19090-60-9 → Adipic Acid

Temperature

200 °C

A 300 mL Parr autoclave was charged with 80 g of synthetic monoammonium adipate and 124 g of water. The autoclave was sealed and the contents stirred and heated to about 200° C. (autogenic pressure was about 203 psig). Once the contents reached temperature, water was then fed to the autoclave at a rate of about 2 g/min and vapor was removed from the autoclave at a rate of about 2 g/min with a back pressure regulator. Vapor exiting the autoclave was condensed and collected in a receiver. The autoclave was run under those conditions until a total of 1210 g of water had been fed and a total of 1185 g of distillate collected. The contents of the autoclave (209 g) were partially cooled and discharged from the reactor. The slurry was allowed to stand with stirring at room temperature over night in an Erlenmeyer flask. The slurry was then filtered and the solids rinsed with 25 g of water. The moist solids were dried in a vacuum oven at 75° C. for 1 hr yielding 59 g of adipic acid product. Analysis via an ammonium ion electrode revealed 0.015 mmole ammonium ion/g of solid. The melting point of the recovered solid was 151° C. to 154° C.

1. customThe autoclave was sealed
2. customwas removed from the autoclave at a rate of about 2 g/min with a back pressure regulator
3. customcondensed
4. customcollected in a receiver
5. temperatureThe contents of the autoclave (209 g) were partially cooled
6. stirringwith stirring at room temperature over night in an Erlenmeyer flask
7. filtrationThe slurry was then filtered
8. washthe solids rinsed with 25 g of water
9. customThe moist solids were dried in a vacuum oven at 75° C. for 1 hr

ORD record

ord-f313f6a283e9471bb21860986780b53c

Source dataset

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08703900B2