Synthesis and micromorphology of long-chain alkyl polymethylsilsesquioxane nano-hybrid emulsion
Hao Lifen, Pei Mengmeng, Wang Xuechuan, Xu Wei, Yang Ruini, Yang Baiqin
Key Laboratory of Auxiliary Chemistry and Technology for Chemical Industry,Ministry of Education,College of Chemistry and Chemical Engineering,Shaanxi University of Science and Technology,Xi'an 710021
Abstract: A sort of long-chain alkyl polymethylsilsesquioxane(PDMSQ) nano-hybrid emulsion was prepared via emulsion polymerization of methyltriethoxysilane (MTES) and dodecyltrimethoxysilane(DTMS) and used sodium hydroxyl as the catalyst,solium dodecyl sulfonate/Twain 80 as mixed emulsifiers.Effects of emulsifier dose,catalyst concentration and oil/water ratio were discussed.Structure,particle size,micromorphology and thermal stability of PDMSQ NPs were investigated by FT-IR,XPS,DLS,SEM and TG.Results indicated that the structure of PDMSQ NPs was consistent with the designed and thermal stability of PDMSQ NPs was excellent.When w(SDS/T80) was 0.71%,NaOH concentration was 50~100mmol/L and the oil/water ratio was 1∶4~6,the average particle sizes of narrowly distributed PDMSQ NPs were less than 80nm.Meanwhile PDMSQ NPs were regularly spheres.
[1] Dong Fuping,Xie Haibo,Zheng Qiang,et al.Superhydrophobic polysilsesquioxane/poly-styrene microspheres with controllable morphology:from raspberry-like to flower-like structure[J].RSC Advances,2017,7(11):6685-6690. [2] Lee Y G,Park J H,Oh C,et al.Preparation of highly monodispersed hybrid silica spheres using a one-step sol-gel reaction in aqueous solution[J].Langmuir,2007,23(22):10875-10878. [3] Yuan Jinfang,Ma Wenshi,Mo Jinpeng.Fabrication of highly monodisperse CeO2@poly(methyl silsesquioxane) microspheres and their application in UV-shielding films[J].Applied Polymer,2017,134(29):45065-45075. [4] Kim S S,Kim V,Kim Y B.Preparation and characterization of polysilsesquioxane particles containing UV-absorbing groups[J].Macromolecular Research,2012,20(5):437-446. [5] Nagappan S,Ha H M,Park S S,et al.One-pot synthesis of multi-functional magnetite-polysilsesquioxane hybrid nanoparticles for the selective Fe3+ and some heavy metal ions adsorption[J].RSC Advances,2017,7(31):19106-19116. [6] Lee Y G,Park J H,Oh C,et al.Preparation of highly monodispersed hybrid silica spheres using a one-step sol-gel reaction in aqueous solution[J].Langmuir,2007,23(22):10875-108878. [7] Hao Lifen,Yang Ruini,Wang Xuechuan,et al.Progress on synthesis and application of polysissesquioxane micro/nanospheres[J].Fine Chemicals,2017,34(1):1-10. [8] Sankaraiah S,Lee J M,Kim J H,et al.Preparation and characterization of surface-functionalized polysilsesquioxane hard spheres in aqueous medium[J].Macromolecules,2008,41(16):6195-6204. [9] Hao L F,Gao T T,Wang X C,et al.Synthesis and characterization of polyaminopropyl methylsilsesquioxane nanospheres[J].Fine Chemicals,2016,33(7):721-725. [10] Ottenbrite R M,Wall J S,Sidiqui J A.Self-catalyzed synthesis of organo-silica nanoparticels[J].Journal of the American Ceramic Society,2000,83(12):3214-3215. [11] Kim S S,Kim V,Kim Y B.Preparation and characterization of polysilsesquioxane partices containing UV-absorbing groups[J].Macromolecular Research,2012,20(5):437-446. [12] Lee D,Kim Y A,Kim Y B,et al.One step preparation of spherical silicon resins from immiscible reaction mixtures[J].Macromolecular Research,2008,16(4):353-359. [13] Mori H,Sada C,Konno T,et al.Film-forming amphiphilic silsesquioxane hybrids prepared by hydrolytic co-condensation of hydroxyl-functionalized and fluorinated triethoxysilanes[J].Polymer,2012,53(18):3849-3860. [14] Li Z,Tolbert S H,Loy D A.Hybrid organic-inorganic menbrances from size exclusion deposition of fluorescent,octylene-bridged polysilsesquioxane partices[J].Journal of Non-Crystalline Solids,2014,403:88-96.