반응 #1829954

ord-74ef643bc01f489b9e418865a576799e

반응 방정식

O=C1COC(=O)CO1
Glycolide
O=C1OCCCO1
Trimethylene carbonate
CCCCC(CC)C(=O)[O-].CCCCC(CC)C(=O)[O-].[Sn+2]
stannous octoate
C[C@@H]1OC(=O)[C@H](C)OC1=O
l-Lactide
C[C@@H]1OC(=O)[C@H](C)OC1=O.O=C1COC(=O)CO1.O=C1OCCCO1
l-LACTIDE GLYCOLIDE TRIMETHYLENE CARBONATE

반응 조건

온도
200°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe mixture was charged into a nitrogen
  2. 2
    기타purged
  3. 3
    workup.STIRRINGThe contents were stirred at this temperature for 25 minutes, at which point the mixture
  4. 4
    기타had obtained maximum
  5. 5
    workup.ADDITIONcharged into the reactor
  6. 6
    workup.STIRRINGThe contents were stirred at 200° C. for 2 hours at which point the mixture
  7. 7
    기타dried in a vacuum oven at 100° C.
  8. 8
    기타measured at 30° C. on a 0.5% solution

실험 절차

Trimethylene carbonate (TMC, 34.0 grams), diethylene glycol (DEG, 17.7 mg) and stannous octoate (20.2 mg) were combined and melted under a nitrogen atmosphere. The mixture was charged into a nitrogen purged stirred reactor at 200° C. The contents were stirred at this temperature for 25 minutes, at which point the mixture had obtained maximum melt viscosity. l-Lactide (l-Lac, 168.7 grams) and Glycolide (Gly, 18.7 grams) were melted and charged into the reactor. The contents were stirred at 200° C. for 2 hours at which point the mixture had again obtained maximum melt viscosity. The polymer was discharged from the reactor, ground, and dried in a vacuum oven at 100° C. and 0.2 mm Hg. The polymer had an inherent viscosity of 1.31 dl/g in chloroform, measured at 30° C. on a 0.5% solution. The polymer composition, as measured by 1H-NMR spectroscopy was 15.9/75.1/9.0 weight percent TMC/l-LAC/Gly.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05342395uspto-grants-1994_08