胜利褐煤和小龙潭褐煤在甲醇中的热溶及热溶物分析  

Thermal dissolution of Shengli and Xiaolongtan lignites in methanol and analysis of the soluble portions

作　　者：闫洁[1] 赵云鹏[1] 肖剑[1] 田由甲[1] 

机构地区：[1]中国矿业大学煤炭加工与高效利用教育部重点实验室,江苏徐州221116

出　　处：《燃料化学学报》2016年第1期15-22,共8页Journal of Fuel Chemistry and Technology

基　　金：国家自然科学基金青年科学基金(21206188);中国博士后科学基金面上项目(2012M511339);江苏省高校优势学科项目资助~~

摘　　要：研究了胜利褐煤(SL)和小龙潭褐煤(XLT)在甲醇中的热溶行为,并利用傅里叶变换红外光谱、气相色谱/质谱(GC/M S)和大气压固体分析探针/飞行时间质谱(ASAP/TOF-M S)对320℃热溶物的组成和结构特征进行了分析。两种褐煤热溶物产率均随温度升高而增加,但240℃后XLT热溶物(SPXLT)产率明显高于SL热溶物(SPSL)。GC/MS分析表明,两种褐煤热溶物以含氧化合物为主,尤其酚类的相对含量超过49%;与SPXLT相比,SPSL中烯烃、芳烃、醚类、羧酸、酯类和有机硫化合物(OSCs)含量较高,而烷烃、酚类、酮类和有机氮化合物含量较低;SPSL中的OSCs以噻吩为主,而SPXLT中的OSCs以硫醇为主。ASAP/TOF-M S可检测出热溶物中大量GC/M S无法检测出的较强极性和难挥发化合物;与SPXLT相比,SPSL中CHO和CHS族分含量较低,而CHN、CHNO、CHOS、CHNS和CHNOS族分含量较高;两种褐煤热溶物中化合物的碳数和双键数(double bond equivalent,DBE)主要分布在3-15和0-10,SPXLT中化合物的碳数和DBE分布相对集中。Thermal dissolution behaviors of Shengli（ SL） and Xiaolongtan（ XLT） lignite in methanol were investigated. The composition and structural characteristics of soluble portions（ SPs） obtained at 320 ℃ were characterized with Fourier transform infrared spectroscopy,gas chromatograph / mass spectrometer（ GC / MS）and atmospheric solid analysis probe / time of flight mass spectrometer（ ASAP / TOF-MS）. For the two lignites,the yield of SPs increase with temperature increasing,while the yield of SPs from XLT（ SPXLT） is obvious higher than that from SL（ SPSL） above 240 ℃. GC /MS analysis results showthat compounds in the SPs are dominated in oxygen-containing organic species,especially the relative content of phenols is higher than 49%.The relative contents of alkenes,arenes,ethers,carboxylic acids,esters,organosulfur compounds（ OSCs） in SPSLare higher,while the relative contents of alkanes,phenols,ketones and organonitrogen compounds in SPSL are lower than those in SPXLT. Additionally,the OSCs in SPSLand SPXLTare mainly composed of thiophenes and mercaptan,respectively. Many compounds with high polarity and lowvolatility which could not be identified by GC / MS were identified using ASAP / TOF-MS. The relative contents of CHO and CHS class species in SPSLare higher,but the relative contents of CHN,CHNO,CHOS,CHNS and CHNOS in SPSLare lower than those in SPXLT. The carbon number and double bond equivalent（ DBE） of the compounds in SPSLand SPXLTmainly distribute in 0-10 and 3-15,respectively,while the distribution of carbon number and DBE of the compound in SPXLTare more concentrated than those in SPSL.

关 键 词：褐煤 热溶 气相色谱/质谱 大气压固体分析探针/飞行时间质谱 

分 类 号：TQ530[化学工程—煤化学工程]