Ethylene → Ethylene Vinylethylene Carbonate

Temperature

23 °C

Upon removal from the glove box, the flask was evacuated and backfilled with ethylene. The catalyst was dissolved in CH2Cl2 (25 mL) and immediately treated with vinyl ethylene carbonate (5 mL). The resulting orange solution was stirred at 23° C. under an ethylene atmosphere (1 atm) for 20 hours. A small amount of polymer had precipitated out of solution. The polymerization was quenched with MeOH and acetone leaving gray oil adhering to the walls of the flask. The polymer was washed several times with acetone and MeOH to remove any remaining monomer. The polymer was dissolved in CH2Cl2 and transferred to a storage jar. The solvent was left to evaporate and the resulting oily polymer was dried in vacuo at ~80° C. for 3 days to afford a tacky solid (2.15 g, 1100 TO). 1H NMR was consistent with a copolymer containing approximately 96.5 weight % ethylene and 3.5 weight % vinyl ethylene carbonate monomer units.; Mn 40,000 g /mol ; Mw 92,000 g /mol ; DSC Tg -68° C., Tm -38° C.

1. customUpon removal from the glove box
2. customthe flask was evacuated
3. dissolutionThe catalyst was dissolved in CH2Cl2 (25 mL)
4. additionimmediately treated with vinyl ethylene carbonate (5 mL)
5. customA small amount of polymer had precipitated out of solution
6. customThe polymerization was quenched with MeOH and acetone leaving gray oil adhering to the walls of the flask
7. washThe polymer was washed several times with acetone and MeOH
8. customto remove any remaining monomer
9. dissolutionThe polymer was dissolved in CH2Cl2
10. waitThe solvent was left
11. customto evaporate
12. customthe resulting oily polymer was dried in vacuo at ~80° C. for 3 days
13. customto afford a tacky solid (2.15 g, 1100 TO)
14. customDSC Tg -68° C., Tm -38° C.

ORD record

ord-6e03554d938c40939e9e43ff58be5b76

Source dataset

uspto-grants-2000_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06090900