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CCl_4溶剂下CO_2超临界萃取枣庄煤的产物分析
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作者 鞠彩霞 李凤刚 +6 位作者 闫鹏 赵玉亮 孟宪鑫 张洪 魏贤勇 宗志敏 丛兴顺 《化学工程》 CAS CSCD 北大核心 2018年第6期6-10,共5页
在CCl_4夹带剂作用下CO_2超临界萃取枣庄煤,为煤超临界萃取产物的利用提供了的理论依据,同时对煤的成煤环境进行分析。萃取物中共检测出48种有机化合物。其中包括7种芳烃类(占35.382%)、9种酯类(占36.148%)、19种烷烃类(占14.410%)、1... 在CCl_4夹带剂作用下CO_2超临界萃取枣庄煤,为煤超临界萃取产物的利用提供了的理论依据,同时对煤的成煤环境进行分析。萃取物中共检测出48种有机化合物。其中包括7种芳烃类(占35.382%)、9种酯类(占36.148%)、19种烷烃类(占14.410%)、1种酸酐类(占0.376%)、1种脂肪酸类(占2.199%)、1种烯烃类(占0.382%)、1种酮类(占1.953%)和9种其他物质(占9.151%)。其中卤代烃(占3.007%),检测出一种环八硫(占1.397%)。检测出的正烷烃具有偶碳优势,从而可推测成煤环境多出现在碳酸盐岩和蒸发岩系中,盐湖或高含盐地层中。检测到生物标志物:2,6,10,14-四甲基十六烷(植烷)占1.028%。扫描电镜观察萃取前后的煤表面形貌变化,比表面测试表明萃余煤的比表面积和孔径分布变大,XRD显示出θ为29.5°时有机峰减弱至不明显。 展开更多
关键词 枣庄煤 CO2 超临界萃取 GC/MS/MS SEM 成煤环境
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褐煤中有机氮的赋存形态分布和分子结构特征
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作者 柳方景 别蕾蕾 +2 位作者 郭佳培 宗志敏 魏贤勇 《燃料化学学报》 EI CAS CSCD 北大核心 2020年第7期776-784,共9页
利用X射线光电子能谱(XPS)分析了先锋褐煤(XL)、小龙潭褐煤(XLT)和胜利褐煤(SL)及其萃取残渣表面有机氮的形态分布。结果表明,三种萃取残渣表面五种有机氮的含量分布各异,但均以吡咯型氮为主。考察了在300℃下Na OH催化的褐煤萃取残渣... 利用X射线光电子能谱(XPS)分析了先锋褐煤(XL)、小龙潭褐煤(XLT)和胜利褐煤(SL)及其萃取残渣表面有机氮的形态分布。结果表明,三种萃取残渣表面五种有机氮的含量分布各异,但均以吡咯型氮为主。考察了在300℃下Na OH催化的褐煤萃取残渣的超临界甲醇解反应,XL、XLT和SL萃取残渣超临界甲醇解所得石油醚可溶物的收率分别为46.0%、43.8%和47.6%(质量分数)。用傅里叶变换离子回旋共振质谱(FTICR/M S)分析石油醚可溶物中的含氮化合物(NCCs)。结果表明,NCCs主要包括N1、N1O1-N1O5、N2、N2O1-N2O4、N3O2和N5O2-N5O4类化合物。根据不饱和度和碳原子数的分布推测了NCCs的分子结构特征,表明绝大部分NCCs含羟基和羧基等含氧官能团,氮原子主要以吡咯、吡啶和氨基的形式存在于芳环结构中,以1-3个芳环的结构为主。褐煤中的-C-O-桥键的断裂是生成NCCs的一个重要路径。 展开更多
关键词 褐煤 有机氮 超临界甲醇解 傅里叶变换离子回旋共振质谱仪
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陕北中低温煤焦油中含氧有机化合物的质谱分析 被引量:2
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作者 郭宪厚 魏贤勇 +3 位作者 柳方景 宗志敏 樊星 郁章玉 《分析化学》 SCIE EI CAS CSCD 北大核心 2018年第11期1755-1762,共8页
中低温煤焦油中含氧有机化合物的含量较高,其中诸多含氧有机化合物是高附加值的有机化学品。本研究采用气相色谱/质谱联用仪(GC-MS)和负离子模式电喷雾傅里叶变换离子回旋共振质谱仪(NIESIFTICRMS)分析了陕北中低温煤焦油中的含氧有机... 中低温煤焦油中含氧有机化合物的含量较高,其中诸多含氧有机化合物是高附加值的有机化学品。本研究采用气相色谱/质谱联用仪(GC-MS)和负离子模式电喷雾傅里叶变换离子回旋共振质谱仪(NIESIFTICRMS)分析了陕北中低温煤焦油中的含氧有机化合物(OCOCs),旨在了解OCOCs的组成结构,为有效分离OCOCs提供科学依据。结果表明,用GC-MS检测到的OCOCs中,含1个氧原子(O_1,主要为芳酚)和2个氧原子(O_2)的化合物的相对含量分别为99.4%和0.6%;用NIESIFTICRMS检测到的OCOCs中碳原子数、氧原子数和芳环数范围分别为8~35、1~5和1~4,其中O_1和O_2占绝大多数;检测到的主要酸性OCOCs是苯酚、苯二酚和苯甲酸及其烷基取代物以及环烷和链烷酸,其中O_1的主要成分是1~4环的一元芳酚。GCMS与NIESIFTICRMS优势互补,是从分子水平上了解中低温煤焦油中OCOCs组成结构的有效工具。 展开更多
关键词 中低温煤焦油 含氧有机化合物 质谱分析
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Group separation and analysis of a carbon disulfide-soluble fraction from Shenfu coal by column chromatography 被引量:6
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作者 DING Ming-jie zong zhi-min +7 位作者 zong Ying OUYANG Xiao-dong HUANG Yao-guo ZHOU Lei ZHENG Yu-xuan ZHOU Xiao WEI Yan-bin WEI Xian-yong 《Journal of China University of Mining and Technology》 EI 2008年第1期27-32,共6页
A carbon disulfide-soluble fraction (CDSSF) from Shenfu coal was separated into five fractions by silica-gel column chromatography using hexane and n-hexane/ethyl acetate binary eluent. The five fractions include four... A carbon disulfide-soluble fraction (CDSSF) from Shenfu coal was separated into five fractions by silica-gel column chromatography using hexane and n-hexane/ethyl acetate binary eluent. The five fractions include four clear group fractions and a nonpolar fraction. All the fractions were analyzed by GC/MS. A total of 204 compounds were detected from the original CDSSF and its further separated fractions, with 173 compounds more than those detected by studying the original CDSSF directly. The results demonstrate a clear group separation by column chromatography in coal organic components and a more accessibility to coal components compared with the solvent extraction only. 展开更多
关键词 group separation column chromatography COAL
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Separation and analysis of aromatic hydrocarbons from two Chinese coals 被引量:3
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作者 DING Ming-jie LI Wen-dian +6 位作者 XIE Rui-lun zong Ying CAI Ke-ying PENG Yao-li zong zhi-min WIE Rui-lun WEI Xian-yong 《Journal of China University of Mining and Technology》 EI 2008年第3期432-436,共5页
Separation and analysis of aromatic hydrocarbons (AHs) from coals is of considerable significance for both fuel and non-fuel use of the coals. In present work two Chinese bituminous coals were selected for separation ... Separation and analysis of aromatic hydrocarbons (AHs) from coals is of considerable significance for both fuel and non-fuel use of the coals. In present work two Chinese bituminous coals were selected for separation of AHs by ultrasonic extrac-tion with CS2 followed by column chromatography using hexane as eluent. A series of AHs were separated from the two coals and analyzed by GC/MS. FTIR was employed to characterize the raw coals and the extracted residues. The results of GC/MS analysis show that the separated AHs are mono- to tetracyclic arenes, among which the principle AHs are alkyl naphthalenes and phenan-threnes. Obvious differences in the composition and the structure of AHs exist between the two coals, i.e., the AHs from Tongting coal tend to be higher rings compared to those from Pingshuo coal both from the variety and from the abundance of the AHs. FTIR analysis shows that the raw and extracted coals are similar in terms of functional groups, suggesting that the composition and structure of CS2 extract, especially the AHs, from coals can be used to interpret the coal structure to some extent. 展开更多
关键词 aromatic hydrocarbon column chromatography COAL GC-MS
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Reactivities of Shenfu Chars Toward Gasification with Carbon Dioxide 被引量:3
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作者 ZHANG Jia-wei zong zhi-min +7 位作者 WANG Tao-xia XIE Rui-lun DING Ming-jie CAI Ke-ying HUANG Yao-guo GAO Jin-sheng WU You-qing WEI Xian-yong 《Journal of China University of Mining and Technology》 EI 2007年第2期197-200,共4页
Five Shenfu char samples were prepared from Shenfu raw coal at different temperatures (950, 1100, 1200, 1300 and 1400℃) using a muffle furnace. Demineralization of the char samples was performed by treating them wi... Five Shenfu char samples were prepared from Shenfu raw coal at different temperatures (950, 1100, 1200, 1300 and 1400℃) using a muffle furnace. Demineralization of the char samples was performed by treating them with 10% nitric acid for 10 min in a CEM Discover microwave reactor. The gasification of the chars, and corresponding demineralized chars, in a carbon dioxide (CO2) atmosphere was conducted in a Netzsch STA 409Cl31F tempera- ture-programmed thermogravimetry apparatus. The effects of charring temperature and demineralization on the gasification reactivity of chars were systematically investigated. The results show that a char formed at a lower temperature is more reactive except for demineralized char formed at 1100℃, which is less reactive than char formed at 1200℃. Demineralization decreases the char reactivities toward gasification with CO2 to a small extent. 展开更多
关键词 DEMINERALIZATION temperature-programmed thermogravimetry reactivity
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Investigation on the structural feature of Shengli lignite 被引量:1
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作者 Zhang Yang-Yang zong zhi-min +4 位作者 Sun Yi-Bing Liu Fang-Jing Li Wei-Tu Wang Ya-Nan Wei Xian-Yong 《International Journal of Mining Science and Technology》 SCIE EI CSCD 2018年第2期335-342,共8页
The extraction residue from Shengli lignite was sequentially dissolved in cyclohexane, benzene, methanol, ethanol, and isopropanol in an autoclave at 320℃ to afford soluble portions(SPs) 1–5(SP_1-SP_5) and the final... The extraction residue from Shengli lignite was sequentially dissolved in cyclohexane, benzene, methanol, ethanol, and isopropanol in an autoclave at 320℃ to afford soluble portions(SPs) 1–5(SP_1-SP_5) and the final residue(FR). The total yield of SP_1-SP_5 is ca. 55.1%. The FR was subjected to ruthenium ioncatalyzed oxidation and the resulting products were isolated from the reaction mixture and esterified.Both the esterified products and SP_1-SP_5 were analyzed with a gas chromatograph/mass spectrometer.In total, 342 compounds were identified in SP_1-SP_5. They can be classified into normal alkanes, branched alkanes, alkenes, alkanedienes, arenes, alkanols, methylcycloalkanes, alkenols, alkylbenzenemethanols,arenols, anisol and substituted anisols, polymethyldihydrobenzofurans, arenofurans, dibenzofurans,ethoxymethylbenzenes, aldehydes, ketones, esters, nitrogen-containing organic compounds, sulfurcontaining organic compounds, and other compounds. Among the compounds, arenols are predominant in SP_1 and SP_2 and the main compounds in SP_3, while the main compounds in SP_4 and SP_5 are esters and arenes, respectively. According to the esterified products identified, the products from the FR oxidation can be grouped into non-benzene ring carboxylic acids(NBCAs) and benzenepolycarboxylic acids(BPCAs). The total yield of BPCAs is much higher than that of NBCAs, suggesting that the FR is rich in condensed aromatic moieties. 展开更多
关键词 LIGNITE Arenols ESTERS ARENES Condensed AROMATIC MOIETIES
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