N-vinyl-2-pyrrolidone → Acrylic Acid

Temperature

65 °C

Into a 1-liter, four-necked glass kettle, equipped with 2 feeding pumps an anchor agitator, a thermocouple and a condenser, was charged 300 g of CERAPHYL 494 (iso-cetyl stearate) and 60 g of hexylene glycol and heated to 65° C. for 30 minutes. The solution was purged with nitrogen throughout the ensuing reaction process. T-butylperoxypivalate was added as well as a mixture of 15 g of methyl methacrylate, 36.75 g of butyl methacrylate, 32.25 of stearyl methacrylate and 0.2 g PETE was added to the kettle over a period of 3 hours. The resulting solution was held at 65° C. for 1 hour and then heated to 90° C. Five times every 2 hours, 0.1 g of the initiator was added and the resulting solution was held at 90° C. for 2 additional hours after the last initiator charge. The resulting crosslinked acrylate polymer mixture was then cooled to 65° C. and Solution I of 50 g of vinylpyrrolidone and Solution II of 50 g of acrylic acid were prepared and fed into the kettle at a constasnt rate over a 4 hour period. The resulting solution was held at 65° C. for 1 hour before raising the temperature to 80° C. T-butylperoxypivalate (0.1 g) was added 4 times every 2 hours. The resulting solution containing the polymeric, crosslinked methacrylate polymer network penetrated with the vinyl pyrrolidone polymer was held for an additional 2 hours after which 1 g of water was added and stirred for another 5 hours at 100° C. and then cooled and a homogenized product was recovered.

1. customInto a 1-liter, four-necked glass kettle, equipped with 2 feeding pumps an anchor agitator
2. customThe solution was purged with nitrogen throughout the ensuing reaction process
3. additionT-butylperoxypivalate was added as
4. additionwell as a mixture of 15 g of methyl methacrylate, 36.75 g of butyl methacrylate, 32.25 of stearyl methacrylate and 0.2 g PETE
5. additionwas added to the kettle over a period of 3 hours
6. temperatureheated to 90° C
7. additionFive times every 2 hours, 0.1 g of the initiator was added
8. customwas held at 90° C. for 2 additional hours
9. additioncharge
10. temperatureThe resulting crosslinked acrylate polymer mixture was then cooled to 65° C.
11. waitfed into the kettle at a constasnt rate over a 4 hour period
12. waitThe resulting solution was held at 65° C. for 1 hour
13. temperaturebefore raising the temperature to 80° C
14. waitwas held for an additional 2 hours
15. temperaturecooled
16. customa homogenized product was recovered

ORD record

ord-55aaaac361d14394b1a77a899decd01d

Source dataset

uspto-grants-2008_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07371369B2