Isopropanol → HCID 86755407, compound

Temperature

70 °C

To a 15-liter autoclave vacuum dried and purged with nitrogen, 887 g of norbornene, 1,100 ml of styrene, 777 ml of cyclohexane and 3 ml of a cyclohexane solution of triisobutylaluminum (1 mmol/ml) were introduced at ambient temperature. The autoclave was pressurized up to 6 kg/cm2 -G with ethylene while stirring, and then the pressure was released. The operations of pressurizing and pressure release were repeated three times. Thereafter, the system was pressurized to 1.5 kg/cm2 -G with ethylene, and the temperature was raised to 70° C. The system was then pressurized with ethylene so that the internal pressure became 6 kg/cm2 -G. After stirring for 15 minutes, 13.7 ml of the catalyst solution previously prepared was added to the system to initiate copolymerization of ethylene and norbornene. With respect to the catalyst concentration at this time, the concentration of the isopropylidene-bis(indenyl)zirconium dichloride in the whole system was 0.0123 mmol/l, and the concentration of the methylaluminoxane in the whole system was 7.5 mmol/l. During the polymerization, ethylene was continuously fed to maintain the internal pressure at 6 kg/cm2 -G. After 60 minutes, isopropyl alcohol was added to terminate the polymerization reaction. After the pressure was released, the polymer solution was drawn out and washed with an aqueous solution of 5 ml of concentrated hydrochloric acid in 1 liter of water in a ratio between the polymer solution and the aqueous solution of 1:1, to transfer the catalyst residue into the aqueous phase. This contact mixed solution was allowed to stand, then the aqueous phase was removed by separation, and the remainder was further washed twice with distilled water to separate the polymerization liquid phase into an oil portion and an aqueous portion. The oil portion was brought into contact with acetone in an amount 3 times as much as the oil portion with vigorous stirring to precipitate a polymer and then sufficiently washed with acetone. The resulting solid portion (copolymer) was collected by filtration and dried at 130° C. and 350 mmHg for 12 hours in a stream of nitrogen. Thus, an ethylene/norbornene/styrene copolymer was obtained in a yield of 240 g, and the copolymer had an intrinsic viscosity [η], as measured in a decalin solvent at 135° C., of 0.8 dl/g, a glass transition temperature (Tg) of 142° C., a norbornene content of 41.1% by mol, a styrene content of 9.8% by mol and an activity of 6,500 g/mmol-Zr.

1. customTo a 15-liter autoclave vacuum dried
2. custompurged with nitrogen, 887 g of norbornene, 1,100 ml of styrene, 777 ml of cyclohexane and 3 ml of a cyclohexane solution of triisobutylaluminum (1 mmol/ml)
3. additionwere introduced at ambient temperature
4. stirringAfter stirring for 15 minutes
5. custom13.7 ml of the catalyst solution previously prepared
6. additionwas added to the system
7. concentrationWith respect to the catalyst concentration at this time
8. customDuring the polymerization, ethylene
9. temperatureto maintain the internal pressure at 6 kg/cm2 -G
10. customto terminate
11. customthe polymerization reaction
12. washwashed with an aqueous solution of 5 ml of concentrated hydrochloric acid in 1 liter of water in a ratio between the polymer solution
13. additionThis contact mixed solution
14. customthe aqueous phase was removed by separation
15. washthe remainder was further washed twice with distilled water
16. customto separate
17. customthe polymerization liquid phase into an oil portion
18. stirringwith vigorous stirring
19. customto precipitate a polymer
20. washsufficiently washed with acetone
21. filtrationThe resulting solid portion (copolymer) was collected by filtration
22. customdried at 130° C.
23. wait350 mmHg for 12 hours in a stream of nitrogen

ORD record

ord-a73d2cf7681b43329406cbee3fac7411

Source dataset

uspto-grants-2000_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06063886