Ethylene → Ethene;oct-1-ene

HRID 1279675Notes

Reaction equation

HRID 1279675 reaction equation
C=C.[CH2:3]=[CH:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]>C1(C)C=CC=CC=1.CCCCCCC>[CH2:3]=[CH2:4].[CH2:3]=[CH:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]

Participants

5

Procedure

A 260 ml glass autoclave, provided with magnetic stirrer, temperature indicator and feeding line for the ethylene, was purified and fluxed with ethylene at 35° C. At room temperature were introduced 86 ml of heptane and 4.1 ml of 1-octene distilled over LiAlH4. The catalytic system was prepared by consecutively introducing MAO (0.21 mmol. as 1M toluene solution) and 0,1 mg (0.000205 mg.at. Zr) of the metal locene of example 1 solved in toluene (the low amount as possible). After 5 minutes stirring, the solution was diluted to 10 ml with heptane and was introduced into the autoclave under ethylene flow, the reactor was closed, the temperature risen to 70° C. and pressurized to 4 bar. The total pressure was kept constant by feeding ethylene for 20 minutes. The polymerization was stopped by cooling, degassing the reactor and the introduction of 1 ml of methanol. The achieved polymer was washed with acidic methanol, than with methanol and dried in oven at 60° C. under vacuum. 1.68 g. of polymer was obtained (270 Kg/gZr/h) with the following characteristics: I.V.=1.82 dL/g; 1-octene=5.73 mol.%, Tm=92.5° C.; ΔH=63 J/g;

Workup

  1. customwas purified
  2. customfluxed with ethylene at 35° C
  3. additionAt room temperature were introduced 86 ml of heptane and 4.1 ml of 1-octene
  4. distillationdistilled over LiAlH4
  5. customThe catalytic system was prepared by consecutively introducing MAO (0.21 mmol. as 1M toluene solution) and 0,1 mg (0.000205 mg.at. Zr) of the metal locene of example 1
  6. additionwas introduced into the autoclave under ethylene flow
  7. customthe reactor was closed
  8. customrisen to 70° C.
  9. customfor 20 minutes
  10. temperatureby cooling
  11. customdegassing the reactor
  12. washThe achieved polymer was washed with acidic methanol, than with methanol
  13. customdried in oven at 60° C. under vacuum
  14. customof polymer was obtained (270 Kg/gZr/h) with the following characteristics
  15. customTm=92.5° C.

Sources & evidence

ORD record
ord-3815f4dd93dd45aa9082d35782d32c8d
Source dataset
uspto-grants-2002_09
Patent number
US06448350B1

Reaction notes

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