Separation And Analysis Of Group Components Of The Petroleum Ether Insoluble Fraction Of The Coal Tar

The petroleum ether insoluble fraction of the coal tar(that was named CTPI)had high separation value,because there were abundant phenols and polycyclic aromatic structures in it.But the separation and analysis of the components of CTPI was premise of classified and qualitative utilization.This paper took CTPI as the study subject,and it was separated by the way of cloumn chromatography and gradient extraction.The isolates of CTPI were analyzed by elemental analysis,GPC,Uv-fluorescence spectra,TG-FTIR,FTIR 13 C NMR and Py-GC/MS.The strong and weak points of cloumn chromatography and gradient extraction in the case of the separation of CTPI were also studied in the same time.The column chromatography separation process took the solvent extraction column chromatography device as the separator.CTPI was speparated into toluene eluate(TS),ethanol eluate(EAS),methanol eluate(MAS),tetrahydrofuran eluate(THFS)and residue(IS)with toluene,ethanol,methanol and tetrahydrofuran as eluent in order.The gradient extraction process took soxhlet extractor as the separator.First of all,CTPI was extracted into aether extract(EE),ethyl acetate extract(EACE),tetrahydrofuran extract and residue(THFR)with aether,ethyl acetate and tetrahydrofuran as extraction agent in order.And then EE was extracted into carbon tetrachloride extract(CTE),toluene extract(TE)and residue(TR)with carbon tetrachloride,toluene as extraction agent in order.The main conclusions are as follows:(1)The molecular weight from small to large followed by TS,EAS,MAS and THFS.The molecular weight of elutions of cloumn chromatography gradually increased as the elution continued.The largest number of polycyclic aromatic structures were gradually decreased in the order of THFS,MAS,TS,EAS.Nitrogenous compounds were mostly found in TS.Acid compunds were maily found in EAS and MAS.Aliphatic hydrocarbons were maily distrubuted in THFS.In addition,there were oxygen compunds,heterocyclic compunds,acid compunds and a little aliphatic hydrocarbons in IS.The total yield of eluate was 55.30 %.The separation and enrichment of nitrogen compunds,acid compunds and aliphatic hydrocarbons was achieved by cloumn chromatography,but the separation amount was too low.(2)The molecular weight from small to large followed by THFR,EE,CTE,TE,EACE,TR,THFE in the isolates of gradient extraction.The largest polycyclic aromatic structures were found in THFE and THFR.And the largest number of polycyclic aromatic structures were gradually decreased in the order of TE,EACE,TR,CTE,EE.EE,EACE,THFE,THFR,CTE,TE and TR all contained acid compounds,aliphatic hydrocarbons,oxygen compounds,aromatic hydrocarbons,heterocyclic compounds but the contents of compounds in different isolates were different.The contents of methoxy group in THFE and EACE were higher.The contents of aliphatic hydrocarbons in TR was lower.The total yield of isolate was 98.40 %.A few components of CTPI were enriched by gradient extraction.And the separation amount was large.However,the components of the separation by gradient extraction were seriously overlapped.(3)Column chromatography was stronger than gradient extraction in separation and enrichment.Gradient extraction was stronger than column chromatography in separation amount.Gradient extraction was proper for crude separation.And column chromatography was proper for separation and purification.