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The Synthetical Research of Polyhedral Oligomeric Silsesquioxane (POSS) and POSS/Polymer

Author: LiuXueYing
Tutor: MaJiaJu；WangBin
School: Anhui University of Technology
Course: Applied Chemistry
Keywords: Cage silsesquioxane (POSS) POSS / PMMA composite Atom transfer radical polymerization (ATRP) Synthesis
CLC: TQ320.7
Type: Master's thesis
Year: 2011
Downloads: 181
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Abstract


Polyhedral oligomeric silsesquioxane (Polyhedral oligomeric silsesquioxane, referred POSS) is a kind of novel nanoscale organic - inorganic hybrid structure of the compounds, which consists of Si-O-Si short-chain a 3D hexahedron inorganic framework and the cover It is composed of an organic substituent, cage-type structure having a symmetrical molecular design and easy to carry. According to the vertices of different organic substituent groups, the POSS into the polymer system, the polymer can, after the thermal properties, mechanical properties, mechanical strength, flame resistance, anti-oxidation performance is improved, therefore, the development of new POSS and POSS-based polymer hybrid materials has important theoretical significance and practical value. In this thesis, direct hydrolysis of silane condensation process, an eight chloropropyl successfully synthesized cage silsesquioxane (POSS), discuss the product yield and the relationship between reaction conditions, and the structure of the product was characterized; addition, there were also prepared POSS / PMMA composite particles, and its structure and thermal properties were characterized. Main work as follows: 1, Y-chloropropyl trimethoxy silane as the raw material, methanol as a solvent, hydrochloric acid as a catalyst, direct use of silane hydrolysis condensation method of synthesis of an eight chloropropyl silsesquioxane cage ( POSS). Of reaction time, temperature, reactant feed ratio on the yield of the product, the preferred synthetic product explore the reaction conditions: temperature maintained at 40 ℃, continuing the reaction for 15 days, were put in γ-chloropropyl trimethoxy silane, preferably concentrated hydrochloric acid and methanol feed volume ratio of 20:15:400, the highest yield of 37%. 2, eight of the synthesized product chloropropyl cage silsesquioxane (POSS) structures for infrared spectroscopy (FTIR), X-ray diffraction (XRD), nuclear magnetic resonance (1HNMR, 29SiNMR) and gel permeation chromatography (GPC) characterization. Test results showed that: the synthesized chloropropyl POSS cage symmetrical structure with high purity. 3, using atom transfer radical polymerization (ATRP) method to synthesize eight chloropropyl POSS cage as initiator, prepared POSS / PMMA composites discussed amount of initiator, reaction time, temperature of the product yield effects. Infrared spectroscopy (FTIR), X-ray diffraction (XRD), nuclear magnetic resonance (1HNMR) and gel permeation chromatography (GPC) to characterize the structure of the product, and use thermal analysis (DSC, TGA) was studied after the introduction of the polymerization POSS Thermal properties of matter. Test results showed that: Preparation of POSS / PMMA polymer, POSS content of 5% and 10%, POSS / PMMA composite glass transition temperature (Tg) than pure PMMA glass transition temperature (Tg) were increased by 12.8 ℃ and 22.6 ℃, TGA and DTG results showed: POSS content of 5% and 10%, POSS / PMMA composites decomposition temperature (Td) than pure PMMA decomposition temperature (Td) were increased by 24.4 ℃ and 40.1 ℃. Figure [24] Table [7] parameter [66]

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