Glycerol → Aluminum isopropoxide

Into the shell of a 500 ml Autoclave Engineers reactor are placed 90 g of a propoxylate of glycerin that has an average molecular weight of 260 (Voranol® CP230-660, The Dow Chemical Company). This polyol is a mixture of propoxylates having molecular weights from 150 to 614, and contains 2% by weight glycerin. 3.6 microliters of a 0.15 M phosphoric acid solution in water and 100 parts per million, based on the expected mass of the product, of the Arcol 3 catalyst are added. 0.0075 mole of aluminum isopropoxide/gram of DMC catalyst complex (enough to provide 20 parts per million aluminum based on the expected mass of the product) is added and stirred in. The shell of the reactor is then placed on the reactor frame, and the reaction mixture is stirred and heated at a temperature of 145° C. for 90 minutes with a slow purge of nitrogen (0.5 standard cubic feet per hour) passing through the reactor contents. The reactor contents are heated to 140° C., and, while maintaining that temperature, enough PO is introduced into the reactor to produce an internal reactor pressure of 20.5+/−0.5 psig (141±3.49 kPa), at which time the reactor is sealed. The pressure inside the reactor is monitored. The amount of time (153 minutes) required for internal reaction pressure to decline to about 10.25 psig (70.5 kPa) is recorded as the time to catalyst activation. Still maintaining a temperature of 140° C., a PO feed is introduced into the reactor, at a rate sufficient to maintain an internal reactor pressure of 27±3 psig (186±20.7 kPa). This feed is continued until a total of 76.6 mL (65.8) g of PO (including the initial PO charge) has been fed into the reactor. The time required to complete the PO feed after the catalyst has become activated is 5 hrs and 17 minutes. After all the PO has been fed into the reactor, the reaction mixture is cooked down at 140° C. for 88 minutes, until a steady internal reactor pressure (indicative of complete polymerization of the charged PO) is achieved. A 450 number average molecular weight product is obtained having a polydispersity of 1.1.

1. additiona mixture of propoxylates
2. additionof the Arcol 3 catalyst are added

ORD record

ord-13705167f7ed4b12adbee00128078b1c

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09040657B2