反应详情

A 2/1 molar ratio of 5,6-dimethyl-2-norbornene to dicyclopentadiene was used to prepare the 5,6-dimethyl-2-norbornene/1-hexene/dicyclopentadiene copolymer of example 13. 500 ml dry benzene cosolvent, 25.7 ml dicyclopentadiene solution (90 wt.% in dry benzene), 46.5 ml 5,6-dimethyl-2-norbornene, 10 ml of the 1-hexene solution, and 6 ml of the diethylaluminum iodide solution were charged to a dry, nitrogen-purged quart bottle. 7.5 ml of the MoCl5 solution was charged last with shaking. Polymerization occurred rapidly, and after 1 hour the reaction was cooled to room temperature and shortstopped with 1 ml ethanolamine and 3 ml Solution A. 12 ml of an antioxidant solution was also added (0.1 g/ml of Ethyl 712 in benzene; Ethyl 712 is 4,4-bis[2,6-di-t-butylphenol]). A polymer cement was coagulated using excess Solution A in a Waring blender. The polymer was filtered and vacuum dried at 60° C. It weighed 60.5 grams after drying and was a solid, ring-opened 5,6-dimethyl-2-norbornene/1-hexene-dicyclopentadiene copolymer having a DSV of about 1.37. 5,6-dimethyl-2-norbornene/1-hexane/dicyclopentadiene copolymers were prepared by the above method with 1/1 (example 14) and 1/2 (example 15) dimethylnorbornene/DCPD molar ratios using the following recipes respectively:

1. custompurged quart bottle
2. addition7.5 ml of the MoCl5 solution was charged last
3. customPolymerization
4. filtrationThe polymer was filtered
5. customvacuum dried at 60° C
6. customafter drying