鄂尔多斯褐煤显微组分结构与其热解特性间的关系

doi:10.16085/j.issn.1000-6613.2024-0397

化工进展 ›› 2024, Vol. 43 ›› Issue (5): 2370-2385.DOI: 10.16085/j.issn.1000-6613.2024-0397

• 化石能源的清洁高效转化利用 • 上一篇

鄂尔多斯褐煤显微组分结构与其热解特性间的关系

吴琪¹(), 白柏杨², 尹永杰¹, 马晓迅¹()

^1.西北大学化工学院，碳氢资源清洁利用国际科技合作基地，陕北能源先进化工利用技术教育部工程研究中心，陕西省洁净煤转化工程技术研究中心，陕北能源化工产业发展协同创新中心，陕西西安 710127
^2.陕西煤基特种燃料研究院有限公司，陕西西安 710069

收稿日期:2024-03-11 修回日期:2024-04-04 出版日期:2024-05-15 发布日期:2024-06-15
通讯作者: 马晓迅
作者简介:吴琪（1999—），男，硕士研究生，研究方向为煤炭的清洁高效利用。E-mail：13546626853@163.com。
基金资助:
国家科学技术基金(21536009);陕西省科技计划(2017ZDCXL-GY-10-03);陕西省教育部专项科研计划(19JK0854)

Relationship between the structure of macerals of Ordos lignite and its pyrolysis characteristics

WU Qi¹(), BAI Boyang², YIN Yongjie¹, MA Xiaoxun¹()

^1.International Science & Technology Cooperation Base of MOST for Clean Utilization of Hydrocarbon Resources, Chemical Engineering Research Center of the Ministry of Education for Advanced Use Technology of Shanbei Energy, Shaanxi Research Center of Engineering Technology for Clean Coal Conversion, Collaborative Innovation Center for Development of Energy and Chemical Industry in Northern Shaanxi, School of Chemical Engineering, Northwest University, Xi’an 710127, Shaanxi, China
^2.Shannxi Coal Based Special Fuel Research Institute Co. , Ltd. , Xi’an 710069, Shannxi, China

Received:2024-03-11 Revised:2024-04-04 Online:2024-05-15 Published:2024-06-15
Contact: MA Xiaoxun

摘要/Abstract

摘要：

采用浮沉分离法将鄂尔多斯褐煤分离成富镜质组（EL-V）和富惰质组（EL-I），通过工业分析、元素分析、X射线衍射光谱（XRD）、傅里叶变换红外光谱（FTIR）和固体核磁（¹³C NMR）分析了原煤及显微组分的结构和组成。采用粉-粒流化床和TG-FTIR装置分别考察了原煤及显微组分的热解特性和气态挥发物的逸出规律，进一步构建原煤及显微组分的大分子结构模型，并进行了量子化学计算，认识了化学键的断裂规律。结果表明，富镜质组的挥发分含量较高，含有丰富的烷基侧链，热失重速率最大，表明镜质组的热解反应性较强。与原煤和惰质组相比，富镜质组热解气体含量和焦油含量较高，且热解焦油含有较多的脂肪烃和轻质芳烃（TXE）。富惰质组的H/C比较低，含氧量和芳环缩合程度较高，所得热解焦油中多环芳烃和酚类物质含量较高。此外，通过TG-FTIR重点分析了CO₂、CO、CH₄、脂肪烃和芳烃的析出行为。根据煤样大分子结构中化学键的断裂和气态挥发物的逸出规律，提出了煤热解过程中可能进行的反应路线。

关键词: 煤, 热解, 流化床, 显微组分, 计算机模拟

Abstract:

The Ordos lignite was separated into vitrinite-rich group (EL-V) and inertinite-rich group (EL-I) by floating-sinking separation method, and the structures and compositions of the raw coal and its maceral were analyzed by industrial analysis, elemental analysis, X-ray diffraction spectroscopy (XRD), Fourier transform infrared spectroscopy (FTIR) and solid state nuclear magnetic resonance (¹³C NMR). The pyrolysis characteristics and the escape pattern of gaseous volatiles of the raw coal and its maceral were investigated by powder-particle fluidized bed and TG-FTIR devices, respectively, to further construct the macromolecular structure models of the raw coal and its maceral and quantum chemical calculations were carried out to recognize the law of chemical bonds breaking. The results showed that the vitrinite-rich group had a higher content of volatiles, contained abundant alkyl side chains, and the largest heat weight loss rate, suggesting that the vitrinite-rich group was more reactive in pyrolysis. Compared with the raw coal and inertinite-rich group, the vitrinite-rich group had higher the pyrolysis gas content and tar contend, and its pyrolysis tar contained more aliphatic hydrocarbons and light aromatic hydrocarbons (TXE). The inertinite-rich group had lower H/C ratio, and higher oxygen content and aromatic ring condensation, and its pyrolysis tar contained higher PAHs and phenolics. In addition, the precipitation behaviors of CO₂, CO, CH₄, aliphatic hydrocarbons and aromatic hydrocarbons were analyzed by TG-FTIR. Based on the breaking of chemical bonds in the macromolecular structure of coal samples and the escape pattern of gaseous volatiles, the possible reaction routes carried out in the coal pyrolysis process were proposed.

Key words: coal, pyrolysis, fluidized bed, macerals, computer simulation

中图分类号:

TQ53

吴琪, 白柏杨, 尹永杰, 马晓迅. 鄂尔多斯褐煤显微组分结构与其热解特性间的关系[J]. 化工进展, 2024, 43(5): 2370-2385.

WU Qi, BAI Boyang, YIN Yongjie, MA Xiaoxun. Relationship between the structure of macerals of Ordos lignite and its pyrolysis characteristics[J]. Chemical Industry and Engineering Progress, 2024, 43(5): 2370-2385.

图/表 22

表1 EL的工业分析和岩相分析

工业分析（干燥无灰基）

/%（质量分数）

图1 粉-粒流化床快速热解装置1—气体质量流量计；2—转子流量计；3—压力表；4—粉煤进料装置；5—温控仪；6—热解炉；7—粉-粒流化床；8—保温箱；9—过滤器；10—旋风分离器；11—半焦收集装置；12—冷凝吸收装置；13—湿式流量计；14—气相色谱仪；15—热解焦油检测仪

表2 原煤及显微组分的工业分析和元素分析

样品	工业分析（干燥无灰基）/%（质量分数）				元素分析（干燥无灰基）/%（质量分数）					原子比
样品	水分	灰分	挥发分	固定碳^①	C	H	N	S	O^①	A_O/C	A_H/C
EL	1.49	7.95	37.27	62.73	70.60	4.19	1.43	0.10	23.69	0.25	0.71
EL-V	2.47	2.11	38.62	61.38	73.77	5.01	1.55	0.15	19.52	0.20	0.81
EL-I	0.78	17.77	31.68	68.32	64.04	3.52	1.22	0.16	31.06	0.36	0.66

图2 原煤及显微组分的XRD谱图及原煤的曲线拟合谱图Q—石英；C—方解石；K—高岭石；N—钠长石

表3 原煤及显微组分的碳微晶结构参数

样品	2θ/(°)	d₀₀₂/nm	L_c/nm	L_a/nm	f_a
EL	25.80	0.3452	1.21	1.36	0.60
EL-V	25.23	0.3528	1.55	0.98	0.51
EL-I	25.81	0.3450	1.67	1.04	0.63

图3 原煤及显微组分的FTIR光谱及拟合曲线

表4 原煤及显微组分的结构参数

样品	COOH/C_Ar	R—O—R/C_Ar	Ar—OH/C_Ar	CH₂/CH₃
EL	0.16	0.93	0.29	2.70
EL-V	0.20	1.01	0.17	3.63
EL-I	0.22	1.21	0.41	2.59

图4 原煤及显微组分煤样固体核磁共振谱图及拟合曲线

表5 核磁共振中碳原子化学位移归属

化学位移	归属	化学位移	归属
0~17	脂甲基R—CH₃	60~90	环内氧接脂碳
17~22	芳甲基Ar—CH₃	90~126	质子化碳
22~35	亚甲基—CH₂	126~137	桥接芳碳
35~40	次亚甲基—CH	137~148	侧支芳碳
40~50	季碳	148~165	氧取代芳碳
50~60	甲氧基	165~250	羧基（羰基碳）

表6 原煤及显微组分的碳结构参数

样品	ƒ_a	ƒ_Al	ƒ $a C$	ƒ $a'$	ƒ $a H$	ƒ $a N$	ƒ $a P$	ƒ $a S$	ƒ $a B$	ƒ $A l *$	ƒ $A l H$	ƒ $A l O$
EL	74.68	25.32	5.35	69.34	46.66	22.68	6.68	5.61	10.39	7.43	17.21	0.67
EL-V	69.10	30.90	5.21	63.88	41.64	22.25	6.40	5.88	9.96	10.23	18.59	2.08
EL-I	75.56	24.44	9.03	66.52	44.52	22.00	6.01	4.65	11.34	11.84	12.60	0.00

表6 原煤及显微组分的碳结构参数

样品	ƒ_a	ƒ_Al	ƒ $a C$	ƒ $a'$	ƒ $a H$	ƒ $a N$	ƒ $a P$	ƒ $a S$	ƒ $a B$	ƒ $A l *$	ƒ $A l H$	ƒ $A l O$
EL	74.68	25.32	5.35	69.34	46.66	22.68	6.68	5.61	10.39	7.43	17.21	0.67
EL-V	69.10	30.90	5.21	63.88	41.64	22.25	6.40	5.88	9.96	10.23	18.59	2.08
EL-I	75.56	24.44	9.03	66.52	44.52	22.00	6.01	4.65	11.34	11.84	12.60	0.00

图5 原煤及显微组分的热失重和失重速率曲线

表7 原煤及显微组分的TG和DTG相关数据

样品	质量损失范围（daf）/%	净失重损失质量（daf）/%	最大热失重峰温度/℃	最大热失重速率/%·min^-1
EL	98.42~72.22	26.21	448.7	-1.02
EL-V	99.21~66.32	32.89	444.1	-1.85
EL-I	98.27~75.56	22.70	452.4	-0.76

图6 原煤及显微组分热解过程中3D红外谱图

图7 原煤及显微组分热解过程中挥发性气体组分的红外光谱分析

图8 原煤及显微组分煤样的热解产物分布

图9 原煤及显微组分煤样的热解焦油分析

图10 原煤及显微组分煤样的热解焦油中轻质芳烃和芳烃化合物分析

图11 原煤及显微组分煤样热解气体组成

图12 原煤及显微组分的模拟13C NMR谱图及大分子平面结构模型

图13 原煤及显微组分的三维大分子结构模型（左侧为主视图，右侧为左视图）

表8 原煤及显微组分煤样大分子结构模型参数

样品	分子式	总能量/kcal·mol^-1	元素含量/%				分子量
样品	分子式	总能量/kcal·mol^-1	C	H	O	N	分子量
EL	C₁₄₂H₁₁₂N₂O₃₅	448.37	70.87	4.69	23.27	1.16	2404
EL-V	C₁₄₇H₁₁₆N₂O₃₀	459.48	73.86	4.89	20.08	1.17	2388
EL-I	C₁₄₈H₁₀₀N₂O₅₀	446.52	65.68	3.72	29.56	1.04	2704

图14 褐煤及显微组分[富镜质组（EL-V）和富惰质组（EL-I）]热解过程的路线图a—气体的解吸与蒸发；b—脱烷基反应；c—脱氧反应；d—脱氢（芳构化）反应

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鄂尔多斯褐煤显微组分结构与其热解特性间的关系

Relationship between the structure of macerals of Ordos lignite and its pyrolysis characteristics

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