白音华褐煤可溶有机质的组成和结构特征

杜姣姣; 赵云鹏; 田由甲; 张迪

白音华褐煤可溶有机质的组成和结构特征

杜姣姣¹,
赵云鹏^{1, 2, ,},
田由甲¹,
张迪¹

1.
中国矿业大学煤炭加工与高效利用教育部重点实验室, 江苏徐州 221116
2.
太原理工大学煤科学与技术省部共建国家重点实验室培育基地, 山西太原 030024

基金项目:

国家自然科学基金 21206188

中央高校基本科研业务费 China University of Mining and Technology, 2015QNA25

煤科学与技术省部共建国家重点实验室培育基地开放课题 MKX201502

详细信息

通讯作者:
赵云鹏, E-mail:yunpengzhao2009@163.com

中图分类号: TQ530
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- 被引次数: 0
出版历程
- 收稿日期: 2016-09-14
- 修回日期: 2016-11-06
- 网络出版日期: 2021-01-23
- 刊出日期: 2017-01-10

Composition and structural characteristics of soluble organic species in Baiyinhua lignite

1.
Key Laboratory of Coal Processing and Efficient Utilization, Ministry of Education, China University of Mining & Technology, Xuzhou 221116, China
2.
State Key Laboratory Breeding Base of Coal Science and Technology Co-founded by Shanxi Province and Ministry Education, Taiyuan University of Technology, Taiyuan 030024, China

Funds:

the National Natural Science Foundation of China 21206188

Fundamental Research Funds for the Central Universities China University of Mining and Technology, 2015QNA25

Open Foundation from State Key Laboratory Breeding Base of Coal Science and Technology Co-founded by Shanxi Province and Ministry Education MKX201502

摘要

摘要: 依次采用石油醚、环己烷、二硫化碳、丙酮、甲醇和等体积的丙酮/二硫化碳混合溶剂对白音华褐煤（BL）进行分级萃取得到萃取物（E₁-E₆），利用甲醇、甲苯和等体积的甲醇/甲苯混合溶剂对萃取残渣进行连续热溶得到热溶物（SP₁-SP₃）。利用傅里叶变换红外光谱（FT-IR）、气相色谱质谱（GC/MS）和实时直接分析-质谱（DART-MS）对萃取物和热溶物的组成和结构特征进行了分析。BL总的萃取物产率和热溶物产率分别为9.37%和21.84%。E₅和E₆的FT-IR谱图中有较强的羟基吸收峰，而E₁的FT-IR谱图中脂肪C-H的伸缩振动峰强度明显高于其他萃取物；三种溶剂热溶物的FT-IR谱图相似，但SP₁和SP₃的FT-IR谱图中羟基吸收峰较强。E₁和E₅中GC/MS可检测化合物分别以烷烃和芳烃为主，E₅中还含有较多的含氧化合物；三种热溶物中化合物均以烷烃和芳烃为主，SP₃中酚类、酮类和酯类等含氧化合物的含量较高。DART-MS可检测出萃取物和热溶物中GC/MS无法检测出的较强极性和难挥发化合物；热溶物中含量较高的化合物的碳数和等价双键数（Double bond equivalent，DBE）分别集中分布在10-25和2-16，并且DBE随碳数增加而增加。
- 褐煤 /
- 分级萃取 /
- 连续热溶 /
- 气相色谱/质谱 /
- 实时直接分析质谱
Abstract: Baiyinhua lignite was sequentially extracted with petroleum ether, cyclohexane, carbon disulfide, acetone, methanol and isometric acetone/carbon disulfide mixed solvent affording extracts, i.e. E₁-E₆, then extraction residue was sequentially thermal dissolved using methanol, toluene and isomeric methanol/toluene mixed solvent affording soluble portions (SPs), i.e.SP₁-SP₃. The composition and structural characteristics of extracts and SPs were characterized with Fourier transform infrared (FT-IR) spectroscopy, gas chromatography/mass spectrometer (GC/MS), direct analyze in real time mass spectrometer (DART-MS). The total extracts yield and SPs yield of BL are 9.37% and 21.84%, respectively. There exist strong adsorption peaks ascribed to hydroxyl in the FT-IR spectra of E₁ and E₆, while the intensity of adsorption peaks ascribed to aliphatic C-H in the FT-IR spectrum of E₁ is obviously higher than that of other extracts. There are similar FT-IR spectra among those 3 SPs, whereas the intensity of adsorption peak originated from hydroxyl in the FT-IR spectra of SP₁ and SP₃ is higher than those of SP₂. The compounds GC/MS detected in E₁ and E₅ are dominated with alkanes and arenes, respectively, and the content of oxygen-containing compounds (OCCs) in E₅ are more than that in E₁. The compounds in the 3 SPs are composed of alkanes and arenes, while the contents of OCCs, such as phenols, ketones and esters, in SP₃ are higher than those in SP₁ and SP₂. Many compounds with high polarity and low volatility which could not identified by GC/MS were detected using DART-MS. The carbon number and double bond equivalent (DBE) of the compounds with high content in SPs mainly distribute in 10-25 and 2-16, respectively, and the DBE increases with carbon number increasing.
- lignite /
- solvent extraction /
- thermal dissolution /
- GC/MS /
- DART-MS

HTML全文

图 1 BL分级萃取实验流程示意图

Figure 1 Fractional extraction procedure of BL

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图 2 R_E连续热溶实验流程示意图

Figure 2 Sequential thermal dissolution procedure of R_E

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图 3 萃取物的红外光谱谱图

Figure 3 FT-IR spectra of extacts

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图 4 热溶物的红外光谱谱图

Figure 4 FT-IR spectra of SPs

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图 5 E₁和E₅中GC/MS可检测物化合物分布

Figure 5 Distributions of group components in E₁ and E₅ identified by GC/MS

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图 6 热溶物中GC/MS可检测物化合物分布

Figure 6 Distributions of group components in SPs identified by GC/MS

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图 7 萃取物的DART-MS质谱图

Figure 7 DART-MS mass spectra of extracts

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图 8 热溶物的DART-MS质谱图

Figure 8 DART-MS mass spectra of SPs

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图 9 热溶物中DART-MS可检测化合物的DBE与碳数目气泡图

Figure 9 Iso-abundance plots of DBE versus carbon numbers for the compounds in SPs identified by DART-MS analysis

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表 1 白音华褐煤的工业分析和元素分析

Table 1 Proximate and ultimate analyses of BL

Proximate analysis w/%			Ultimate analysis w_daf/%
M_ad	A_d	V_daf	C	H	N	S	O^a
20.40	7.55	41.64	59.94	5.24	1.82	2.27	30.73
^a：by difference

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表 2 白音华褐煤的萃取物和热溶物产率

Table 2 Yields of extracts and SPs of BL

Extract	Yield w_daf/%	SP	Yield w_daf/%
E₁	0.81	SP₁	9.29
E₂	0.09	SP₂	6.62
E₃	0.19	SP₃	5.93
E₄	0.73
E₅	7.02
E₆	0.53
Total	9.37	total	21.84

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