• 论文
主办单位:煤炭科学研究总院有限公司、中国煤炭学会学术期刊工作委员会
中温煤焦油沥青逐级萃取的产物组成与结构分析
  • Title

    Composition and structure analysis of products from the sequential ex-traction process of medium temperature coal tar pitch

  • 作者

    崔瀛丹 钟梅 哈丽丹·买买提 杨超 樊星

  • Author

    CUI Yingdan,ZHONG Mei,HALIDAN Maimaiti,YANG Chao,FAN Xing

  • 单位

    新疆大学化工学院,新疆大学新疆煤炭清洁转化与化工过程新疆维吾尔自治区重点实验室

  • Organization
    School of Chemical Engineering and Technology,Xinjiang University,Key Laboratory of Coal Cleaning Conversion and Chemical Engineering Process in Xinjiang Uyghur Autonomous Region,Xinjiang University
  • 摘要

    以中温煤沥青为原料,根据Hansen溶解度参数软件(HSPiP)的计算结果,选择无水乙醇、正戊烷、异丙醇、甲苯、四氢呋喃和N-甲基吡咯烷酮为萃取剂对沥青进行逐级索氏抽提,以解析其结构与组成。高分辨质谱分析结果表明各级萃取物中含有3 000多种化合物,分子量集中在100~400 u,CH类化合物的含量高达60%,相对含量较高的20种化合物中芳香杂环为9种,以含氧化合物为主,Nn类化合物的相对含量为4.3%~12.9%,主要是吡啶型和吡咯型氮化物;ONS类化合物的相对含量之和为10.1%~12.0%。各级萃取物的不饱和度双键当量(DBE)值主要分布在15~19,碳数为21~28。对萃余物进行XPS、红外、热重、13C NMR和晶相分析,结果表明C主要以芳碳形式存在,比例高于80%;相较于吡啶氮,吡咯氮更易被溶剂萃取,致使其相对含量随萃取级数增加而下降;S则主要以噻吩硫形式存在。13C NMR分析显示沥青及各级萃余物中表征平均芳环尺寸大小的Xb约为0.7,意味着其平均芳环数约为5;芳桥碳含量fBa超过65%,说明各级萃余物中芳碳缩合度较高。随着萃取级数的增加,各物质中弱键和侧链等基团逐渐减少,分子量增加和芳环缩合度增加,热稳定性增强,各物质的饱和链间距和芳香片层间距逐渐减小,芳香层片间的直径、堆砌高度及芳香片层数逐渐增加。



  • Abstract

    According to the results of Hansen solubility parameter calculated by software HSPiP,anhydrous ethanol,npentane,isopropanol,toluene,the tetrahydrofuran and Nmethylpyrrolidone were selected as extractants for medium temperature coal tar pitch soxhlet extraction to analyze the composition and structure.The results of highresolutionmassspectrometry analysis show that more than 3 000 compounds are detected and the molecular weight is in the range of 100 to 400,wherein,the content of compounds containing carbon and hydrogen is up to 60%.It can be observed that the relative content of 20 compounds is higher,among which 9 compounds mainly contain heteroatoms and oxygen.In addition,the content of Nn species,consisting by pyridine and pyrrole,is 4.3%-12.9%,while it is 10.1%-12.0% for ONS compounds.The unsaturation double bond equivalent (DBE) values of the extracts range from 15 to 19,and the carbon number is between 21 and 28.Meanwhile,the residues were characterized by XPS,FTIR,TG-DTG and 13C NMR.The XPS results show that the aromatic carbon is the major form of carbon and its content is up to 80%.For nitrogen element,it exists in pyridine and pyrrole,and the latter is more easily to be extracted by solvent,thus leading to the gradual decrease of relative content with the raising extraction series.The thiophene is the main form of sulfur.According to the analysis of 13C NMR,the Xb of coal tar pitch and all residues is 0.7,indicating that the average number of aromatic rings is about 5.It is noted that the content of aromatic bridge carbon faB is 65%,suggesting the highly condensed aromatic structure.As the extraction proceeds,the weak bonds and side chain groups in the residues gradually decrease,while the condensation of aromatics and molecular weight increases,resulting in an enhancement of the thermal stability of the samples.Correspondingly,saturated chain and aromatic sheet spacing in residues gradually reduce,however,the diameter,stacking height and number of aromatic lamellar present an increase tendency


  • 关键词

    ​煤焦油沥青逐级萃取萃取物萃余物结构分析

  • KeyWords

    coal tar pitch,sequential extraction,extract,reusidue;structure analysis

  • 基金项目(Foundation)
    国家重点研发计划资助项目(2016YFF0102602); 国家自然科学基金资助项目(21766035)
  • 文章目录

    1 实验部分

        1.1 原料

        1.2 实验过程

    2 结果与讨论

        2.1 萃取剂选择

        2.2 萃取物与萃余物结构分析

    3 结论

  • 引用格式
    崔瀛丹,钟梅,哈丽丹·买买提,等. 中温煤焦油沥青逐级萃取的产物组成与结构分析[J]. 煤炭学报,2020,45
    (11):3930-3939.
  • Citation
    CUI Yingdan,ZHONG Mei,HALIDAN Maimaiti,et al. Composition and structure analysis of products from the sequential
    extraction process of medium temperature coal tar pitch[J]. Journal of China Coal Society,2020,45(11):3930-
    3939.
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