淖毛湖煤慢速热解过程官能团相互作用

doi:10.11949/0438-1157.20211530

摘要/Abstract

摘要：

采用滴管炉，在短停留时间下，制备具有一定低温反应活性而消除主要低温交联位点的淖毛湖煤（NMHcoal）快速热解半焦（NRPchar），再将NMHcoal和NRPchar混合进行慢速热解，研究官能团间的相互作用。热重分析结果表明，NMHcoal/NRPchar混合比为5∶5，温度为500℃热解时具有较强的负协同作用。固定床热解结果表明，NMHcoal热解生成的挥发物部分扩散至NRPchar中，?CH₃与芳碳自由基以及?O有更多的结合概率与时间，使焦油中含甲基的萘、酚类增多，半焦中烷基化邻氧芳碳结构与醚类结构增加。析出的酚类增多，使半焦中连氧芳碳结构减少。NRPchar中生成较多的多环芳烃前体，它们与酚类物质发生反应生成多环芳烃和CO，使共热解焦油中5、6环化合物含量增加，而另一部分滞留在半焦中使其比表面积降低。

关键词: 热解, 自由基, 固定床, 半焦, 官能团, 相互作用

Abstract:

To study the interaction between functional groups during slow pyrolysis of coal, Naomaohu coal (NMHcoal) sample was pyrolyzed in a drop tube furnace reactor with a short residence time to prepare rapid pyrolysis char (NRPchar) with part remained reactivity of coal but most of the low-temperature crosslinking site precursor eliminated. TG results indicated that the pyrolysis of NMHcoal/NRPchar with a ratio of 5∶5 at 500℃ shows a strong negative synergy. The fixed bed pyrolysis results show that some volatiles generated by the pyrolysis of NMHcoal diffused into the NRPchar, which provided more probability and time to the combination of ?CH₃ with aromatic carbon radicals and ?O. As a result, the structure of naphthalenes and phenols containing methyl groups in tar, and also the alkylated oxyaromatic carbon structure and ether structure in the char increased. The increased release of phenols reduced the oxyaromatic carbon structure in the char. More polycyclic aromatic hydrocarbon precursors are generated in NRPchar, they react with phenolic substances to generate polycyclic aromatic hydrocarbons and CO, which increase the content of 5 and 6 ring compounds in the co-pyrolysis tar, while the other part is retained in the semi-coke to reduce its specific surface area.

Key words: pyrolysis, free radical, fixed bed, char, functional group, interaction

中图分类号:

TQ 530.2

杨英杰, 杨赫, 朱家龙, 郭双淇, 尚妍, 李扬, 靳立军, 胡浩权. 淖毛湖煤慢速热解过程官能团相互作用[J]. 化工学报, 2022, 73(2): 865-875.

Yingjie YANG, He YANG, Jialong ZHU, Shuangqi GUO, Yan SHANG, Yang LI, Lijun JIN, Haoquan HU. Interaction between functional groups during slow pyrolysis of Naomaohu coal[J]. CIESC Journal, 2022, 73(2): 865-875.

图/表 17

图1 滴管炉实验系统装置图

Fig.1 Schematic diagram of drop tube furnace experimental system

表1 NMHcoal和NRPchar的工业与元素分析

Table 1 Proximate and ultimate analyses of NMHcoal and NRPchar

样品	工业分析/%(质量)			元素分析/%(质量，daf)
样品	M_ad	A_d	V_daf	C	H	N	O	S
NMHcoal	3.37	5.29	54.83	71.64	6.01	0.85	21.08	0.42
NRPchar	2.43	10.36	14.37	90.19	1.46	2.25	5.33	0.77

图2 固定床热解装置示意图

Fig.2 Schematic diagram of the fixed-bed equipment for coal pyrolysis

图3 NMHcoal和NRPchar的红外谱图

Fig.3 FT-IR spectra of NMHcoal and NRPchar

图4 NMHcoal和NRPchar在2800~3000 cm-1的拟合曲线

Fig.4 Fitting curves of NMHcoal and NRPchar in 2800—3000 cm-1

表2 NMHcoal和NRPchar 2800~3000 cm-1拟合结果

Table 2 Fitting results of NMHcoal and NRPchar in 2800—3000 cm-1

峰位置/cm^-1	峰归属	峰面积的比例
峰位置/cm^-1	峰归属	NMHcoal	NRPchar
2825	O—CH₃	3.20	3.39
2851、2920	sym.R₂CH₂、asym.R₂CH₂	61.60	54.97
2874、2953	sym.RCH₃、asym.RCH₃	24.69	22.94
2893	R₃CH	10.51	18.69

图5 NMHcoal、NRPchar及NMHcoal/NRPchar共热解的TG/DTG曲线E—实验值;C—加权平均值

Fig.5 TG/DTG curves of NMHcoal /NRPchar co-pyrolysis

表3 NMHcoal、NRPchar及NMHcoal/NRPchar共热解的特征参数

Table 3 Characteristic parameters of NMHcoal， NRPchar and NMHcoal/NRPchar pyrolysis

样品	初温/ ℃	峰温/ ℃	终温/ ℃	失重量/%		DTG_max/(%/℃)
样品	初温/ ℃	峰温/ ℃	终温/ ℃	实验值	加权平均值	实验值	加权平均值
NMHcoal	201	443	636	47.3	—	-0.215	—
NRPchar	368	—	—	22.3	—	-0.058	—
20% char	197	443	637	41.8	42.3	-0.166	-0.175
40% char	203	443	625	34.8	37.3	-0.134	-0.134
50% char	209	442	625	32.7	34.8	-0.101	-0.114
60% char	203	443	608	29.5	32.3	-0.097	-0.094
80% char	207	443	583	24.6	27.3	-0.055	-0.054

图6 NMHcoal/NRPchar（5∶5）在不同温度下的红外谱图

Fig.6 FT-IR spectra of NMHcoal/NRPchar(5∶5) at different temperature

表4 NMHcoal、NRPchar及其混合物在500℃热解得到的焦油样品中检测到的主要单环、多环芳烃和长链脂肪烃

Table 4 Main single-ring， polycyclic aromatic compounds and long-chain aliphatic hydrocarbons detected in tar samples obtained from pyrolysis of NMHcoal， NRPchar and their mixtures at 500℃

序号	化合物	NMHcoal-fb	NMHcoal/NRPchar-fb	NRPchar-fb
1环芳香化合物
1	甲苯	0.806	0.243	0.732
2	乙苯	0.366	0.206	0.058
3	对二甲苯	1.400	0.594	0.409
4	1,2,3-三甲苯	1.362	1.194	—
5	苯酚	6.274	5.582	1.548
6	2-甲基苯酚	9.222	8.639	0.916
7	2,6-二甲基苯酚	10.04	6.08	—
8	2-乙基苯酚	0.475	1.709	—
9	3-甲基-1,2-苯二酚	0.715	2.765	—
10	2,3,6-三甲基苯酚	0.371	0.840	—
11	4,5-二甲基-1,3-苯二酚	0.445	0.594	—
12	4-乙基-1,3-苯二酚	0.431	0.814	—
2环芳香化合物
13	茚	0.437	0.280	0.061
14	萘	1.238	1.647	66.852
15	4,7-二甲基苯并呋喃	0.317	0.230	—
16	1,3-二甲基-1-氢茚	0.85	1.006	—
17	2,3-二氢化-5-羟基茚	0.744	1.236	—
18	2-甲基萘	3.377	2.912	—
19	2,6-二甲基萘	3.117	2.844	—
20	1,4,6-三甲基萘	3.266	4.052	—
21	2-甲基-1-萘酚	3.388	3.994	—
3环以上芳香化合物
22	1-甲基-9H-笏	0.268	0.874	—
23	菲	—	1.132	5.773
24	3,6-二甲基菲	0.187	—	—
25	2,3,5-三甲基菲	—	0.131	—
26	芘		0.974	4.428
27	荧蒽	—	—	5.437
28	苯并芘	—	0.340	1.080
29	苯并荧蒽	—	1.692	—
30	苝	0.166	0.405	—
31	苯并苝	—	0.548	0.117
长链脂肪烃化合物
32	十一烷	0.741	0.552	—
33	十二烷	0.958	1.567	—
34	十四烷	1.058	1.383	—
35	十五烷	1.009	1.165	—
36	十七烷	1.004	1.100	—
37	十八烷	0.945	0.947	—
38	十九烷	0.873	0.962	—
39	二十烷	0.909	1.025	—
40	二十一烷	1.005	1.154	—
41	二十二烷	1.110	1.170	—
42	二十三烷	1.357	1.445	—
43	二十四烷	1.170	1.035	—
44	二十五烷	1.019	2.473	—

图7 NMHcoal-fb、NRPchar-fb及NMHcoal/NRPchar（5∶5）-fb热解气体产率

Fig.7 Gas production during pyrolysis of NMHcoal-fb, NRPchar-fb and NMHcoal/NRPchar (5∶5) -fb

图8 单环、多环芳香族化合物和长链脂肪烃在500℃下的协同效应(x轴上的数字1~44对应于表4中的化合物)

Fig.8 Synergetic effects from single-ring, polycyclic aromatic compounds and long-chain aliphatic hydrocarbons obtained from NMHcoal/NRPchar (5∶5)at 500℃ (The numbers 1—44 on x-axis correspond to the compounds in Table 4)

图9 半焦的N2吸/脱附曲线（a）和孔径分布（b）

Fig.9 N2 adsorption/desorption isotherms (a) and pore size distributions (b) of char

表5 半焦的比表面积及孔隙结构参数

Table 5 Specific surface area and pore structure parameters of char

样品	比表面积/ (m²/g)	孔容/ (cm³/g)	孔径/nm
NMHcoal-fb	10.7	0.016	5.44
NRPchar-fb	285.9	0.171	4.27
NMHcoal/NRPchar-fb（实验值）	105.0	0.088	4.23
NMHcoal/NRPchar -fb（加权平均值）	148.3	0.093	4.86

图10 NMHcoal、NRPchar及其混合物在固定床500℃热解的半焦FT-IR谱图

Fig.10 FT-IR spectra of NMHcoal, NRPchar and their blends in fixed bed at 500℃

图11 NMHcoal-fb和NMHcoal /NRPchar(5∶5)-fb半焦的13C NMR光谱及其拟合曲线

Fig.11 13C NMR spectra and their fitting curves for NMHcoal-fb and NMHcoal /NRPchar(5∶5)-fb

表6 NMHcoal-fb和NMHcoal /NRPchar（5∶5）-fb半焦的碳分布

Table 6 Distribution of carbon types in NMHcoal-fb and NMHcoal /NRPchar（5∶5）-fb

峰	碳类型	符号	峰化学位移		摩尔分取/%
峰	碳类型	符号	NMHcoal-fb	NMHcoal/NRPchar-fb	NMHcoal-fb	NMHcoal/NRPchar-fb
脂肪碳
1	脂肪甲基	$f a l M$	12.2	11.0	1.64	0.74
2	芳环甲基	$f a l A$	20.2	20.3	3.13	1.24
3	亚甲基	$f a l H$	30.2	29.2	1.36	0.99
4	次甲基	$f a l D$	36.8	36.1	1.88	1.67
5	季碳	$f a l D$	45.5	45.9	2.23	2.81
6	连氧脂肪碳	$f a l O$	55.5 67.6 86.0	55.0 66.7 88.0	15.12	16.98
总					25.36	24.43
芳碳
7	质子化邻氧芳碳	$f a O 1$	108.9	108	5.49	5.96
8	烷基化邻氧芳碳	$f a O 2$	116.1	116.8	4.78	7.64
9	质子化芳碳	$f a H$	122	122.3	7.13	7.86
10	桥头芳碳	$f a B$	129	128.6	23.61	24.29
11	烷基取代芳碳	$f a S$	138.9 147.1	138.8 147.8	13.13	11.06
12	连氧芳碳	$f a O 3$	155 165	155 165	6.51	4.45
总					60.65	61.26
羰基
13	羧基、酯的羰基碳	$f a C 1$	178.5	176.3	1.55	1.02
14	酮、醛的碳	$f a C 2$	199.3	197.3	12.41	13.27
总					13.96	14.29

表6 NMHcoal-fb和NMHcoal /NRPchar（5∶5）-fb半焦的碳分布

Table 6 Distribution of carbon types in NMHcoal-fb and NMHcoal /NRPchar（5∶5）-fb

峰	碳类型	符号	峰化学位移		摩尔分取/%
峰	碳类型	符号	NMHcoal-fb	NMHcoal/NRPchar-fb	NMHcoal-fb	NMHcoal/NRPchar-fb
脂肪碳
1	脂肪甲基	$f a l M$	12.2	11.0	1.64	0.74
2	芳环甲基	$f a l A$	20.2	20.3	3.13	1.24
3	亚甲基	$f a l H$	30.2	29.2	1.36	0.99
4	次甲基	$f a l D$	36.8	36.1	1.88	1.67
5	季碳	$f a l D$	45.5	45.9	2.23	2.81
6	连氧脂肪碳	$f a l O$	55.5 67.6 86.0	55.0 66.7 88.0	15.12	16.98
总					25.36	24.43
芳碳
7	质子化邻氧芳碳	$f a O 1$	108.9	108	5.49	5.96
8	烷基化邻氧芳碳	$f a O 2$	116.1	116.8	4.78	7.64
9	质子化芳碳	$f a H$	122	122.3	7.13	7.86
10	桥头芳碳	$f a B$	129	128.6	23.61	24.29
11	烷基取代芳碳	$f a S$	138.9 147.1	138.8 147.8	13.13	11.06
12	连氧芳碳	$f a O 3$	155 165	155 165	6.51	4.45
总					60.65	61.26
羰基
13	羧基、酯的羰基碳	$f a C 1$	178.5	176.3	1.55	1.02
14	酮、醛的碳	$f a C 2$	199.3	197.3	12.41	13.27
总					13.96	14.29

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