D-L-丙交酯的合成及表征

3022003JOURNALOFBEIJINGUNIVERSITYOFCHEMICALTECHNOLOGYVol.30,No.22003D,L2(,100029):,D,L2;IR1H2NMRMS;,,,95%:;D,L2;;:O6231624:2002206225:(QN0114):,1971,,E2mail:[e-mail],,(FDA)[1],[2][3],,,,1111(80%),,;,,Aldrich;,,;,,112,(170),80%95%230240,1133kPa34,501133kPa113,5/min,1/minCARLOERBA1106VGVG702SE,Nicolet2210BRUKERAC280NMR,:TMS,:CDCl3TU-1221,2,,1nCH3CHOHCOOHCH3CHOCOCHCH3COO1Fig.1Reactionoflactidesynthesis21180%,:20%,,111Table1Effectofexperimentationonthelacticesterification/h/%710NaOH25132610NaOH8011101056143310,NaOH85191.ZnO;2.10011050%;3102h100170,80%1,,,,(NaOH),;,,,-,,212,,,,,,2h95%,,,,,,,,,,,213,(OH)(),OH,,;,,,9910%,,,,,,:;,,,,,2142141134,,,,,,,12510,110,[4],21412,m/z,,1,14421413C6H8O422Table2Elementalanalysisoflactidew/%C50105013H516515O44144412,332:D,L2C6H8O421414,Nicolet2210,232IRFig.2IRoflactide3IRTable3IRanalysisoflactide/cm-1300411CH3CH3144418CH3300411295016292419CHCH138612CH175112COCO126212COOCO109912CO93016650152141531H2NMR3,=510737,1331,12177;=116307,11,39189,(CH3)(CH),CH3CHOCOCHCH3COO31H2NMRFig.31H2NMRoflactide21416214nm,[5]3(1),,95%(2)(3)[1],,,.[J].,1999,1:24-32[2],,,.CO2D,L2[J].,1999,16(3):41-43[3]KulkarniBK,MooreEG,HegyeliAF,etal.Biodegradablepoly(lacticacid)polymers[J].JBiomedMaterRes,1971,5:169-181[4],,.[J].,2002,30(2):10-12[5],.[J].,1998,4:15-16(39)432003[7]HirooIwata,IsaoHirata,YoshitoIkada.AtomicforcemicroscopicanalysisofaporousmembranewithpH2sensitivemolecularvalves[J].Macromolecules,1998,31:3671-3678[8]HirooIwata,IsaoHirata,YoshitoIkada.Atomicforcemicroscopicimagesofsolvatedpolymerbrushes[J].Langmuir,1997,13:3063-3066[9]YangWT,R¼nbyB.TheroleoffarUVradiationinthephotograftingprocess[J].PolymerBulletin,1996,37:89-96Preparationoftemperature2sensitivetrackmembranebybulkPhotograftingYANGBiaoYANGWan2tai(TheKeyLaboratoryofScienceandTechnologyofControllableChemicalReactions,MinistryofEducation,BeijingUniversityofChemicalTechnology,Beijing100029,China)Abstract:Thecompositemembranewiththermo2sensitiveeffectwaspreparedbybulkphotograftingNIPAAmontothePETtrackmembranesubstrate.ThegraftedmembranewascharacterizedbyFTIR2ATRandSEM.ItwasfoundthatphotograftmainlyproceedsonthemembranesurfaceexposingtoUVradiationandnograftpolymerizationoccursonthebacksidesurfaceandinsidepores.IncreasingtheUVintensityandtheratioofinitiatorinreactionmixtureresultsintheincreaseingraftingdegree.Atroomtemperature,thegraftingdegreeincreaseslinearlywiththeprolongationofradiationtime.Athighertemperature,theincreaseingraftingdegreebecomessmoothwhenradiationtimeexceedsninetyseconds.OncethetemperatureishigherthanthemeltpointofNIPAAm,thegraftingdegreedecreasesstrikingly.Thegraftedpoly2NIPAAmhaspore2coveringeffectandthusregulatesthefiltrationpropertiesofgraftedmembranes.ThetestresultsshowthatthefluxofgraftedmembranewithhighDghasaleapnearthetemperaturerangeof30to35;Graftedmembraneactasavalvebyresponsetothetemperature.Keywords:bulkphotografting;photografting;thermo2sensitivemembranes;pore2covering()(34)SynthesisandcharacterizationofD,L2lactideSHIShu2xianXIAYu2zhengGUOZu2pengJIAOShu2keLIXiao2yu(CollegeofMaterialsScienceandEngineering,BeijingUniversityofChemicalTechnology,Beijing100029,China)Abstract:TheD,L2lactidewaspreparedfromD,L2lacticacidwiththestannousoctoateasthecatalystandthefactorsaffectingthepreparationwerediscussed.ThelactidewascharacterizedbyIR,1H2NMR,MS,elementalanalysisandUltravioletspectrophotometry.Theresultsshowthatthewaterweightdetachedfromthelacticacidis95%andthestructureoflactideiscyclicdiester.Keywords:lactic;lactide;synthesis;characterization()932: