波谱学杂志 ›› 2006, Vol. 23 ›› Issue (1): 41-47.

• 研究论文 • 上一篇    下一篇

   煤直接液化中油煤浆热溶产物的 13C NMR 研究

  

  1. 华东理工大学  分析测试中心, 上海  200237
  • 收稿日期:2005-03-07 修回日期:2005-09-30 出版日期:2006-03-05 发布日期:2006-03-05
  • 基金资助:

    “973”资助项目(2004CB217601)与国家自然科学基金资助项目(20476029).

Thermally Dissolved Products of Coal-oil Slurry During Direct Coal Liquefaction Studied by NMR Spectroscopy

  1. Analysis and Research Center, East China University of Science and Technology, Shanghai 200237
  • Received:2005-03-07 Revised:2005-09-30 Online:2006-03-05 Published:2006-03-05

摘要:

研究油煤浆热溶产物的成分及含量的变化是控制煤直接液化工艺的重要因素之一. 本文采用固体核磁共振研究了在高压釜中用不同溶剂在不同温度下(250~370 ℃)得到的神华煤及其热溶产物的一些变化规律. 通过对神华煤及其热溶中间产物与抽余煤的13C CP/MAS/TOSS NMR分析可知, 神华煤经热溶处理后, 脱除了一些含氧官能团以及某些脂肪烃结构. 同时, 一些芳香桥碳分子和被取代的芳香碳环发生了断裂, 随着反应温度逐渐升高, 由于不断供氢, 四氢呋喃抽提物的芳香度逐渐降低, 抽提率逐渐增大. 

关键词: 固体核磁共振, 13C CP/MAS/TOSS NMR, 热溶产物, 前沥青烯, 芳香度

Abstract:

Studying the composition of product of thermally dissolved coaloil slurry can provide important information on how to control direct coal liquefaction. In this study, Shenhua coal was thermally dissolved in an autoclave using different solvents at different temperatures (250~370 ℃). Solid state 13C CP/MAS/TOSS NMR spectroscopy was used to analyze Shenhua coal, its thermally dissolved products and extracted residue. The results showed that thermal extraction removed oxygen-containing functional groups and some aliphatic hydrocarbon in the Shenhua coal, and fractured a fraction of aromatic bridgehead carbons and nonprotonated carbons. Increasing reaction temperature and continuous supply of hydrogen decreased the aromaticity of the THF extract, but increased the extraction yield.

Key words: solid state NMR, 13C CP/MAS/TOSS NMR, thermally dissolved products, preasphaltene, aromaticity

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