胜利褐煤超临界乙醇脱氧实验研究

为有效脱除褐煤中含氧官能团,采用超临界乙醇工艺处理胜利褐煤,研究温度、停留时间和醇煤质量比对胜利褐煤脱氧效果的影响,并利用FT-IR和GC/MS对固液相产物进行表征。结果表明,胜利褐煤超临界乙醇脱氧的最佳工艺条件为:温度270℃,停留时间90 min,醇煤质量比5∶1,此时煤样总氧含量为9.29%,脱氧率为61.40%,固相产率为89.62%。在220℃得到的液相产物中,80%左右为芳香族类化合物,酚类和酯类含氧化合物体积分数低于5%,其他含氧类化合物11.29%。270℃得到的液相产率中芳香族类化合物体积分数降低31.69%,含氧类化合物体积分数增加2.81%,酚类和酯类含氧化合物增至35%左右。褐煤经超临界醇解后,乙醇与煤分子作用发生了醚氧桥键的断裂反应,煤分子发生了脱羧反应,液相产物中含有大量酚类(主要为苯酚及其取代物)和酯类(主要为乙酯类)。

Experimental study of supercritical ethanol deoxygenation of Shengli lignite

In order to remove the oxygen-containing functional groups in lignite,the Shengli lignite was treated through supercritical etha-nol process.The influence of the temperature,residence time and ratio of ethanol and coal on the deoxygenation was researched.The FT-IR and GC/ MS were used to characterize the solid and liquid products.The results showed that the optimal deoxygenation condition of super-critical ethanol deoxygenation was temperature 270 ℃ ,residence time 90 minutes and the mass ratio of alcohol to coal 5 ∶ 1,and the total oxygen content was 9.29%,the deoxygenation rate was 61.40%,the solid yield was 89.62%.In the liquid product which was obtained at 220 ℃ ,the content of aromatic compounds was about 80%,the content of phenols and ester compounds was less than 5%,the other oxygen-containing compounds was 11.29%.However,in the liquid product which was obtained at 270 ℃ ,the content of aromatic compounds was decreased by 31.69%,the volume fraction of oxygen containing compounds was increased by 2.81%,the content of phenols and ester com-pounds was increased to about 35%.Ether oxygen bonds were broken up during supercritical ethanol,there were large amount of phenolsin in which phenol and its derivatives were the main components and esters,mainly ethyl esters in liquid products.