1,4-Butanediol → Phenyl isocyanate

Participants

Reaction Conditions

Reaction Steps

In a 1 liter three-necked resin flask equipped with nitrogen inlet and outlet, thermometer, condenser and mechanical stirrer, were placed 194 grams (1 moles) of dimethyl terephthalate, 207 grams (2.3 moles) of 1,4-butanediol and 0.173 grams of titanium tetraisopropoxide. The mixture was heated at 210° C. for 2 hours while distilling out methanol. The resulting mixture was heated at 250° C. for 30 minutes, and then vacuum was applied for 3 hours. After vacuum was released and replaced with nitrogen, 2,4-toluenediisocyanate (5.48 grams, 0.0314 moles) was added into the flask. The resulting polymer was stirred for 10 minutes at 250° C., and then was cooled to room temperature to obtain phenyl isocyanate terminated copolyester with an intermediate molecular weight, I.V. 1.98 dL/g as determined at 25° C. and 0.1% concentration in HFIP/PFP 50/50; Tmp 220° C.; heat of fusion 37 j/g; Tg 47° C.

Provenance & Evidence