TY - GEN
T1 - Study on synthesis of cyclotriphosphazene containing aminopropylsilicone functional group as flame retardant
AU - He, Lanlan
AU - Zhang, Yi
AU - Qin, Zhaolu
AU - Lan, Yanhua
AU - Li, Dinghua
AU - Yang, Rongjie
PY - 2013
Y1 - 2013
N2 - A novel non-halogen flame retardant APESP, cyclotriphosphazene containing six aminopropyltriethoxysilicone functional groups N3P3 [NH(CH2)3Si(OCH2CH3)3]6, was synthesized by menas of SN2 nucleophilic substitution reaction, using hexachlorocyclotriphosphazene(HCCP) and 3-aminopropyltriethoxy-silane (KH550) as material. Firstly the industrial grade HCCP was purified through recrystallization and sublimation. Then the reaction process was investigated to prompt the yield, and the optimum reaction conditions were as follows: triethylamine as acid-binding agent, tetrahydrofuran as solvent, HCCP/KH550/triethylamine molar ratio 1:7.2:7.2, dripping time: 1 hour, temperature: 67°C and reaction time: 20h. Maximum APESP yield reached 94.3%. The chemical structure and purity was characterized by element analysis, Fourier-transformed infrared spectroscopy (FTIR), mass spectrum, gel permeation chromatography (GPC) and nuclear magnetic resonance (NMR) analysis. The results showed that the structure of synthesized product is consistent with the theoretical structure, in which the chlorine atoms were completely substituted. The charge distribution calculation of HCCP and KH550 confirmed the reaction mechanism.
AB - A novel non-halogen flame retardant APESP, cyclotriphosphazene containing six aminopropyltriethoxysilicone functional groups N3P3 [NH(CH2)3Si(OCH2CH3)3]6, was synthesized by menas of SN2 nucleophilic substitution reaction, using hexachlorocyclotriphosphazene(HCCP) and 3-aminopropyltriethoxy-silane (KH550) as material. Firstly the industrial grade HCCP was purified through recrystallization and sublimation. Then the reaction process was investigated to prompt the yield, and the optimum reaction conditions were as follows: triethylamine as acid-binding agent, tetrahydrofuran as solvent, HCCP/KH550/triethylamine molar ratio 1:7.2:7.2, dripping time: 1 hour, temperature: 67°C and reaction time: 20h. Maximum APESP yield reached 94.3%. The chemical structure and purity was characterized by element analysis, Fourier-transformed infrared spectroscopy (FTIR), mass spectrum, gel permeation chromatography (GPC) and nuclear magnetic resonance (NMR) analysis. The results showed that the structure of synthesized product is consistent with the theoretical structure, in which the chlorine atoms were completely substituted. The charge distribution calculation of HCCP and KH550 confirmed the reaction mechanism.
KW - Cyclotriphosphazene
KW - Flame retardant
KW - Nucleophilic substitution
KW - Purification
UR - http://www.scopus.com/inward/record.url?scp=84878298208&partnerID=8YFLogxK
U2 - 10.4028/www.scientific.net/AMR.683.25
DO - 10.4028/www.scientific.net/AMR.683.25
M3 - Conference contribution
AN - SCOPUS:84878298208
SN - 9783037856666
T3 - Advanced Materials Research
SP - 25
EP - 29
BT - Advanced Materials and Engineering Materials II
T2 - 2nd International Conference on Advanced Materials and Engineering Materials, ICAMEM 2012
Y2 - 29 December 2012 through 30 December 2012
ER -