Propylene Oxide → HCID 86744912, compound

Temperature

90 °C

The one-liter reactor previously described was charged with a 480 molecular weight poly(propylene oxide) triol (78.9 g), zinc hexacyanocobaltate/zinc chloride/glyme/water catalyst (0.575 g, 980 ppm), and tetrahydrofuran (60 mL). The load-cell reservoir was charged with propylene oxide (341 g). The reactor was purged several times with nitrogen, then pressurized to about 5 psi. The reactor contents were stirred and heated to 90° C. over a 1.5 hour period. An initial charge of 37 g of PO was added to the reactor. A pressure drop was observed about 1 hour after addition of the initial charge, indicating that initiation of the catalyst had occurred. The remaining PO was added over about a 10-hour period. The product was heated for an additional 8 hours at 90° C. following addition of the propylene oxide. ε-Caprolactone (165 g was charged to the load-cell reservoir, and was added to the reactor at 90° C. at a rate of about 40 g/hour. The product was heated for an additional 8 hours at 90° C. following addition of the ε-caprolactone. The product was cooled, drained from the reactor, and filtered through diatomaceous earth. Tetrahydrofuran was removed using a rotary evaporator. Residual ε-caprolactone was removed by passing the polymer product through a wiped-film evaporator under vacuum at 150° C. The ε-caprolactone-capped poly(PO) triol product had a hydroxyl number of 60.5 mg KOH/g and a GPC number average molecular weight of 2410.

1. customThe reactor was purged several times with nitrogen
2. additionAn initial charge of 37 g of PO
3. additionwas added to the reactor
4. additionafter addition of the
5. additioninitial charge
6. additionThe remaining PO was added over about a 10-hour period
7. temperatureThe product was heated for an additional 8 hours at 90° C.
8. additionaddition of the propylene oxide
9. additionε-Caprolactone (165 g was charged to the load-cell reservoir
10. additionwas added to the reactor at 90° C. at a rate of about 40 g/hour
11. temperatureThe product was heated for an additional 8 hours at 90° C.
12. additionaddition of the ε-caprolactone
13. temperatureThe product was cooled
14. filtrationfiltered through diatomaceous earth
15. customTetrahydrofuran was removed
16. customa rotary evaporator
17. customResidual ε-caprolactone was removed
18. customthrough a wiped-film evaporator under vacuum at 150° C
19. customThe ε-caprolactone-capped poly(PO) triol product

ORD record

ord-3cc43190cb684abebb20d0cc8ff1113d

Source dataset

uspto-grants-1991_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05032671