冶金分析

,2009,29(1):21224MetallurgicalAnalysis,2009,29(1):21224:1000-7571(2009)01-0021-041,31,2,1,1,1(11,102200;21,100871):,112mol/LNaOH,200,,(101,V/V),/:3400cm-1,15001600cm-1,1700cm-1,1200cm-1,-OH-C=O:918,,No1497%,():;;/;;:O657163,O657133:A:2008-03-05:(1980-),,,:,,,;Tel:[phone],E2mail:qilu@pku1edu1cn,2(F2T)[1-2],[3-5],H2O2[6],,,Jun2ichiroH[7]100,;KazuhiroM[8]H2O2,H2O2,/,,1111QP2010plus/();FTIR28400();pHS23C();()H2O2(=30%)NaOH(,);(,);1125010g200,H2O2112mol/LNaOH,2002mol/LpH2,,60,NaCl,,(101,V/V),GC2MS113GC2MS:RTX25MS30m0125mm0125m;:30,10/min280,5min;:1L;:250;:;:EI2,12FENGBo,QILu,ZHANGJing2hua,etal.Qualitativeanalysisofbrowncoaloxidationproductsinmildoxidizingatmosphere.MetallurgicalAnalysis,2009,29(1):21224,,[9-11],,211,,1:3400cm-1,O2H;3000cm-1=C2H;15001600cm-1;1700cm-1C=O;1380cm-1-CH3;1200cm-11Fig11Fouriertransforminfraredspectrafortheseparatedsample212GC2MS2GC2MS21NIST05s1LIB,,11,9182Fig12TICoftheseparatedsample22,,,..,2009,29(1):212241Table1PossiblestructuresofthecomponentsinseparatedsampleNo1Compound(Similarity)No1Compound(Similarity)11,22121,22dichlorocyclopentane(91)n2tridecanoicacid(63)2221322chlorocyclopentanol(89)n2tetradcanoicacid(88)314n2nonylicacid(86)n2pentadecanoicacid(62)4221522hydroxy2benzoicacid(97)n2hexadecoicacid(85)516n2decanoicacid(87)n2heptadecoicacid(80)6222321722hydroxy232methyl2benzoicacid(89)n2pentadecanoicacid(91)7222521822hydroxy252methyl2benzoicacid(95)Dibutylphthalate(96)81912n2undecylicacid(91)1H2indenol(79)922(22)201,6,7221,4222,3222(22methyl2propenyl)2phenol(80)1,6,72trimethyl21,42dihydro22,32quinoxaline(61)10422322142hydroxy232methoxyphenyl2acetophenone(94)n2octadecanoicacid(85)11n2dodecanoicacid(91)213GC2MS2No11No12,,[12]13400cm-1,1700cm-1,1No13,No15,No18,No11117No121918,,No14,No16,No17,No14,97%,,3MccutcheonAL[13],C=O,C2OCOOH,,No120,61%,3No14()()Fig13MSgraphsoftheNo14(left)ando2hydroxy2benzoicacidstandardsample(right)32FENGBo,QILu,ZHANGJing2hua,etal.Qualitativeanalysisofbrowncoaloxidationproductsinmildoxidizingatmosphere.MetallurgicalAnalysis,2009,29(1):212243/,918,,:[1]1[J]1(ModernChemicalIndustry),2005,25(10):172221[2]1[J]1(CoalmineDesign),2000,3:412421[3],LawrencePN,EdwinlL,1[J]1(JournalofFuelChemistryandTechnology),2001,29(2):21422181[4]1[J]1(CoalQualityandTechnology),2004,3:562571[5],,1NMR[J]1(CoalConversion),2006,29(3):372391[6],,,1GC/MS[J]1(JournalofFuelChemistryandTechnology),2005,33(1):12121241[7]Jun2ichiroH,YoshihiroM,KatsukiK,etal1Depo2lymerizationoflowerrankcoalsbylow2temperatureO2oxidation[J]1Energy&Fuels,1997,11:22722351[8]KazuhiroM,TaisukeM,JunA,etal1Extractionoflow2rankcoalsoxidizedwithhydrogenperoxideinconventionallyusedsolventsatroomtemperature[J].Energy&Fuels,1997,11:82528311[9],,1[J]1(CoalConversion),2006,29(2):922981[10]1[J].(CoalConversion),1995,18(1):1291[11],1[J]1(JournalofPetrochemicalUni2versities),1997,10(4):1251[12],,,12/[J]1(Metal2lurgicalAnalysis),2007,27(1):72111[13]MccutcheonAL,WilsonMA1Low2temperatureoxidationofbituminouscoalandtheinfluenceofmoisture[J]1Energy&Fuels,2003,17:92929331QualitiativeanalysisofbrowncoaloxidationproductsinmildoxidizingatmosphereFENGBo1,QILu31,2,ZHANGJing2hua1,SUNXiao2man1,YANGFan1(11CITICGuo’anMGLNewMaterialsandTechnologyResearchCompanyLimited,Beijing102200,China;21DepartmentofAppliedChemistry,CollegeofChemistry&MolecularEngineering,PekingUniversity,Beijing100871,China)Abstract:In1.2mol/LNaOHsolution,browncoalwasoxidizedbyhydrogenperoxideafterpro2grammedheatedupto200.TheoxidationproductwasthenacidifiedbyHClandextractedbysoxhletextractionmethodwithmixedsolventofchloroformandethylacetate(VchloroformVethylacetate=101).TheobtainedorganiccompoundswereanalyzedqualitativelybyIRandGC2MS.Theabsorp2tionat3400cm-1,1500-1600cm-1,1700cm-1,and1200cm-1inIRspectrumindicatesthereare-OH,benzenering,-C=Oandphenolichydroxylinthecompounds.TheGC2MSanalysisre2sultsindicatethat,besidecarboxylicacidwith9-18carbons,theoxidationproductalsocontainsphe2nolicacid.AndthemassspectrumsimilarityoftheNo.4inthetotalionchromatogramwithsalicylicacidisupto97%.Theoxidationproductisconfirmedtobesalicylicacid.Keywords:browncoal;oxidation;gaschromatography/massspectrometry(GC2MS);fouriertrans2forminfraredspectra(FTIR);phenolicacid42