Journal of South China University of Technology(Natural Science Edition) ›› 2012, Vol. 40 ›› Issue (4): 95-100,106.

• Materials Science & Technology • Previous Articles     Next Articles

Preparation and Formation Mechanism of Narrow-Dispersed Poly( Aminopropyl /Phenylsilsesquioxane) Microspheres

Liu Shu-mei1  Sun Zhi-song1  Zhang Yu2  Zhang Li-ping2  Zhao Jian-qing1   

  1. 1.School of Materials Science and Engineering,South China University of Technology,Guangzhou 510640,Guangdong,China; 2.Guangzhou Tinci Silicone Technology Co. ,Ltd. ,Guangzhou 510760,Guangdong,China
  • Received:2011-08-05 Revised:2011-12-29 Online:2012-04-25 Published:2012-03-01
  • Contact: 刘述梅(1968-) ,女,博士,副教授,主要从事有机硅合成、高分子材料改性等的研究. E-mail:liusm@scut.edu.cn
  • About author:刘述梅(1968-) ,女,博士,副教授,主要从事有机硅合成、高分子材料改性等的研究.
  • Supported by:

    广东省教育部产学研结合项目( 2010B090400150) ; 广州市科技攻关项目( 2010J-D00371)

Abstract:

Narrow-dispersed poly( aminopropyl /phenylsilsesquioxane) ( PAPSQ) microspheres were prepared via the hydrolytic cocondensation of γ-aminopropyltriethoxysilane ( APS) and phenyltriethoxysilane ( PTES) under the action of alkali catalysts,and the effects of the APS-to-PTES molar ratio,the water-to-silicon molar ratio,the cosolvent type,the tetramethylammonium hydroxide ( TMAOH) concentration and the total monomer concentration on the morphology and size of PAPSQ microspheres were explored by using a scanning electron microscope and a particle size analyzer. Moreover,the formation mechanism of the microspheres under different reaction conditions was investigated. The results indicate that ( 1) when ethanol is used as the co-solvent,narrow-dispersed microspheres with a diameter ranging from 0.7 to 1.0 μm are obtained at an APS-to-PTES molar ratio of 1 /4,a water-to-silicon molar ratio of 50,a TMAOH concentration of 0.025mol /L and a total monomer concentration of 0.25mol /L; ( 2) with ammonia as the catalyst and with isopropanol as the co-solvent,microspheres with large size and broad distribution can be obtained; ( 3) only partial spherical particles may form at lower water-to-silicon molar ratio and TMAOH concentration; and ( 4) no spherical particles can form if the total monomer concentration is too high.

Key words: γ-aminopropyltriethoxysilane, phenyltriethoxysilane, alkali catalysis, hydrolytic copolycondensation, microspheres, particle size, narrow dispersion