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1、*利£-T業(yè)人學(xué)順I(yè):學(xué)位論文超細(xì)磁性固體超強(qiáng)酸催化合成乳酸乙酯的研究摘要采用化學(xué)共沉淀法制備了超細(xì)磁性Fe304基體,并通過(guò)液相低溫沉淀法制備出Zr02一Fe304,進(jìn)一步用硫酸溶液浸漬得到磁性國(guó)體超強(qiáng)酸S042-/Zr02--Fe304。通過(guò)磁強(qiáng)汁、XRD、激光粒度儀、TPD、IR等手段對(duì)固體超強(qiáng)酸催化劑的磁性、晶體結(jié)構(gòu)、粒徑大小、酸性強(qiáng)度等進(jìn)行了表征,結(jié)果表明制備的磁性催化劑,其磁性表征結(jié)果os=9796emu·g1,or=1232emu·g~,粒徑在27lnm--496nm之間,且屬于中強(qiáng)強(qiáng)度的固體超強(qiáng)酸。用磁性固體超強(qiáng)酸S04’/Zr02-
2、-Fe304作為催化劑催化合成乳酸乙酯進(jìn)行r研究,得到催化劑用量占乳酸質(zhì)量的3%,酸醇比為1:5,以無(wú)水硫酸鎂為脫水劑,(83±1)℃反應(yīng)進(jìn)行4.5h??疾炝舜判怨腆w超強(qiáng)酸催化劑的焙燒溫度、焙燒時(shí)間、磁性基質(zhì)與氧化鋯配比、浸漬液濃度等因素對(duì)催化活性的影響,確定了催化劑活化溫度400。C,活化時(shí)間25h,浸漬濃度l5mol/1,最高酯產(chǎn)率達(dá)到74.13%,能夠用磁場(chǎng)有效的回收,回收率9885%。結(jié)果表明制備的催化劑具有較高的活性,基本達(dá)到了預(yù)期目的。最后對(duì)動(dòng)力學(xué)進(jìn)行了初步研究。得出酯化反應(yīng)為二級(jí)反應(yīng),水解為零級(jí)反應(yīng),其反應(yīng)動(dòng)力學(xué)模型為:警吐c乳酸CL醇
3、一k一=o.13857e-27‰C№Cc口一545捌5e一?‰關(guān)鍵詞:乳酸乙酯,超細(xì),磁性,固體超強(qiáng)酸,酯化型型絲生望竺望生堅(jiān)堡些竺竺塾壁圣塑些!!塞STUDYONSYNTHESISEOFETHYLLACTATEBYULTRAFINEMAGNETICSUPERSOLIDACIDCATALYSTABSTRACTWeadoptedchem-depositionmethodintegratingdispersanttoprepareultrafinemagnelicparticles.Throughlowtemperaturedeposition,wepr
4、epareultrafineZr02一Fe304particlesAfterimmersinginsulfuracid,WegettheS04’/Zr02--Fe304ultrafinemagneticsupersolidacidThroughXRD,TPD,IRetc.methodtocharacterthecatalyst.theresultindicatethattheparticlesizeiSbetween27lnln--496nmmaditbelongstomiddingintensitysupersolidacid.Themagneti
5、cresultsshowsthatos=97.96emu·g~.OF】2.32emu·g-l,particlesizeiSat271nln一496nmUsingthecatalysttocatalysethereactionoflactieacidandethanol,westudiedtheeffectofcalcinedtemperature,calcinedtime,ratioofZr02andFe304,andconcentrationofimmersingsolutionontheactivityofcatalyst.Theexperime
6、ntalresultsindicatethattheoptimizationofpl‘eparationis:Fe304:Zr02=l:5.5,pH=11.5,amountofdispersantaccountsforl%ofcatalyst.a(chǎn)ctivationtemperatueiS400℃.a(chǎn)ctivationtimeiS25h.Theoptimizationresultwehavegottenis:catalystaccoutfor3%oflacticacidamount.proportionofethanoltoacidisl:5,reac
7、tiontimeiS45hThehighestyieldrateofethyllactestiS74l3%.Catalystcanberecycled,andtherecycleratiois98.85%.Theseresultsilluminatethecatalystwepreparedhasreachedouranticipation,Atlast,wetakeapiotstudyonkinetics.Theconclusionisobtained:theesterificationissecond—orderreaction,andthehy
8、drolysisiSzero~orderreaction,SOthemodelforreactionkine