功能材料
功能材料
공능재료
JOURNAL OF FUNCTIONAL MATERIALS
2012年
18期
2568-2572
,共5页
马文石%张冬桥%段宇%万兆荣%王洪%徐迎宾
馬文石%張鼕橋%段宇%萬兆榮%王洪%徐迎賓
마문석%장동교%단우%만조영%왕홍%서영빈
聚硅氧烷微球%制备%甲基三甲氧基硅烷%乙烯基三甲氧基硅烷%巯丙基三甲氧基硅烷
聚硅氧烷微毬%製備%甲基三甲氧基硅烷%乙烯基三甲氧基硅烷%巰丙基三甲氧基硅烷
취규양완미구%제비%갑기삼갑양기규완%을희기삼갑양기규완%구병기삼갑양기규완
polysilsesquioxane microsphere%preparation%methyitrimethoxysilane(MTMS)%vinyltrimethoxysilane(VTMS)%3-mercaptopropyltrimethoxysilane(MPTMS)
以乳液聚合法制备粒径分布均匀、球形度良好的聚甲基硅氧烷微球(MPSQ)、聚乙烯基硅氧烷微球(VPSQ)、聚巯丙基硅氧烷微球(MPPSQ),采用SEM、DLS、FT-IR、XRD、TGA、接触角等测试技术对微球的微观形貌、粒径大小及分布、聚集态结构、耐热性、疏水性等进行了表征。研究结果表明,有机基团对微球的耐热性与疏水性有重要影响,MPSQ和VPSQ的耐热性优于MPPSQ,疏水性从高到低依次为:MPSQ〉VPSQ〉MPPSQ。聚硅氧烷微球的形成过程可能是单体首先在催化剂的作用下,水解生成硅醇,硅醇开始缩聚形成核,之后通过吸取溶液的硅醇,不断成长,最终形成微球,其中同时存在核生成和核生长,两过程相互竞争,哪个过程占优势取决于反应条件。提高反应温度,使得核生成占优势,最终生成的微球粒径变小,单分散性变差。
以乳液聚閤法製備粒徑分佈均勻、毬形度良好的聚甲基硅氧烷微毬(MPSQ)、聚乙烯基硅氧烷微毬(VPSQ)、聚巰丙基硅氧烷微毬(MPPSQ),採用SEM、DLS、FT-IR、XRD、TGA、接觸角等測試技術對微毬的微觀形貌、粒徑大小及分佈、聚集態結構、耐熱性、疏水性等進行瞭錶徵。研究結果錶明,有機基糰對微毬的耐熱性與疏水性有重要影響,MPSQ和VPSQ的耐熱性優于MPPSQ,疏水性從高到低依次為:MPSQ〉VPSQ〉MPPSQ。聚硅氧烷微毬的形成過程可能是單體首先在催化劑的作用下,水解生成硅醇,硅醇開始縮聚形成覈,之後通過吸取溶液的硅醇,不斷成長,最終形成微毬,其中同時存在覈生成和覈生長,兩過程相互競爭,哪箇過程佔優勢取決于反應條件。提高反應溫度,使得覈生成佔優勢,最終生成的微毬粒徑變小,單分散性變差。
이유액취합법제비립경분포균균、구형도량호적취갑기규양완미구(MPSQ)、취을희기규양완미구(VPSQ)、취구병기규양완미구(MPPSQ),채용SEM、DLS、FT-IR、XRD、TGA、접촉각등측시기술대미구적미관형모、립경대소급분포、취집태결구、내열성、소수성등진행료표정。연구결과표명,유궤기단대미구적내열성여소수성유중요영향,MPSQ화VPSQ적내열성우우MPPSQ,소수성종고도저의차위:MPSQ〉VPSQ〉MPPSQ。취규양완미구적형성과정가능시단체수선재최화제적작용하,수해생성규순,규순개시축취형성핵,지후통과흡취용액적규순,불단성장,최종형성미구,기중동시존재핵생성화핵생장,량과정상호경쟁,나개과정점우세취결우반응조건。제고반응온도,사득핵생성점우세,최종생성적미구립경변소,단분산성변차。
Highly uniform and monodisperse methyl-functionalized polysilsesquioxane microspheres(MPSQ)、 vinyl-functionalized polysilsesquioxane microspheres(VPSQ) and thiol-functionalized polysilsesquioxane microspheres(MPPSQ) were prepared by emulsion polymeration.The morphology,size distribution,and state of aggregation were characterized by SEM,DLS,FT-IR,XRD.The thermodecomposition and hydrophobicity of these microspheres were investigated with TGA and water contact angle measurement.The results showed that the organofunctional groups played a key role in thermostability and hydrophobicity of microspheres,MPSQ and VPSQ possessed better thermostability than MPPSQ,the order of hydrophobicity was as following : MPSQ 〉VPSQ〉MPPSQ.The formation mechanism of polysilsesquioxane microspheres may be explained by nucleation theory.First,the silanol groups came out when the precursor was catalyzed by triethylamine,then the polycondensation of silanol groups began and a large number of nuclei generated,and all the nuclei started to grow up by absorption of silanol groups in the solvent.Finally,monodisperse polysilsesquioxane microspheres formed.The nuclei generation process and nuclei growth process competed with each other during the reaction.The reaction condition determined the process which dominated the reaction.The particle would turn smaller and less monodisperse with increasing of the reaction temperature rises.