Trimethylolpropane → Tetraethoxysilane

Participants

Reaction Conditions

Reaction Steps

5 wt % Fluorinated Masterbatch. To a 500 mL, three-neck round bottom flask containing dry tetrahydrofuran (THF) (150 mL) under nitrogen was added Terathane™ 650 polytetramethylene glycol (20.62 g, 0.032 mol), 1,4-butanediol (4.50 g, 0.050 mol), Polyfox™ PF-6320 (2.84 g, 0.0008 mol) and trimethylolpropane (1.38 g, 0.010 mol). The mixture was stirred under nitrogen until a solution was obtained; then isophorone diisocyanate (20.66 g, 0.093 mol) was added, and then the mixture was degassed under reduced pressure (0.1 mm Hg). Dibutyltin dilaurate (0.10 g, 0.0002 mol) was added, and the mixture was heated at 60° C. under nitrogen for 5 hours. To the above solution was added 3-isocyanatopropyltriethoxysilane (2.11 g, 0.0085 mol) and additional THF (35 mL). The mixture was heated at 60° C. for 15 hours, yielding a solution containing 24 wt % dissolved solids.

Provenance & Evidence