高分散Co3O4对LaCoO3乏风甲烷催化燃烧性能的影响

陈雪; 王雪峰; 王荀; 邓存宝; 曹敏敏

doi:10.1016/S1872-5813(22)60051-3

高分散Co₃O₄对LaCoO₃乏风甲烷催化燃烧性能的影响

doi: 10.1016/S1872-5813(22)60051-3

陈雪^1,,
王雪峰^1, ,,
王荀^{1, 2,},
邓存宝¹,
曹敏敏¹

1.
太原理工大学安全与应急管理工程学院, 山西太原 030024
2.
山西焦煤集团有限责任公司, 山西太原 030024

基金项目: 国家自然科学基金联合基金项目（U1810206），国家自然科学基金面上项目（51774172）

详细信息

作者简介:
王荀（1984−），女，河北保定人，博士，讲师，Tel：18634300787，E-mail：wangxun@tyut.edu.cn

通讯作者:
王雪峰（1975− ），女，辽宁阜新人，博士，副教授、硕士生导师，Tel：13303433823，E-mail：wangxuefeng01@tyut.edu.cn

中图分类号: X959
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出版历程
- 收稿日期: 2022-04-23
- 录用日期: 2022-06-21
- 修回日期: 2022-06-10
- 网络出版日期: 2022-07-19

Effect of highly dispersed Co₃O₄ on catalytic combustion of ventilation air methane of LaCoO₃

CHEN Xue^1
,,
WANG Xue-feng^{1
, ,},
WANG Xun^{1, 2
,},
DENG Cun-bao¹,
CAO Min-min¹

1.
School of Engineering for Safety and Emergency Management, Taiyuan University of Technology, Taiyuan 030024, China
2.
SHANXI COKING COAL GROUP CO., LTD. , Taiyuan 030024, China

Funds: Supported by the NSF Joint Foundation Program (U1810206) and the NSF Facial Program (51774172).

摘要

摘要: 钙钛矿因具有良好的热稳定性而广泛应用于低浓度甲烷催化燃烧，但同时存在低温催化活性低这一问题。本文采用溶胶凝胶法，通过调变镧钴比例合成了一种纳米新型钙钛矿类催化剂。利用ICP、XRD、BET、H₂-TPR、O₂-TPD和XPS等技术对催化剂进行了表征，并通过CH₄氧化活性测试评价了催化剂的催化性能。当La/Co=0.9时，在空速30000 mL/(g_cat • h)条件下，甲烷的起燃温度为382 ℃，稳定运行72 h后，甲烷转化率保持在95%以上，说明高分散性的Co₃O₄纳米颗粒有利于CH₄的低温活化，且催化剂中镧钴钙钛矿体相可提供大量的晶格氧，促进高温条件下CH₄的催化燃烧速率和催化剂的高温稳定性。通过调变镧钴比例，可有效调变催化剂中Co₃O₄纳米颗粒的分散状态，进而实现催化剂低温活性和高温稳定性的有效统一，为今后开发低成本、高活性、高稳定性的甲烷催化燃烧催化剂提供参考。
- 甲烷催化燃烧 /
- LaCoO₃ /
- Co₃O₄ /
- 高分散 /
- 晶格氧
Abstract: Perovskite is widely used in catalytic combustion of methane at low concentration because of it’s good thermal stability, but it also suffers from the major problem of low catalytic activity at low temperatures. In this paper, a new nano-type perovskite catalyst was effectively synthesized by a sol-gel method by modulating the ratio of lanthanum to cobalt. The catalysts were characterized by ICP, XRD, BET, H₂-TPR, O₂-TPD, and XPS techniques, and their catalytic performance were evaluated by CH₄ oxidation activity test. When La/Co=0.9, the catalyst exhibited good methane catalytic combustion activity and high-temperature stability. At space velocity of 30000 mL/(g_cat • h), the light-off temperature of methane is 382 ℃, and the methane conversion rate is still maintained above 95% after 72 h of stable operation, indicating that the highly dispersed Co₃O₄ nanoparticles were beneficial to the low-temperature activation of CH₄, and the lanthanum-cobalt-perovskite bulk phase in the catalyst could provide a large amount of lattice oxygen, which promotes the catalytic combustion rate of CH₄ and the high-temperature stability of the catalyst under high-temperature conditions. By modulating the lanthanum-cobalt ratio, the dispersion state of Co₃O₄ nanoparticles in the catalyst can be effectively modulated, and then the effective unification of low-temperature activity and high-temperature stability of the catalyst can be achieved, which guides the future development of low-cost, high-activity and high-stability catalysts for methane catalytic combustion.
- catalytic combustion of methane /
- lacoo₃ /
- co₃o₄ /
- high dispersion /
- lattice oxygen

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图 1 (a)镧钴系列催化剂的X射线衍射图；(b)2-Theta=36−38.5°的局部X射线衍射图

Figure 1 (a)XRD pattern of La_xCoO₃ samples；(b)XRD pattern of La_xCoO₃ samples from 36 ° to 38.5°

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图 2 La_0.9CoO₃的(a)TEM和(b)HRTEM图像

Figure 2 (a)TEM and (b) HRTEM images of La_0.9CoO₃

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图 3 (a)镧钴系列催化剂的Co 2p谱图和(b) Co 2p3/2拟合谱图

Figure 3 (a)Co 2p spectra and (b)Co 2p3/2 fitting spectra of La_xCoO₃ samples

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图 4 镧钴系列催化剂的O 1s拟合谱图

Figure 4 O 1s fitting spectra of La_xCoO₃ samples

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图 5 镧钴系列催化剂的O₂-TPD谱图

Figure 5 O₂-TPD spectra of La_xCoO₃ samples

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图 6 镧钴系列催化剂的H₂-TPR谱图

Figure 6 H₂-TPR spectra of La_xCoO₃ samples

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图 7 (a)镧钴系列催化剂的甲烷氧化活性；(b)La_0.9CoO₃在640 ℃下的稳定性测试

Figure 7 (a)Methane oxidation activity of La_xCoO₃ samples; (b)Stability test of La_0.9CoO₃ at 640 ℃(0.2g catalysts, CH₄∶O₂∶N₂=1∶20∶79, GHSV=30000 mL• g_cat⁻¹• h⁻¹)

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图 8 (a)甲烷浓度和(b)氧气浓度对La_0.9CoO₃催化甲烷燃烧的影响

Figure 8 Effects of (a)methane and (b)oxygen concentrations on methane combustion catalyzed by La_0.9CoO₃(CH₄∶O₂∶N₂=x∶20∶80−x or CH₄∶O₂∶N₂=1∶y∶99−y, GHSV=30000 mL• g_cat⁻¹• h⁻¹)

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表 1 镧钴系列催化剂的物性参数

Table 1 Physical properties of La_xCoO₃ samples

Sample	La/Co molar ratio^a	S_BET（m² •g⁻¹）^b	V（cm³ •g⁻¹）^b	d_Co3O4-XRD (nm)^c
LaCoO₃	0.917	4.436	0.034	27.76
La_0.95CoO₃	0.906	4.311	0.121	27.59
La_0.9CoO₃	0.879	5.504	0.037	28.78
La_0.8CoO₃	0.781	5.466	0.066	21.05
Co₃O₄	/	4.276	0.055	79.68
a. La/Co molar ratio determined by ICP； b. S_BET and V represent the specific surface area and pore volume of La_xCoO₃ samples； c. d_Co3O4 is calculated by Scherrer's formula.

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表 2 镧钴系列催化剂的Co 2p3/2谱图拟合数据

Table 2 Co 2p3/2 spectrum fitting data of La_xCoO₃ samples

Sample	Co^{3 +}		Co^{2 +}		Co^{3 +}/Co^{2 +}
Sample	Binding energy (eV)	Area percentage (%)	Binding energy (eV)	Area percentage (%)	Co^{3 +}/Co^{2 +}
LaCoO₃	779.53	61	781.29	39	1.56
La_0.95CoO₃	779.76	60.16	781.47	39.84	1.51
La_0.9CoO₃	779.67	47.78	781.08	52.22	0.92
La_0.8CoO₃	779.61	43.71	780.99	56.29	0.78
Co₃O₄	779.52	45.06	781.02	54.94	0.82

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表 3 镧钴系列催化剂的O 1s谱图拟合数据

Table 3 O 1s fitting data of La_xCoO₃ samples

Sample	O_latt		O_surf		O_surf/ O_latt
Sample	Binding energy (eV)	Area percentage (%)	Binding energy (eV)	Area percentage (%)	O_surf/ O_latt
LaCoO₃	528.59	36.92	530.98	63.08	1.71
La_0.95CoO₃	528.9	39.3	531.27	60.7	1.54
La_0.9CoO₃	528.85	48.1	531.3	51.9	1.08
La_0.8CoO₃	528.84	48.49	531.25	51.51	1.06
Co₃O₄	529.81	47.53	531.15	52.47	1.10

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表 4 镧钴系列催化剂的H₂-TPR拟合数据

Table 4 H₂-TPR fitting data of La_xCoO₃ samples

Sample	Peak 1 Co^{3 +}→Co^{2 +}（Co₃O₄）		Peak 2 Co^{2 +}→Co⁰（Co₃O₄） Co^{3 +}→Co^{2 +}（LaCoO₃）		Peak 3 Co^{2 +}→Co⁰（LaCoO₃）		Co₃O₄／LaCoO₃^b
Sample	T_red^a （℃）	Area percentage^a （%）	T_red （℃）	Area percentage （%）	T_red （℃）	Area percentage （%）	Co₃O₄／LaCoO₃^b
LaCoO₃	359.26	13.39	401.57	21.24	588.94	65.37	0.0149
La_0.95CoO₃	353.94	14.19	406.89	24.26	599.33	61.55	0.0623
La_0.9CoO₃	352	32.17	406.5	7.2	593.58	60.63	0.0747
La_0.8CoO₃	359.26	23.15	409.37	11.91	594.26	64.94	0.0199
Co₃O₄	350.56	22.52	447.7	77.48	／	／	／
a. T_red refers to the temperature corresponding to the maximum value of the reduction peak, and area percentage refers to the percentage of the reduction peak area to the total reduction peak area； b. According to the stoichiometric number, the relative content of Co₃O₄ and LaCoO₃ is calculated by the reduction peak area in H₂-TPR, that is, Co₃O₄/LaCoO₃ = S_{peak 1}/(0.5 × S_{peak 3}).

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表 5 甲烷催化燃烧代表性催化剂性能对比

Table 5 Performance comparison of representative catalysts for methane catalytic combustion

Number	Catalyst	Preparation method	Methane initial concentration （vol%）	GHSV (mL• g_cat⁻¹• h⁻¹)	T₁₀ （℃）	T₅₀ （℃）	T₉₀ （℃）	Stability test		References
Number	Catalyst	Preparation method	Methane initial concentration （vol%）	GHSV (mL• g_cat⁻¹• h⁻¹)	T₁₀ （℃）	T₅₀ （℃）	T₉₀ （℃）	Temperature- time	Conversion	References
1	La_0.9CoO₃	sol-gel method	1	30000	382	449	530	640 ℃-72h	96%	This work
2	Pd/Al₂O₃	impregnation	1	12000	298	346	401	370 ℃-20h	68%	[36]
3	BaMnAl₁₁O_19−d	coprecipitation	0.5	18000	545	640	/	/	/	[37]
4	Co₃O₄	coprecipitation	1	18000	285	373	455	360 ℃-30h	80%	[38]
5	LaCoO₃	template method	3	30000	370	485	578	650 ℃-70h	82%	[11]
6	LaMnO₃	template method	3	30000	405	480	570	650 ℃-70h	98%	[11]
7	MnO_x/LaMnO₃	acid etching method	2.5	30000	351	441	519	/	/	[39]
8	La_0.8Sr_0.2CoO₃	acid etching method	1	44000	385	491	595	600 ℃-24h	90%	[40]

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高分散Co₃O₄对LaCoO₃乏风甲烷催化燃烧性能的影响

doi: 10.1016/S1872-5813(22)60051-3

作者简介:
王荀（1984−），女，河北保定人，博士，讲师，Tel：18634300787，E-mail：wangxun@tyut.edu.cn

通讯作者:
王雪峰（1975− ），女，辽宁阜新人，博士，副教授、硕士生导师，Tel：13303433823，E-mail：wangxuefeng01@tyut.edu.cn

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Effect of highly dispersed Co₃O₄ on catalytic combustion of ventilation air methane of LaCoO₃

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