Hydroquinone → 2,6,6-Trimethyl-3,3-bis(2,6,6-trimethyl-3-bicyclo[3.1.1]hept-1-enyl)bicyclo[3.1.1]hept-1-ene

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

A 1 liter Parr reactor equipped with a mechanical stirrer, bottom drain valve and distillation apparatus, was charged with NDC (111.0 g, 0.453 moles, 0.121 eq), PPG (211.0 g, 2.768 moles, 0.508 eq; excess 0.232 eq), terpinene-maleic anhydride adduct (42 g, 0.180 moles, 0.048 eq), Rosin-Ar (88 g, 0.249 moles, 0.0667 eq), DDSA (118 g, 0.445 moles, 0.119 eq), SA (53.0 g, 0.453 moles, 0.121 eq) followed by 1.0 g of both Fascat 4100 and Vertec AC422 titanium catalyst. About 0.4 g of hydroquinone were added as a free radical scavenger to prevent crosslinking of resin. The reactor was blanketed with nitrogen and the temperature of the reactor was slowly raised to 170° C. with stirring (once the solids melted). The reaction mixture was maintained for 15 hours under nitrogen at 205° C. while methanol was continuously collected in a collection flask. The reaction mixture was heated to 215° C. and low vacuum was applied. A higher vacuum (<0.1 Torr) was applied. During that time, propylene glycol distilled off and when the softening point of the resin reached 97.8° C., the reactor temperature was reduced to 180° C. and the second portion of terpinene-maleic anhydride (14 g, 0.058 moles, 0.0154 eq) was added. The reaction mixture temperature was slowly raised to 225° C. while under high vacuum for another 10 hours until a softening point of 103.5° C. was achieved. The temperature was then lowered to 190° C. and the polymer was discharged onto a polytetrafluoroethylene (Teflon) pan.

Herkunft & Nachweise