Propylene → HCID 22386386, compound

A reaction vessel equipped with a mechanical stirrer, reflux condenser, and temperature control was dried and filled with nitrogen. The vessel was charged with 400 g of 1-hexene (from Ethyl Corp.), the temperature was adjusted to 25° C., and hydrogen (Oxygen Services ultra high purity) bubbled in at a rate of about 60 mL/min. 2.2 nL of a 1.8M solution of diethylaluminum chloride (from Aldrich Chemical Co.) was added followed by the addition of 0.4 g AATiCl3 and immediately propylene was bubbled into the reaction mixture at about 60 mL/min for 30 minutes. Methanol (20 mL) was added to terminate the polymerization and the polymer precipitated in excess methanol to extract the catalyst residues. A tacky amorphous polymer was obtained in 72% conversion having an inherent viscosity of 5.7 dL/g in n-hexane and a Tg of -32° C. 3C NMR analysis indicated that the polymer contained 87 mole percent of 1-hexene and 13 mole percent of propylene.

1. customA reaction vessel equipped with a mechanical stirrer
2. temperaturereflux condenser
3. customtemperature control was dried
4. additionfilled with nitrogen
5. additionThe vessel was charged with 400 g of 1-hexene (from Ethyl Corp.)
6. customwas adjusted to 25° C.
7. customhydrogen (Oxygen Services ultra high purity) bubbled in at a rate of about 60 mL/min
8. addition2.2 nL of a 1.8M solution of diethylaluminum chloride (from Aldrich Chemical Co.) was added
9. additionfollowed by the addition of 0.4 g AATiCl3
10. customimmediately propylene was bubbled into the reaction mixture at about 60 mL/min for 30 minutes
11. additionMethanol (20 mL) was added
12. customto terminate
13. customthe polymerization
14. customthe polymer precipitated in excess methanol
15. extractionto extract the catalyst residues
16. customA tacky amorphous polymer was obtained in 72% conversion

ORD record

ord-fefb83c532d34ebf8baa8b98eee21627

Source dataset

uspto-grants-1999_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05859088