Propylene Oxide → HCID 86744912, compound

Temperature

90 °C

The one-liter reactor described in Example 1 was charged with a 480 molecular weight poly(propylene oxide) triol initiator (78.9 g), zinc hexacyanocobaltate/zinc chloride/glyme/water catalyst (0.575 g, 1000 ppm), and tetrahydrofuran (60 mL). The load cell was charged with a mixture of ε-caprolactone (140 g) and propylene oxide (357 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 the ε-caprolactone/PO mixture 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 remainder of the ε-caprolactone/PO mixture was added over about a 10-hour period. The product was heated for an additional 8 hours at 90° C. following addition of the monomer mixture, then 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 triol product had a hydroxyl number of 51.0 mg KOH/g and a GPC number average molecular weight of 2980.

1. customThe reactor was purged several times with nitrogen
2. additionAn initial charge of 37 g of the ε-caprolactone/PO mixture
3. additionwas added to the reactor
4. additionafter addition of the
5. additioninitial charge
6. additionThe remainder of the ε-caprolactone/PO mixture 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 monomer mixture
9. temperaturecooled
10. filtrationfiltered through diatomaceous earth
11. customTetrahydrofuran was removed
12. customa rotary evaporator
13. customResidual ε-caprolactone was removed
14. customthrough a wiped-film evaporator under vacuum at 150° C

ORD record

ord-089c57043a6a413a8725066ee5f3c339

Source dataset

uspto-grants-1991_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05032671