Toluene → Ethylene styrene

HRID 1739534Notes

Reaction equation

HRID 1739534 reaction equation
[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[H][H].C=C.C1(C)C=CC=CC=1.C[Al]1CCCCO1>>[CH2:1]=[CH2:2].[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

Participants

6

Reactant 5

HCID 1140TolueneHCID 6325Ethylene2×HCID 7501StyreneHCID 23511181MethylalumoxaneHCID 178418361HCID 178418361, compound

Product 1

HCID 22558332Ethylene styrene

Procedure

A two-liter Parr reactor is charged with approximately 360 g of Isopar-E™ mixed alkanes solvent (available from Exxon Chemicals Inc.) and about 460 g of styrene comonomer. Hydrogen is added as a molecular weight control agent by differential pressure expansion from a 75 mL addition tank at 25 psid (2070 kPa). The reactor is heated to 90° C. and saturated with ethylene at 200 psig (1.4 MPa). The appropriate amount of catalyst and cocatalyst (trispentafluorophenylborane) as 0.005 M solutions in toluene (approximately 2 μmole) are premixed in the drybox to give a 1:1 molar ratio of catalyst and cocatalyst. (Excepting for run 3 where the cocatalyst was methylalumoxane in a ratio Al:Ti of 1000:1.) After the desired premix time, the solution is transferred to a catalyst addition tank and injected into the reactor. The polymerization conditions are maintained for 30 minutes with ethylene on demand. Additional quantities of premixed catalyst are added periodically. The resulting solution is removed from the reactor, quenched with isopropyl alcohol and a hindered phenol antioxidant (Irganox™ 1010 from Ciba Geigy Corporation) is added to the resulting solution. Polymers formed are dried in a vacuum oven set at 135° C. for about 20 hours. Results using the catalysts of the invention are shown in Table 1.

Workup

  1. additionA two-liter Parr reactor is charged with approximately 360 g of Isopar-E™
  2. customto give a 1
  3. addition) After the desired premix time
  4. additionthe solution is transferred to a catalyst addition tank
  5. customThe polymerization conditions
  6. additionAdditional quantities of premixed catalyst are added periodically
  7. customThe resulting solution is removed from the reactor
  8. customquenched with isopropyl alcohol
  9. additiona hindered phenol antioxidant (Irganox™ 1010 from Ciba Geigy Corporation) is added to the resulting solution
  10. customPolymers formed
  11. customare dried in a vacuum oven
  12. customResults

Sources & evidence

ORD record
ord-f8b1f8510e1640ab9840d2bebc13ca06
Source dataset
uspto-grants-1999_10
Patent number
US05965756

Reaction notes

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