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1、南京理工大学硕士学位论文2,4,6-三甲基苯甲醛合成与工艺研究姓名:杨光申请学位级别:硕士专业:应用化学指导教师:方志杰;张跃20060701'●“~_JI’’.曼主堡苎型受=三!苎苎里坠堕竺翌塞ABSTRACT2,4,6-trimethylbenzaktehyde(mes矗aJdehyde)isanovelfinalchemicalintermediate.Astheshortageofindusu'iali∞m栅叫kt啦technology,highpuritymesitaldehydeis9茂惭inthemarke
2、t.So,theresearchforthesynthesisofmeshakiehydeise懿圮miaLIndomesticandoverseas,therearemanysyntheticalmethods,includingincompleteoxidation,bromimtlonandhydro蛳Gl-ig∞rdreaction,usingzinccyanide,chloromethylatlonandhydrolyzation,reducingbenzoicacid.oxkIatmgbenzylalcoho
3、l,formylalionandSOOILInn霹鼯mcl呐theproductarecomplicated,theyieldislowandthecostishi血Weadoptmeansofformylationtosynthesizem骼妇I如hyde,usingm鼯it)riene、COandHCI∞thematerials,l,2-Chloroetbaneasthesolvent,Lewiseacid撼thecatalyst.nIistechnologyhassomemeritssuchaslowCOstofm
4、aterial,lowrequirementforreactioncondition,littlee41vironi删pollution.Comparedwithtechnicsandequipmemofdifferentsyntheticrouksfor2,4,6-trimethyibanzaldehyde.Lowtempe鞠lll心forn啦ionprocessw勰adopted'underspecialrcactofandmild托a吐ionconditions,theproductwasⅣel'啪dbyformy
5、htereactionofmesit3rlenewithCOandHCl,usingLewiseacidasthecatalyst,1,2-Odoroethaneasthesolvent.WemakeoutsinglefactorexperimemandoptimaltrialtOoptimizationcatalysissystemandtechnicsofthereaction,,Theinfluencefactorsonpurityoffinalproductwereinvestigatedindetail'sus
6、hascatalyst,reactiontimeandtcmpc卿慨Thesyntheticrouteandreagtionmechanismof2,4,6-trimethylbenzaldehydewe犯alsointroducedinthispsper.Aftera簧堍sofstableexperiment,theoptimalCOnditionsofsynthesiswere:mesitylene/AICl3/Cu2C12/1,2-CH2CICHzC
7、=I:2.0:0.21:2.o.reactiontime:18h
8、ours,temperature-25tO30"C,thesingle-pass-conversion啪reach80%一90‰andtheyieldreached59%.Variouselementweresepardtedbyrectification,theCOlltentoftbeaimed阳,ductreached98.5%bythe搬normalizationmethod,Theproductwas(k'terminatedbyNMR、IRandGC·MS.duringtheCOurseofreaction,
9、GCwasusedtOquantitativedetermination.Thismethodofformylatlonhassoftiemerits,mc姗ingabundantrawmaterials,mildreactionCOnditions,muchlessoftheCOntentofisomer.Atth