TiO-2溶胶的制备及其胶凝过程影响因素分析

TiO2,,(,430074)[]利用乙酰丙酮(Acac)为螯合剂,钛酸丁酯为前驱物,用溶胶凝胶法制备TiO2溶胶通过改变乙酰丙酮(Acac)的量加水量溶剂量催化剂的量水解温度等因素,研究了溶胶胶凝时间随其影响因素的变化规律[]TiO2溶胶,Acac,溶胶凝胶,胶凝时间[]TQ031.2[]A[]1001-3660(2004)01-0030-02PreparationofTiO2SolandAnalysisonGelationProcessWENMin,QIGongtai,SUNJumei(CentralChinaUniversityofScienceandTechnology,Wuhan430074,China)[Abstract]Withacetylacetone(Acac)ascomplexationpreparation,Ti(OBu)4asprecusor,TiO2solwaspreparedbysolgelmethod.ThroughchangingtheamountofAcac,water,solvent,catalystandhydrolysistemperature,thegelationtimewiththeirdifferentfactorswerestudied.[Keywords]TiO2Sol;Acac;Solgel;Gelationtime[]2003-09-30[](1979-),,,,0TiO2TiO2[1~4],(Acac),TiO2,[5~10],TiO21TiO21[Ti(OC4H9)4](C2H5OH)(CH3COCH2COCH3)HClTiO2,Acac,,78130min,KQ11810min,,++++Acac30min10min1TiO22[M(OR)n],:M(OR)n+H2OM(OH)(OR)n-1+ROH(1)M(OH)(OR)n-1+H2OM(OH)2(OR)n-2+ROH,M(OH)n-M-OH+HO-M--M-O-M+H2O(2)-M-OR+HO-M--M-O-M+ROH(1)(2),,,Kh=10-3mol/(L!s)[6],,,(Acac):TiO230Ti(OBun)4+mAcacHTi(OBun)4-mAcacm+mBun-OH,,,OH-,,Ti(OBun)4OH-Ti(OBun)4,,2.1,,,,,AcacA,B,BA,,,,,TiO2,2.2Acac,n(C2H5OH)/n[Ti(OBu)4]=10n(HCl)/n[Ti(OBu)4]=0.03,,Acac,TiO22,3n(Acac)/n[Ti(OBu)4]=00.10.3,23,Acac,,,Acacn(Acac)/n[Ti(OBu)4]∀2[11],[8],n(H2O)/n[Ti(OBu)4]=4,,Acac(n=00.10.3),,,,,,,,n(Acac)/n[Ti(OBu)4],(∀2),Acac,,n=4,TiO2,(n4),,,TiO2,TiO2,,,2#n(Acac)/n[Ti(OBu)4]#0.4,22.3n(H2O)/n[Ti(OBu)4]=3n(Acac)/n[Ti(OBu)4]=0.3n(HCl)/n[Ti(OBu)4]=0.03,,33,,,40∃,,40∃,,,,,,,,,,,,,2.4n(H2O)/n[Ti(OBu)4]=3n(Acac)/n[Ti(OBu)4]=0.3n(HCl)/n[Ti(OBu)4]=0.03,,n(C2H5OH)/n[Ti(OBu)4],4,,n,H2O,H2O,,TiO2,,,,,,,,45HCl2.5HCln(C2H5OH)/n[Ti(OBu)4]=10n(H2O)/n[Ti(OBu)4]=1n(Acac)/n[Ti(OBu)4]=0,HClpH,,n(HCl)/n[Ti(OBu)4],5,HCl(下转第39页)331Vol.33NO.120042SURFACETECHNOLOGYFeb.2004315;75h,,CO2H2S,,,,,[6]:,;,,;,,;,Fe2Al5,3(1)0%~1.0%,,,;(2)CO2:0%~1.0%,,;1.0%,,2(3)H2S:CO2;1.0%,,3[][1].[J].,1991,18(5):51~55.[2].[J].,1997,18(5):48~50.[3],.[J].,1998,18(5):1~3.[4].[J].,1999,20(1):69~71.[5],.[J].,1999,17(1):42~45.[6],,,.H2S3%NaClH2O[J].,2001,34(6):10~12.(上接第31页)5,,pH,n(HCl)/n[Ti(OBu)4]#0.3,pH2,22.6HCl,TiO2[][1],,.TiO2[J].,2002,35(7):4~5.[2],,,.[J].,2001,34(12):12~13.[3],,,.SiO2[J].,1994,25(1):82.[4],,.SiO2TiO2ZrO2[J].,2002,35(5):7~9.[5]C.LegrandBuscema,C.Malibert,S.Bach.ElaborationandcharacterizationofthinfilmofTiO2preparationbysolgelprocess[J].ThinSolidFilms,2002,418:79~84.[6],.NMPTiO2[J].,2002,19:882~885.[7],.Ti(OC4H9)4[J].,2002,2(2):435~438.[8],,,.TiO2[J].,1999,30(4):407~409.[9],.TiO2[J].,2001,25(6):88~91.[10]Attia,SM,,.TiO2[J].,2001,29(10):1209~1212.[11]PontonA,BarbouxDoeuffS,SanchezC.Rheologyoftitaniumoxidebasedgels:determinationofgelationtimeversustemperature[J].ColloidsandSurface,2000,162:177~192.331Vol.33NO.120042SURFACETECHNOLOGYFeb.200439