金属氧化物活化P/HZSM-5催化生物质热解气重整制备富烃生物油

doi:10.16085/j.issn.1000-6613.2022-0865

化工进展 ›› 2023, Vol. 42 ›› Issue (3): 1353-1364.DOI: 10.16085/j.issn.1000-6613.2022-0865

金属氧化物活化P/HZSM-5催化生物质热解气重整制备富烃生物油

郑云武¹^,²(), 裴涛¹^,², 李冬华¹^,², 王继大¹^,², 李继容¹^,², 郑志锋¹^,³()

^1.西南林业大学林业生物质资源高效利用技术国家地方联合工程研究中心，云南昆明 650224
^2.西南林业大学材料科学与工程学院，云南昆明 650224
^3.厦门市现代农业生物质高值化技术重点实验室（厦门大学），福建省生物质高值化技术工程研究中心（厦门大学），厦门大学能源学院，福建厦门 361102

收稿日期:2022-05-10 修回日期:2022-07-07 出版日期:2023-03-15 发布日期:2023-04-10
通讯作者: 郑志锋
作者简介:郑云武（1983—），男，博士，副教授，硕士生导师，研究方向为生物质热化学转化。E-mail：zyw85114@163.com。
基金资助:
国家重点研发计划(2019YFD1002404);国家自然科学基金(31670599);云南省高等学校大学生创新创业项目

Production of hydrocarbon-rich bio-oil by catalytic biomass pyrolysis over metal oxide improved P/HZSM-5 catalyst

ZHENG Yunwu¹^,²(), PEI Tao¹^,², LI Donghua¹^,², WANG Jida¹^,², LI Jirong¹^,², ZHENG Zhifeng¹^,³()

^1.National Joint Engineering Research Center for Highly-Efficient Utilization Technology of Forest Biomass Resources, Southwest Forestry University, Kunming 650224, Yunnan, China
^2.College of Materials Science and Engineering, Southwest Forestry University, Kunming 650224, Yunnan, China
^3.Xiamen Key Laboratory for High-valued Conversion Technology of Agricultural Biomass (Xiamen University), Fujian Provincial Engineering and Research Center of Clean and High-valued Technologies for Biomass, College of Energy, Xiamen University, Xiamen 361102, Fujian, China

Received:2022-05-10 Revised:2022-07-07 Online:2023-03-15 Published:2023-04-10
Contact: ZHENG Zhifeng

摘要/Abstract

摘要：

为了探讨催化剂的酸性和孔道结构与热解产物之间的构-效关系，采用金属改性的M-P/HZSM-5（M=Zn、Ce、Co、Cu、Ga和Mg）为催化剂，催化生物质热解气相重整制备富烃生物油，探究金属的种类对产品的产率以及选择性的影响，采用XRD、BET、NH₃-TPD、FTIR对催化剂进行表征，采用GC/MS、UV-荧光光谱和元素分析仪对重整生物油的产物组成、脱氧特性以及共轭结构进行分析，并用TGA、拉曼光谱和SEM对失活催化剂进行评价，探究其结构-性能关系以及催化失活机制。结果表明：金属的添加并未改变催化剂的骨架结构，但形成了新的金属位点，调整了催化剂酸性分布，使比表面积以及孔容下降，平均孔径增加。金属位和酸性位的协同作用明显地促进了生物油的脱氧和单环芳烃的转化，脱氧顺序为Zn>Mg>Co>Ce>HZSM-5>Ga>P>Cu，且芳烃产率与总酸含量呈正相关，较高的酸度和平均孔径以及适宜的比表面积有利于芳烃的生成。然而，较低的酸度和较小的孔径促进了烯烃化合物的转化。当采用Zn-P/HZ为催化剂时，碳氢和芳烃产率最高，为86.46%和78.29%，共轭体系最大。Zn促进了苯、甲苯和烷基苯的形成，Mg促进了二甲苯的转化，而Cu和Ga促进了轻质烯烃的形成，金属的添加明显地降低了石墨化程度，提高了抗结焦性能。

关键词: 生物质, 催化热解, 金属改性分子筛, 碳氢化合物, 构-效关系

Abstract:

The effect of acidity and texture properties of M-P/HZSM-5 zeolite on the catalytic biomass pyrolysis to produce hydrocarbon-rich bio-oil derived was investigated. Metals (Zn, Co, Ce, Cu, Mg, Ga) were incorporated into the P/HZ zeolite that was prepared via wet impregnation and systematic physicochemical characterization techniques, such as XRD, BET, NH₃-TPD and FTIR were used to obtain the acidity and textural properties. At the same time, the composition, deoxygenation characteristics and conjugate structure of the upgrading bio-oil were analyzed by GC/MS, UV-fluorescence spectrum and element analyzer. The deactivated catalyst was evaluated by TGA, Raman spectrum and SEM to explore catalytic deactivation mechanism. The results showed that, phosphorus modification significantly reduced the concentration of acid sites, especially the strong ones. This suppressed hydrogen transfer reactions and enhanced the selectivity to olefin, while promoted the stability of the catalyst. The metal loading did not change the framework structure of the catalyst, but formed new metal sites, changed the acid distribution of the catalyst, decreased the specific surface area and pore volume by coverage of the catalyst surface with metal species, and increased the average pore size. The synergistic effect of metal and acid sites significantly promoted the deoxygenation of bio-oil and increased the conversion of monocyclic aromatic hydrocarbons. The deoxygenation degree order was Zn>Mg>Co>Ce>HZSM-5>Ga>P>Cu. The yield of aromatics is positively correlated with the total acid content. High acidity, large average pore size and appropriate specific surface area are conducive to the formation of aromatics. However, low acidity and small pore size promote the conversion of olefin compounds. In addition, the best mass-transfer efficiency and conjugate effect was obtained by using the Zn-P/HZ catalyst, which led to the highest hydrocarbon and monocyclic aromatic hydrocarbons content (86.46% and 78.29%, respectively) among all the investigated metal-modified P/HZ catalysts. Zn promoted the formation of benzene, toluene and alkylbenzene, Mg promoted the conversion of xylene, while Cu and Ga promoted the formation of light olefins. The addition of metal significantly reduced the degree of graphitization and improved the coking resistance.

Key words: biomass, catalytic pyrolysis, metal modified zeolite, hydrocarbons, structure-performance relationship

中图分类号:

TQ35

郑云武, 裴涛, 李冬华, 王继大, 李继容, 郑志锋. 金属氧化物活化P/HZSM-5催化生物质热解气重整制备富烃生物油[J]. 化工进展, 2023, 42(3): 1353-1364.

ZHENG Yunwu, PEI Tao, LI Donghua, WANG Jida, LI Jirong, ZHENG Zhifeng. Production of hydrocarbon-rich bio-oil by catalytic biomass pyrolysis over metal oxide improved P/HZSM-5 catalyst[J]. Chemical Industry and Engineering Progress, 2023, 42(3): 1353-1364.

图/表 13

参考文献 43

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催化剂试样	比表面积S_BET /m²·g^-1	微孔表面积S_micro /m²·g^-1	外表面积S_ext /m²·g^-1	总孔容V_total /mL·g^-1	介孔孔容V_meso /mL·g^-1	微孔孔容V_micro /mL·g^-1	平均孔径D_{pore size} /nm^-1
HZSM-5	263.99	116.92	147.08	0.2522	0.1914	0.06083	5.95
P/HZ	188.67	116.01	70.22	0.1774	0.1171	0.06034	5.54
Zn-P/HZ	149.27	107.40	41.88	0.1158	0.05999	0.05581	6.54
Ce-P/HZ	142.23	104.81	37.43	0.1053	0.05088	0.05442	6.45
Co-P/HZ	167.06	140.96	26.09	0.1119	0.03886	0.07304	6.11
Cu-P/HZ	158.15	119.28	38.86	0.1087	0.04674	0.06196	5.44
Ga-P/HZ	142.91	100.77	42.14	0.1110	0.05862	0.05238	5.18
Mg-P/HZ	169.99	102.81	67.17	0.1283	0.06955	0.05875	6.76

催化剂试样	比表面积S_BET /m²·g^-1	微孔表面积S_micro /m²·g^-1	外表面积S_ext /m²·g^-1	总孔容V_total /mL·g^-1	介孔孔容V_meso /mL·g^-1	微孔孔容V_micro /mL·g^-1	平均孔径D_{pore size} /nm^-1
HZSM-5	263.99	116.92	147.08	0.2522	0.1914	0.06083	5.95
P/HZ	188.67	116.01	70.22	0.1774	0.1171	0.06034	5.54
Zn-P/HZ	149.27	107.40	41.88	0.1158	0.05999	0.05581	6.54
Ce-P/HZ	142.23	104.81	37.43	0.1053	0.05088	0.05442	6.45
Co-P/HZ	167.06	140.96	26.09	0.1119	0.03886	0.07304	6.11
Cu-P/HZ	158.15	119.28	38.86	0.1087	0.04674	0.06196	5.44
Ga-P/HZ	142.91	100.77	42.14	0.1110	0.05862	0.05238	5.18
Mg-P/HZ	169.99	102.81	67.17	0.1283	0.06955	0.05875	6.76

序号	催化剂的种类	热解温度/℃	产物组成	产品产率/%	参考文献
1	HZSM-5/赤泥	475	芳烃	53.44	[34]
2	HZSM-5/MCM-41	600	芳烃	41.44	[35]
3	HZSM-5	600	芳烃	34.41	[35]
4	CaO@HZSM-5	550	芳烃	31.34	[36]
5	TiO₂@HZSM-5	550	BTX	23.58	[37]
6	HZSM-5	550	BTX	16.96	[37]
7	CeO₂-ZrO₂-Al₂O₃	600	芳烃	20.23	[38]
8	ZnO@HZSM-5	500	芳烃	72.28	本研究

序号	催化剂的种类	热解温度/℃	产物组成	产品产率/%	参考文献
1	HZSM-5/赤泥	475	芳烃	53.44	[34]
2	HZSM-5/MCM-41	600	芳烃	41.44	[35]
3	HZSM-5	600	芳烃	34.41	[35]
4	CaO@HZSM-5	550	芳烃	31.34	[36]
5	TiO₂@HZSM-5	550	BTX	23.58	[37]
6	HZSM-5	550	BTX	16.96	[37]
7	CeO₂-ZrO₂-Al₂O₃	600	芳烃	20.23	[38]
8	ZnO@HZSM-5	500	芳烃	72.28	本研究

试样	C/%	H/%	O/%	N/%	S/%	H/C	O/C	热值/MJ·kg^-1	脱氧效率/%	有效氢碳比	重整常数/%
热解油	52.14	6.48	40.71	0.55	0.12	0.124	0.781	21.63	0	0.2913	0
HZSM-5	66.73	7.83	25.05	0.28	0.11	0.117	0.375	29.94	73.23	0.8329	2.3587
P/HZ	64.99	7.64	26.91	0.33	0.13	0.118	0.414	28.92	49.14	0.7750	0.7752
Zn-P/HZ	69.88	8.01	21.63	0.38	0.10	0.115	0.310	31.60	85.98	0.8961	5.6908
Ce-P/HZ	69.26	7.82	22.56	0.27	0.09	0.113	0.326	31.07	77.54	0.8553	3.0561
Co-P/HZ	67.91	6.73	24.76	0.44	0.16	0.099	0.365	29.09	76.60	0.6239	2.1147
Cu-P/HZ	60.02	6.96	32.63	0.28	0.11	0.116	0.544	25.79	38.12	0.5627	0.3588
Ga-P/HZ	65.13	6.58	27.74	0.47	0.08	0.101	0.426	27.62	51.33	0.5540	0.6047
Mg-P/HZ	68.62	7.75	23.33	0.22	0.08	0.113	0.340	30.68	80.26	0.8362	3.5192

金属氧化物活化P/HZSM-5催化生物质热解气重整制备富烃生物油

Production of hydrocarbon-rich bio-oil by catalytic biomass pyrolysis over metal oxide improved P/HZSM-5 catalyst

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