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1、2006年第64卷化学学报Vol.64,2006第24期,2419～2424ACTACHIMICASINICANo.24,2419～2424·研究论文·磺酸功能化三维有序大孔材料的制备与催化性能研究廖菊芳邬泉周尹强王崇太李红玉李玉光*(中山大学化学与化学工程学院广州510275)摘要采用模板法,用正硅酸乙酯和3-巯丙基-三甲氧基硅烷的混合溶胶,在聚苯乙烯胶晶间隙中原位转化,除去模板后用双氧水将巯基氧化成磺酸基,首次成功地制备了大孔规整排列的3DOMSiO2-SO3H材料.样品用SEM,EDS,FT-IR等方法进行了测试表征.结果表明,所得到材料的三维大孔结构规整性
2、十分好,大孔孔径大约250nm,并由大约80nm的小孔相连;磺酸基很好地嵌入孔壁基质中,吡啶吸附测定显示了典型的质子酸特征,而且酸中心随硫含量增加而增多.对乙酸与正丁醇的酯化反应显示了良好的催化性能,磺酸含量越大,催化活性越高.这一研究为开发新型高效的固体酸催化剂提供了很有意义的结果.关键词三维大孔材料;磺酸功能化;酸催化;酯化PreparationandCatalyticPropertiesofSulfonicFunctionalized3DOMMaterialsLIAO,Ju-FangWU,Quan-ZhouYIN,QiangWANG,Chong-TaiLI,
3、Hong-YuLI,Yu-Guang*(SchoolofChemistryandChemicalEngineering,SunYat-SenUniversity,Guangzhou510275)AbstractUsingtemplatedmethod,sulfonicfunctionalizedthreedimensionalorderedmacroporous(3DOM)SiO2-SO3Hhybridmaterialshavebeenfirstpreparedviainsitutransformationofmixedsolcom-posedoftetraeth
4、oxysilane(TEOS)and(3-mercaptopropyl)trimethoxysilane(MPTMS)infiltratedinthein-terstitialvoidsofpolystyrenecolloidalcrystal,andfollowedextractionoftemplateandoxidationofthiolgroupstosulfonicgroupswithH2O2.SampleswerecharacterizedbySEM,EDS,FT-IRmethods.There-sultsshowedthatsynthesizedma
5、terialspossessedwell3DOMstructure.Theporeswereabout250nmandinterconnectedbysmallchannelsof80nm.Sulfonicacidgroupshadbeenwellanchoredintostructure-wall.Thedeterminationofpyridineadsorptionofsamplesrevealedthatmaterialshaveatypiccharacterizationofprotonacid,andtheprotonacidcentersincrea
6、sedwiththeincreaseofScontent.Catalystsshowedgoodperformanceinesterificationofaceticacidwithn-butanol,moreover,thehighercontentofsulfonicacidis,themoreactivecatalystsare.Thisstudyprovidedsignificantresultsfordevelopmentofnewhighperform-ancesolidacidcatalysts.Keywordsthreedimensionalord
7、eredmacroporous;sulfonicacidfuntionalized;acidcatalysis;esterifica-tion三维有序大孔材料(3DOM)是近年发展起来十分新通的特性,在诸如光子晶体、催化剂、生物传感器等物[1～3]颖的研究课题.其孔道系统规则排列,孔径均一而又相理、化学和生物领域有着十分诱人的应用前景.作*E-mail:ceslyg@zsu.edu.cnReceivedMarch13,2006;revisedApril25,2006;acceptedAugust22,2006.广东省科技厅十五重大专项基金(No.A3040302)
8、资助项目.
