Ethylene → ethylene/propylene VNB

HRID 579474Notes

Reaction equation

HRID 579474 reaction equation
[CH:1]([CH:3]1[CH2:8][CH:7]2[CH2:9][CH:4]1[CH:5]=[CH:6]2)=[CH2:2].[CH2:10]([Al](CC(C)C)CC(C)C)[CH:11](C)[CH3:12].[H][H].C=CC.C=C>CCCCCC>[CH2:1]=[CH2:2].[CH2:10]=[CH:11][CH3:12].[CH:1]([CH:3]1[CH2:8][CH:7]2[CH2:9][CH:4]1[CH:5]=[CH:6]2)=[CH2:2]

Participants

7

Reactant 5

HCID 6325EthyleneHCID 8252PropyleneHCID 182735-Vinyl-2-norborneneHCID 16682931TriisobutylaluminumHCID 178418361HCID 178418361, compound

Product 1

HCID 86599654ethylene/propylene VNB

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent2×

Conditions

Temperature
80 °C

Procedure

A 2,000-ml polymerization device fully purged with nitrogen gas was charged with 1,000 ml of dry hexane, 2 ml of 5-vinyl-2-norbornene (VNB), and 0.3 mmol of triisobutylaluminum. After raising the internal temperature of the polymerization device to 80° C., hydrogen (5 NmL) was introduced. Propylene was supplied into the polymerization device so that the system pressure was raised to 0.25 MPa. Subsequently, ethylene was supplied into the polymerization device so that the system pressure was 0.8 MPa. A hexane solution containing 0.001 mmol of (t-butylamide)dimethyl(tetramethyl-η5-cyclopentadienyl)silane titaniumdichloride and 0.005 mml of triphenylcarbenium(tetrakispentafluorophenyl)borate was added in the polymerization device. With maintaining the internal temperature of the polymerization device at 80° C. and system pressure at 0.8 MPa, polymerization was allowed to take place for 10 minutes. Polymerization reactions were quenched by the addition of 2 ml methanol. After the pressure was released, a polymer was precipitated from the polymerization solution in 2 L of methanol, and the precipitated polymer was dried in vacuo at 130° C. for 12 hours to afford 50 g of ethylene/propylene/5-vinyl-2-norbornene copolymer. Physical properties of the copolymer are set forth in Table 1.

Workup

  1. customA 2,000-ml polymerization device
  2. customfully purged with nitrogen gas
  3. temperaturewas raised to 0.25 MPa
  4. additionwas added in the polymerization device
  5. temperatureWith maintaining the internal temperature of the polymerization device at 80° C.
  6. customsystem pressure at 0.8 MPa, polymerization
  7. customfor 10 minutes
  8. customPolymerization reactions
  9. customwere quenched by the addition of 2 ml methanol
  10. customa polymer was precipitated from the polymerization solution in 2 L of methanol
  11. customthe precipitated polymer was dried in vacuo at 130° C. for 12 hours

Sources & evidence

ORD record
ord-80cc84443b0344ceae9d685f230daca8
Source dataset
uspto-grants-2015_05
Patent number
US09040811B2

Reaction notes

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