Trimethylolpropane → Tetraethoxysilane

Participants

Reaction Conditions

Reaction Steps

Non-Fluorinated Masterbatch. To a one liter, three-neck round bottom flask containing dry tetrahydrofuran (THF) (300 mL) under nitrogen was added Terathane™ 2900 polytetramethylene glycol (79.13 g, 0.027 mol), 1,4-butanediol (3.97 g, 0.044 mol), and trimethylolpropane (1.21 g, 0.0090 mol). The mixture was stirred under nitrogen until a solution was obtained; then isophorone diisocyanate (15.69 g, 0.071 mol) was added, and then the mixture was degassed under reduced pressure (0.1 mm Hg). Dibutyltin dilaurate (0.20 g, 0.0003 mol) was added, and the mixture was heated at 60° C. under nitrogen for 5 hours. To the above solution was added 3-isocyanatopropyltriethoxysilane (7.98 g, 0.033 mol) and additional THF (85 mL). The mixture was heated at 60° C. for 15 hours, yielding a solution containing 24 wt % dissolved solids.

Provenance & Evidence