce-t催化剂的XRD谱图；(b) CeO₂ (111)晶面放大图

Figure 1 (a) XRD spectra of CeO₂ and MnCu/Ce-t catalysts; (b) CeO₂ (111) enlarged view of crystal plane

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图 2 CeO₂ (PDF:78-0694)、CeO₂样品和MnCu/Ce-t催化剂(331)晶面的衍射峰相对强度图

Figure 2 The relative intensity of the diffraction peaks of CeO₂(PDF:78-0694), CeO₂ sample and MnCu/Ce-t catalysts (331) crystal faces

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图 3 CeO₂和MnCu/Ce-t催化剂的N₂吸附-脱附等温线

Figure 3 N₂ adsorption desorption isotherms of CeO₂ and MnCu/Ce-t catalysts

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图 4 CeO₂和MnCu/Ce-t催化剂的BJH孔径分布

Figure 4 BJH pore size distribution curves for CeO₂ and MnCu/Ce-t catalysts

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图 5 CeO₂和MnCu/Ce-t催化剂的氢气程序升温还原谱图

Figure 5 Hydrogen temperature programmed reduction spectra of CeO₂ and MnCu/Ce-t catalysts

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图 6 (a) MnCu/Ce-t催化剂Cu 2p X射线光电子能谱； (b) MnCu/Ce-t催化剂Cu LM2 X射线光电子能谱

Figure 6 (a) X-ray photoelectron spectroscopy of Cu 2p over MnCu/Ce-t catalysts; (b) X-ray photoelectron spectroscopy of Cu LM2 over MnCu/Ce-t catalysts

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图 7 MnCu/Ce-t催化剂O 1s X射线光电子能谱谱图

Figure 7 X-ray photoelectron spectroscopy of O 1s over MnCu/Ce-t catalysts

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图 8 MnCu/Ce-t催化剂Ce 3d X射线光电子能谱谱图

Figure 8 X-ray photoelectron spectroscopy of Ce 3d over MnCu/Ce-t catalysts

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图 9 MnCu/Ce-t催化剂Mn 2p X射线光电子能谱谱图

Figure 9 X-ray photoelectron spectroscopy of Mn 2p over MnCu/Ce-t catalysts

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图 10 MnCu/Ce-t催化剂CO₂程序升温脱附曲线

Figure 10 CO₂ temperature programmed desorption curve of MnCu/Ce-t catalysts

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图 11 不同反应原料气下MnCu/Ce-600催化剂一氧化碳转化率

Figure 11 CO conversion of MnCu/Ce-600 catalyst at different reaction feed gas

Reaction conditions: λ=1.2, GHSV: 20266 mL/(g·h), reaction temperature: 130 ℃, raw gas composition: CO: (0.90% CO, 0.54% O₂, 98.56% Ar); CO/H₂: (0.90% CO, 39.47% H₂, 0.99% O₂, 58.64% Ar); CO/H₂/CO₂: (0.90% CO, 11.28% CO₂, 66.77% H₂, 0.54% O₂, 20.51% Ar).

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图 12 不同反应原料气下MnCu/Ce-600催化剂一氧化碳氧化选择性

Figure 12 CO oxidation selectivity of MnCu/Ce-600 catalyst at different reaction feed gas

Reaction conditions: λ=1.2, GHSV: 20266 mL/(g·h), reaction temperature: 130 ℃.

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图 13 MnCu/Ce-t催化剂的一氧化碳转化率

Figure 13 CO conversion of MnCu/Ce-t catalysts

Reaction conditions: λ=1.2, GHSV: 20266 mL/(g·h), raw gas composition: 0.90% CO, 11.28% CO₂, 66.77% H₂, 0.54% O₂, 20.51% Ar.

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图 14 MnCu/Ce-t催化剂的一氧化碳氧化选择性

Figure 14 CO oxidation selectivity of MnCu/Ce-t catalysts

Reaction conditions: λ=1.2, GHSV: 20266 mL/(g·h), raw gas composition: 0.90% CO, 11.28% CO₂, 66.77% H₂, 0.54% O₂, 20.51% Ar.

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图 15 不同气体空速下MnCu/Ce-600催化剂一氧化碳转化率

Figure 15 CO conversion of MnCu/Ce-600 catalyst under different GHSV

Reaction conditions: λ=1.2, reaction temperature: 130 ℃.

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图 16 添加不同分压Ar下MnCu/Ce-600催化剂一氧化碳转化率

Figure 16 CO conversion of MnCu/Ce-600 catalyst under different partial pressure Ar

Reaction conditions: λ=1.2, GHSV: 20266 mL/(g·h), reaction temperature: 130 ℃.

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图 17 不同氧过量系数下MnCu/Ce-600催化剂一氧化碳转化率

Figure 17 CO conversion of MnCu/Ce-600 catalyst at different excess oxygen coefficient

GHSV: 20266 mL/(g·h), reaction temperature: 130 ℃.

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表 1 XRD的最强峰位置、晶胞参数和平均晶粒尺寸

Table 1 Location of the strongest peak, cell parameters and average grain size of XRD

Catalyst	Peak position of (111) plane/(°)	CeO₂ cell parameter/Å	Average size of grains/nm
CeO₂	28.67	5.3969	28.3
MnCu/Ce-400	28.61	5.4032	28.2
MnCu/Ce-500	28.59	5.4045	28.5
MnCu/Ce-600	28.59	5.4039	27.5
MnCu/Ce-700	28.61	5.4032	28.6

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表 2 CeO₂和MnCu/Ce-t催化剂的物理化学性质

Table 2 Physical chemical properties of CeO₂ and MnCu/Ce-t catalysts

Catalyst	Specific surface area /(m²·g⁻¹)	Pore volume /(cm³·g⁻¹)	Average pore size/nm
CeO₂	24.3	0.0577	9.49
MnCu/Ce-400	16.9	0.0568	13.48
MnCu/Ce-500	16.7	0.0497	11.87
MnCu/Ce-600	17.0	0.0514	12.10
MnCu/Ce-700	10.5	0.0524	19.87

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表 3 CeO₂和MnCu/Ce-t催化剂的氢气程序升温还原测试结果

Table 3 Hydrogen temperature programmed reduction test results of CeO₂ and MnCu/Ce-t catalysts

Catalyst	H₂ consumption/(μmol·g⁻¹)
Catalyst	α	β	γ
MnCu/Ce-400	129.6	201.1	—
MnCu/Ce-500	111.6	152.7	62.3
MnCu/Ce-600	108.1	143.8	67.3
MnCu/Ce-700	120.0	113.2	48.3

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表 4 MnCu/Ce-t催化剂的XPS曲线拟合结果

Table 4 XPS curve fitting results of MnCu/Ce-t catalysts

Catalyst	/%
	Ce³⁺/ (Ce³⁺+Ce⁴⁺)	O_ads/ (O_ads+O_lat)	Mn^b/(Mn²⁺+Mn³⁺+Mn⁴⁺)
	Ce³⁺/ (Ce³⁺+Ce⁴⁺)	O_ads/ (O_ads+O_lat)	Mn²⁺	Mn³⁺	Mn⁴⁺
MnCu/Ce-400	12.8	19.9	27.9	37.7	34.4
MnCu/Ce-500	14.0	21.1	25.2	39.9	34.9
MnCu/Ce-600	14.9	22.5	24.9	38.9	36.2
MnCu/Ce-700	13.9	20.9	24.8	40.4	34.8

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表 5 MnCu/Ce-t催化剂的CO₂程序升温脱附测试结果

Table 5 CO₂ temperature programmed desorption test results of MnCu/Ce-t catalysts

Catalyst	Total desorption/(μmol·g⁻¹)	ϕ₁		ϕ₂		ϕ₃
Catalyst	Total desorption/(μmol·g⁻¹)	temp./℃	A/%	temp./℃	A/%	temp./℃	A/%
MnCu/Ce-400	202.73	127.6	61.8	398.3	28.2	586.9	10.0
MnCu/Ce-500	193.23	125.5	58.0	404.8	27.3	578.5	14.7
MnCu/Ce-600	172.77	118.6	43.7	399.3	38.5	657.9	17.8
MnCu/Ce-700	99.53	103.1	47.8	383.1	38.8	747.6	13.4
Notes: temp.: peak temperature; A: peak area percentage.

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