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Ring‐opening metathesis polymerization of tetracyclododecene using various catalyst systems
Author(s) -
Kim Jaehoon,
Wu Chun Ji,
Kim WanJoo,
Kim Junhyuk,
Lee Hyunjoo,
Kim JaeDuck
Publication year - 2009
Publication title -
journal of applied polymer science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.575
H-Index - 166
eISSN - 1097-4628
pISSN - 0021-8995
DOI - 10.1002/app.31557
Subject(s) - romp , polymerization , ring opening metathesis polymerisation , polymer chemistry , catalysis , materials science , norbornene , polymer , metathesis , chemistry , organic chemistry , composite material
Ring‐opening metathesis polymerization (ROMP) of a polycyclic olefin monomer (tetracyclododecene, TCD) was carried out using various catalyst systems. The catalysts included titanium‐based ternary system (titanium tetrachloride, TiCl 4 /triethylaluminum, Et 3 Al/triethylamine, Et 3 N), tungsten‐based ternary system (tungsten hexachloride, WCl 6 /triisobutyl aluminum, (i‐Bu) 3 Al/ethanol), and a ruthenium benzylidene catalyst (Grubbs 1st catalyst). The Grubbs 1st catalyst was most active in ROMP of TCD. The tungsten‐based catalyst was found to be more active than the titanium‐based catalyst. In contrast to the titanium‐based and the Grubbs 1st catalysts, ROMP of TCD with the tungsten‐based catalyst was very sensitive to gelation in the course of reaction. The effects of ethanol, WCl 6 concentration, TCD/WCl 6 ratio, and 1‐hexane on the polymerization yield and the polymer gel formation were investigated in detail, and optimized ROMP conditions were determined. Chemical structure of synthesized polymer was characterized using one‐ and two‐dimensional 150 MHz 13 C and 600 MHz 1 H nuclear magnetic resonance spectroscopy, molecular weights were measured using gel‐permeation chromatography, and thermal properties were characterized using differential scanning calorimetry. Number‐average molecular weights ( M n ) of the polymer were in the range of 1.5–4.7 × 10 4 g/mol, and glass transition temperatures were in the range of 185–220°C. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010