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Solvent degradation during coal liquefaction in a flowing-solvent reactor

机译:流动溶剂反应器中煤液化过程中的溶剂降解

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We have previously observed that primary coal extracts recovered from the flowing solvent reactor appeared to be of large molecular mass. Short residence times in the reaction zone following the solubilisation of the extracts tended to limit their thermal degradation. This observation offered the vista of detailed characterisation and analysis of most (~ 80-90 percent) of the coal mass in solution-and in a state relatively free of thermal degradation. Point of Ayr coal was extracted with tetralin and with non-donor solvents, quinoline and NMP at 350 and 450 deg C. Structural evaluations have been carried out using size exclusion chromatography, UV-fluorescence spectrometry, GC-MS and probe-MS. Little coal derived material could be found in the pentane-soluble part of the reaction mixture; solvent dimers and trimers were prominent and coal-derived components, such as alkanes, were only minor components. In attempting to characterise the main, pentane-insoluble fraction of the coal extract, the level of interference from solvent-derived material emerged as the decisive parameter for the success or failure of the general method. However, the predominantly pentane-insoluble coal extracts from each solvent were contaminated by solvent polymerisation products. For all three solvents, the level of contamination of extracts with solvent derived material tended to interfere with the detailed characterisation/analysis of material extracted from the coal.
机译:我们先前已经观察到从流动溶剂反应器中回收的一次煤提取物似乎具有大分子量。提取物溶解后在反应区中的短停留时间倾向于限制其热降解。该观察结果提供了详细表征和分析溶液中大部分(约80-90%)煤块的状态,并且处于相对没有热降解的状态。用四氢化萘和非供体溶剂,喹啉和NMP在350和450摄氏度下萃取艾尔煤的煤油点。已使用尺寸排阻色谱,紫外荧光光谱,GC-MS和探针MS对结构进行了评估。在反应混合物的可溶于戊烷的部分中几乎找不到煤衍生的物质。溶剂二聚体和三聚体是主要成分,而煤衍生的成分(例如烷烃)只是次要成分。在试图表征煤提取物中戊烷不溶的主要部分时,来自溶剂的物质的干扰水平成为通用方法成功与否的决定性参数。然而,每种溶剂的主要不溶于戊烷的煤提取物均被溶剂聚合产物污染。对于所有三种溶剂,提取物被溶剂衍生的物质的污染程度往往会干扰从煤中提取的物质的详细表征/分析。

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