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1、序号配体条件结构来源1ZrOCl2.8H2O(200mg),H3TATB(60mg)and0.6mLtrifluoroaceticacidin12mLofDEFwereultrasonicallydissolvedinaPyrexvial.Themixturewasheatedat120ºCinanovenfor12h.Aftercoolingdowntoroomtemperature,whitepowdercrystallineprecipitatewasharvestedbyfiltrationPCN-777Angew.Chem.Int.Ed.2014,
2、53,1–72Allsamplesweresynthesizedviaarefluxmethodinvolvingthereactionof2-sulfoterephthalicacidwithZrCl4inwaterunderrelativelyconcentratedconditions.Forthesamplewithnoadditivesduringsynthesis(1),monosodium2-sulfoterephthalicacid(5g,18.6mmol)wasdissolvedinminimalwater,andthenpassedthr
3、oughDOWEX50WX8protonexchangeresintoobtain2-sulfoterephthalicacid.Thewaterwasthenremovedbyrotaryevaporation,then40mLoffreshultrapurewaterwasaddedtodissolvethesolid.Separately,ZrCl4(2.5g,10.7mmol)wasdissolvedinDOI:10.1021/jacs.5b07267J.Am.Chem.Soc.XXXX,XXX,XXX−XXX15mLofultrapurewater
4、(caution,highlyexothermic),thenthetwosolutionsweremixedtomakeaclear,slightlypinksolutionwithpH<1.Thesolutionwasthenheatedtoreflux,andafter~3minutesawhiteprecipitateformed.Refluxwascontinuedfor16hours,thenthesolutionwascooledandthesolidwasrecoveredbycentrifugation.Thesolidwasthenwas
5、hed2xwithultrapurewater,thenrefluxedforanother16hoursinultrapurewatertopurify.3Synthesisof14nmUiO-66-N3(Zr6O4OH4(C8H3O4-N3)62-Azido-1,4-benzenedicarboxylicacid(50mg,0.24mmol)wasdissolvedin1mLofN,NDimethylformamide(DMF).Inaseparatevial,zirconylchlorideoctahydrate(21mg,0.066mmol)wasd
6、issolvedin3mLofDMF.Thetwosolutionsweremixedtogetherina10mLscintillationvial,andaceticacid(300µl)wasaddedtothereactionmixture.纳米级别dx.doi.org/10.1021/jaw
7、J.Am.Chem.Soc.2014,136,7261−7264Thesolutionwasheatedat90˚Cfor18htoyieldUiO-66-N3(Zr6O4OH4(C8H3O4-N3)6.MOFnanoparticleswerepurified
8、bycentrifugation(15000rpm,90min)followedbysolventexchange(3xDMFand3xNANOpureH2O)overa48hperiod.MOFnanoparticlesweresuspendedinH2Oforcharacterizationandfunctionalizationwith4DUT-67.ZrCl4/HfCl4(230mg/320mg,1mmol)wasdissolvedinthemixtureofDMF(12.5mL)andNMP(12.5mL)bysonicationfor10min.
9、2,5-Thiophenedicarboxylica
