Study on reduction performance and kinetics of Sr-modified LaFeO3 for methane chemical looping reforming

doi:10.11949/0438-1157.20240633

Abstract

Abstract:

Chemical looping reforming of methane is a novel low-carbon hydrogen production technology. The reduction characteristics of the oxygen carrier are key factors determining the hydrogen production rate of chemical looping reforming. The effect of different proportions of Sr doping on the reduction characteristics of LaFeO₃was discussed in detail. By characterizing the octahedral distortion and surface oxygen morphology of FeO₆, the effect of Sr doping on oxygen vacancy concentration and lattice oxygen transfer was analyzed. La_0.8Sr_0.2FeO₃ exhibits significant FeO₆ octahedral distortion, showing the lowest lattice oxygen reduction temperature at 750℃. In isothermal reduction, the maximum mass loss of La_0.8Sr_0.2FeO₃ is 2—3 times that of LaFeO₃. Kinetic fitting calculations revealed that the reduction process of La_1-_x Sr _x FeO₃ is controlled by the nucleation and growth model, while also being influenced by the autocatalytic model. Among the four oxygen carriers, La_0.8Sr_0.2FeO₃ exhibits the lowest apparent activation energy. The mass gain rate of La_0.8Sr_0.2FeO₃ in steam oxidation experiments is about 4 times that of LaFeO₃, and it maintains its original phase after 20 cycles. The study of La_1-_x Sr _x FeO₃ in chemical looping reforming and multi-cycle stability provides technical and data support for the selection of materials and process optimization in methane chemical looping reforming for hydrogen production.

Key words: methane, hydrogen production, kinetics, chemical looping, perovskite

摘要：

甲烷化学链重整是新型低碳的制氢技术，载氧体还原特性是决定化学链重整制氢产率的关键因素。重点探讨了不同比例Sr掺杂对LaFeO₃还原特性的影响，通过表征FeO₆八面体畸变和表面氧形态分析了Sr掺杂对氧空位浓度、晶格氧传递的作用。La_0.8Sr_0.2FeO₃具有明显的FeO₆八面体畸变，表现出最低的晶格氧还原温度750℃，恒温还原中La_0.8Sr_0.2FeO₃的最大失重量为LaFeO₃的2~3倍。动力拟合计算发现La_1-_x Sr _x FeO₃的还原过程均受成核核增长模型控制，同时受自催化模型影响，4种载氧体中，La_0.8Sr_0.2FeO₃表现出最低的表观活化能。La_0.8Sr_0.2FeO₃在水蒸气氧化实验中的增重速率约为LaFeO₃的4倍，并且在20周期循环后保持原有物相不变。La_1-_x Sr _x FeO₃化学链重整与多周期稳定性的研究为甲烷化学链重整制氢材料选择和工艺优化提供了技术与数据支撑。

关键词: 甲烷, 制氢, 动力学, 化学链, 钙钛矿

CLC Number:

TQ 116.2⁺5

Haotian MA, Tirui JING, Chengcheng LIU, Turap YUSAN, Zhe ZHANG, Yidi WANG, Qinghong WANG, Chunmao CHEN, Chunming XU. Study on reduction performance and kinetics of Sr-modified LaFeO₃ for methane chemical looping reforming[J]. CIESC Journal, 2024, 75(12): 4532-4546.

马浩天, 荆体瑞, 刘程程, 玉散·吐拉甫, 张喆, 王一迪, 王庆宏, 陈春茂, 徐春明. Sr改性LaFeO₃用于甲烷化学链重整的还原性能与动力学研究[J]. 化工学报, 2024, 75(12): 4532-4546.

Figures/Tables 19

Fig.1 Diagram of CLSR reaction process

Table 1 Differential and integral expressions of mechanism function

函数名称	机理	函数编号	g(α)	f(α)
Avrami-Erofeev方程	成核核增长	A2	[-ln(1-α)]^1/2	2(1-α)[-ln(1-α)]^1/2
		A3	[-ln(1-α)]^1/3	3(1-α)[-ln(1-α)]^2/3
		A4	[-ln(1-α)]^1/4	4(1-α)[-ln(1-α)]^3/4
Prout-Tompkins方程	自催化模型	B1	ln[α/(1-α)]	α/(1-α)
Mampel Power法则	相界面反应(一维)	C1	α	1
收缩模型	收缩圆柱体(面积),相界面反应,圆柱形对称	C2	1- (1-α)^1/2	2(1-α)^1/2
收缩模型	收缩球体(体积),相界面反应,球形对称	C3	1- (1-α)^1/3	3(1-α)^2/3
Jander方程	一维扩散模型	D1	α²	$\frac{1}{2}$ α
Jander方程	三维扩散,球形对称	D3	1- $\frac{2}{3}$ α- (1-α)^2/3	$\frac{3}{2}$ (1-α)^2/3[1- (1-α)^1/3]
反应级数模型	一级化学反应	R1	-ln(1-α)	1-α
	二级化学反应	R2	[1/(1-α)]-1	(1-α)²
	三级化学反应	R3	[1/(1-α)²]-1	(1-α)³

Table 1 Differential and integral expressions of mechanism function

函数名称	机理	函数编号	g(α)	f(α)
Avrami-Erofeev方程	成核核增长	A2	[-ln(1-α)]^1/2	2(1-α)[-ln(1-α)]^1/2
		A3	[-ln(1-α)]^1/3	3(1-α)[-ln(1-α)]^2/3
		A4	[-ln(1-α)]^1/4	4(1-α)[-ln(1-α)]^3/4
Prout-Tompkins方程	自催化模型	B1	ln[α/(1-α)]	α/(1-α)
Mampel Power法则	相界面反应(一维)	C1	α	1
收缩模型	收缩圆柱体(面积),相界面反应,圆柱形对称	C2	1- (1-α)^1/2	2(1-α)^1/2
收缩模型	收缩球体(体积),相界面反应,球形对称	C3	1- (1-α)^1/3	3(1-α)^2/3
Jander方程	一维扩散模型	D1	α²	$\frac{1}{2}$ α
Jander方程	三维扩散,球形对称	D3	1- $\frac{2}{3}$ α- (1-α)^2/3	$\frac{3}{2}$ (1-α)^2/3[1- (1-α)^1/3]
反应级数模型	一级化学反应	R1	-ln(1-α)	1-α
	二级化学反应	R2	[1/(1-α)]-1	(1-α)²
	三级化学反应	R3	[1/(1-α)²]-1	(1-α)³

Fig.2 XRD patterns of La1-x Sr x FeO3 oxygen carrier

Table 2 Crystal structure parameters of La1-x Sr x FeO3 oxygen carrier

参数		LaFeO₃	La_0.8Sr_0.2FeO₃	La_0.6Sr_0.4FeO₃	La_0.4Sr_0.6FeO₃
键长/nm	Fe—O₍₁₎	0.20073	0.204536	0.2116	0.1941
	Fe—O₍₂₎	0.20099	0.212309	0.1960	0.1920
	Fe—O₍₂₎	0.20020	0.180842	0.1960	0.1970
键角/(°)	Fe—O₍₁₎—Fe	155.90	145.35	134.80	170.50
键角/(°)	Fe—O₍₂₎—Fe	157.01	169.06	166.20	177.00
键长方差	$Δ = \frac{1}{6} \sum {(\frac{R_{i} - R_{a v}}{R_{a v}})}^{2} (10^{- 3})$	0.0027	4.50	1.30	0.11

Table 2 Crystal structure parameters of La1-x Sr x FeO3 oxygen carrier

参数		LaFeO₃	La_0.8Sr_0.2FeO₃	La_0.6Sr_0.4FeO₃	La_0.4Sr_0.6FeO₃
键长/nm	Fe—O₍₁₎	0.20073	0.204536	0.2116	0.1941
	Fe—O₍₂₎	0.20099	0.212309	0.1960	0.1920
	Fe—O₍₂₎	0.20020	0.180842	0.1960	0.1970
键角/(°)	Fe—O₍₁₎—Fe	155.90	145.35	134.80	170.50
键角/(°)	Fe—O₍₂₎—Fe	157.01	169.06	166.20	177.00
键长方差	$Δ = \frac{1}{6} \sum {(\frac{R_{i} - R_{a v}}{R_{a v}})}^{2} (10^{- 3})$	0.0027	4.50	1.30	0.11

Table 3 XRF compositional analysis of La1-x Sr x FeO3 oxygen carrier

载氧体	Fe₂O₃/% （质量分数）	La₂O₃/% （质量分数）	SrO/% （质量分数）	La/% （质量分数）	Sr/% （质量分数）	La/Sr 摩尔比	摩尔比理论值
LaFeO₃	34.32	64.76	—	55.23	—	—	—
La_0.8Sr_0.2FeO₃	35.12	53.72	10.22	45.81	8.64	0.78/0.22	0.8/0.2
La_0.6Sr_0.4FeO₃	35.71	42.32	21.01	36.09	17.76	0.57/0.43	0.6/0.4
La_0.4Sr_0.6FeO₃	34.36	27.11	36.57	28.12	27.92	0.39/0.61	0.4/0.6

Fig.3 O 1s XPS spectrum of La1-x Sr x FeO3 oxygen carrier

Table 4 XPS results of oxygen element O 1s in La1-x Sr x FeO3 oxygen carrier

载氧体	不同氧元素百分比/%
载氧体	O1（O^2-）	O2 （ $O_{2}^{2 -}$ ,O^-）	O3 （—OH, $C O_{3}^{2 -}$ ）	O4 （H₂O）	O_ads/O_latt
LaFeO₃	50.53	15.32	18.06	16.09	0.30
La_0.8Sr_0.2FeO₃	37.18	18.82	28.27	15.73	0.51
La_0.6Sr_0.4FeO₃	33.39	15.84	33.82	16.96	0.47
La_0.4Sr_0.6FeO₃	42.68	16.55	29.06	11.72	0.39

Table 4 XPS results of oxygen element O 1s in La1-x Sr x FeO3 oxygen carrier

载氧体	不同氧元素百分比/%
载氧体	O1（O^2-）	O2 （ $O_{2}^{2 -}$ ,O^-）	O3 （—OH, $C O_{3}^{2 -}$ ）	O4 （H₂O）	O_ads/O_latt
LaFeO₃	50.53	15.32	18.06	16.09	0.30
La_0.8Sr_0.2FeO₃	37.18	18.82	28.27	15.73	0.51
La_0.6Sr_0.4FeO₃	33.39	15.84	33.82	16.96	0.47
La_0.4Sr_0.6FeO₃	42.68	16.55	29.06	11.72	0.39

Table 5 Specific surface area and porosity data of La1-x Sr x FeO3 oxygen carriers

载氧体	比表面积/ (m²/g)	孔体积/ (10^-3 cm³/g)	平均孔径/nm
LaFeO₃	15.27	2.4	6.41
La_0.8Sr_0.2FeO₃	19.35	3.7	10.99
La_0.6Sr_0.4FeO₃	17.91	3.2	5.88
La_0.4Sr_0.6FeO₃	12.11	1.7	4.51

Fig.4 CH4-TPR mass loss rate of La1-x Sr x FeO3 oxygen carrier

Fig.5 10% CH4 reduction atmosphere isothermal reduction reaction spectra of La1-x Sr x FeO3 oxygen carrier

Fig.6 Mass loss rate curves of La1-x Sr x FeO3 oxygen carrier

Fig.7 Fitting curves of common kinetic equations for reaction of La0.8Sr0.2FeO3 with CH4 at different temperatures (colored lines represent fitting results of different mechanism functions, black lines represent experimental results)

Fig.8 Arrhenius plot for evaluating activation energy of reduction process

Table 6 Main kinetic parameters of La1-x Sr x FeO3 oxygen carriers in different kinetic models

载氧体	成核核增长模型			自催化枝状模型
载氧体	活化能/(kJ/mol)	指前因子/s^-1	相关系数	活化能/(kJ/mol)	指前因子/s^-1	相关系数
LaFeO₃	159.454	1.337907×10⁶	0.9217	164.87	1.35×10⁷	0.9922
La_0.8Sr_0.2FeO₃	112.798	8.586×10³	0.9933	135.93	4.024×10⁵	0.9595
La_0.6Sr_0.4FeO₃	163.684	2×10⁶	0.9927	167.27	1.09×10⁷	0.9912
La_0.4Sr_0.6FeO₃	167.350	1.988×10⁶	0.9961	144.91	8.4×10⁵	0.9990

Fig.9 Comparison between experimental data and fitted data from kinetic models

Table 7 Reduction kinetic models and activation energies of oxygen carriers reported in literature

载氧体	温度区间/K	实验方法	模型	E_a/（kJ/mol）	文献
LaFeO₃	1023~1173	等温TGA	成核核增长/自催化	159/165	本研究
LaFeO₃	1073~1223	等温质谱	成核核增长	151	[20]
MnFe₂O₄	1073~1173	等温TGA	扩散控制	139	[46]
CeO₂	873~1123	等温TCD	—	137	[47]
CoWO₄	1123~1223	等温TGA	一级化学反应	221	[48]

Fig.10 Mass gain and rate of mass increase during steam oxidation regeneration

Fig.11 (a) Mass change of LaFeO3 during CH4 reduction-air oxidation process;(b) Mass change of La0.8Sr0.2FeO3 during CH4 reduction-air oxidation process; (c) XRD patterns comparison of regenerated and fresh oxygen carrier

Fig.12 SEM-Mapping of initial LaFeO3 (a), LaFeO3 after 20 cycles (b), initial La0.8Sr0.2FeO3 (c), La0.8Sr0.2FeO3 after 20 cycles (d)

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Study on reduction performance and kinetics of Sr-modified LaFeO₃ for methane chemical looping reforming

Sr改性LaFeO₃用于甲烷化学链重整的还原性能与动力学研究

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