7-氨基頭孢烷酸反應結(jié)晶過程研究.pdf

1、天津大學博士學位論文7氨基頭孢烷酸反應結(jié)晶過程研究姓名：王水申請學位級別：博士專業(yè)：化學工程指導教師：王靜康20050601天津大學博士學位論文摘要ABSTRACT7aminocephalsporanicacid(7ACA)isanimportantintermediateinthemanufactureofsemisyntheticcephalosporanieantibioticsWiththeincreasingdemandfor

2、cephalosporinsandhigherquality7ACAinrecentyears，therequirementof7ACAwasincreasedcorrespondinglyCrystallizationprocessisthecriticalstepofdecidingthequalityofproductInthisthesis，thereactivecrystallizationprocessof7ACAwasst

3、udiedsystematicallybothinexperimentandtheoryByindexingthe7ACApowderXraydiffractiondatausingindexingprogramnamedTREOR90，thecrystalMillerindicesandcrystalsystemweredeterminedThecrystalspacelatticeof7ACAWascalculatedbyrunni

4、ngPolymorphincommercialsoftwareCerius2Thetheoreticalcrystalhabitof7ACAwaspredictedbyBFDHandAEmodelrespectivelyIthasbeenprovedthattheproducts，whichwereproducedfromdifferentreactivecrystallizationprocesses，belongtothesamec

5、rystalsystemwiththesamechemicalcomposition，basedonthemeasureddatawithIRspec訂aandpowderXRDinstrumentsUsingtheSEMandpowderXRDinstruments，theagglomerationvaluesoftwocrystallizationprocesses，withacidorbasiccrystallizationcon

6、ditionwerestudiedTheeffectsofagitationspeedon7ACAproductagglomeratingvalueswereobservedBydealingwithSEMphotographesofabovetwoprocesses，itCanbeseenthatthegrayscaledistributionsforthesamesamplealeextremelysimilarwhichindic

7、atesthatthemorphologyof7ACAcrystallizationexhibitsselfsimilarityatdifferentscalesThefractaldimensionsof7ACAcrystalsfromtwodifferentcrystallizationprocessesweredeterminedbyboxdimensionmethodAccordingtofractaldimensionsof7

8、ACAcrystals，agglomerationmechanismhasbeenpresumedZetapotentialsweremeasuredfordifferentialpHvaluebyzetapotentialanalyzerInaddition，thecapillaryriseofliquidincolumnspackedv“tll7ACApowderwaSmeasuredandthewettabilitiesoface

9、toneandwatertotwo7ACAsamplesweredeterminedCombiningthetestresultsofIRandpowderXraydiffraction，thefunctionalgroupsonthesurfacesofcrystalsmanufacturedfromabovetwoprocesseswerepresumedThe7ACAagglomerationratemodelwasestabli

10、shedCrystalyieldisdecidedbycrystallizationthermodynamicsThesolubilityof7ACAunderdifferenttemperature，solventandpHweremeasuredbythelightextinctionmeasurementThesolubilitydatainbinarymixturesolventacetonewaterwerefittedwit

11、hboththeRKequationandthe2h—equationandthecorrelativeparameterswereestimatedbylinearandnonlinearleastsquareregressionmethodsrespectivelyCrystallizationmtastablezoneof7ACAinacidicandbasiccrystallizationconditionsweredeterm