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1、河北工业大学硕士学位论文负载Ru催化剂上芳香胺加氢制脂环胺的研究姓名:郭迎秋申请学位级别:硕士专业:化学工艺指导教师:王延吉20070301负载Ru催化剂上芳香胺加氢制脂环胺的研究STUDYONSYNTHESISOFCYCLOALIPHATICAMIDESFROMAROMATICAMIDESHYDROGENATIONOVERSUPPORTEDRuCATALYSTABSTRACTSynthesisofcycloaliphaticamidesfromaromaticamideshydrogenationonsupportedRucatalystwasstudied,including
2、quantitativeanalysisoftheTDAhydrogenationproducts,thermodynamicanalysisofthehydrogenationreaction,thechoiceofcatalystsandoptimizationofoperatingconditionsforaromaticaminehydrogenation.Basedonqualitativeanalysisofaniline,OMA,MPDhydrogenationproductswithGC,TDAhydrogenationproductswasdeterminedb
3、yGC-MSandspaciousstructureanalysis.ThermodynamicanalysisoftheTDAhydrogenationsystemwasdonebythegroupcontribu-tionapproach.Thiswasanexothermicreactionwiththermodynamicsuperiorityandsidereactionsequilibriumconstantswereallgreaterthanthatofthemainreaction.Theby-productMCHAwasmainlyformedbydeamin
4、ationofthemainproductMCHD.Ru/γ-Al2O3(4%load),aromaticaminehydrogenationcatalyst,waspreparedwithanilinehydrogenationastheprobereaction.Anilinehydrogenationwasstudiedwithsinglefactorstestandtheoptimaloperatingconditionswereasfollows:w(aniline)/w(catalyst)was100:1(massratio),7MPa,160℃,4h.Underth
5、econditions,anilineconversionwas98.2%andanilineselectivity(cyclohexylaminetoaniline)was91.4%.OMAhydrogenationwasstudiedwithorthogonalexperimentandtheoptimalconditionswere:w(OMA)/w(catalyst)was100:1,8MPa,170℃,4h,OMAconversionwas99.4%.Theselectivity(OMCHAtoOMA)was97.9%.MPDhydrogenationwasstudie
6、dwithsinglefactorstest.Theoptimalconditionswere:w(MPD)/w(catalyst)was25:1,THF(solvent)20ml,highpressure,lowtemperatureandshorttime.Theselectivity(DACHtoMPD)couldreach49.5%.TDAhydrogenationwasstudiedwiththeaboveoptimalconditions.Calcinationtemperatureofthecatalysthasthegreatestinfluenceonselec
7、tivityofthemainproduct(MCHD).Theoptimalselectivitywas71.3%withthecalcinationtemperature400℃.KEYWORDS:aromaticamides,cycloaliphaticamides,hydrogenation,supportedRucatalystii河北工业大学硕士学位论文第一章文献综述§1-1工作背景及意义脂环胺是重要的有机化工和精细化工中间体,广泛用于橡胶助剂、食物添加剂、制药、防腐