Ethylene → Ethylene styrene
Reaction equation
[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C=C.F[C:12]1C(B(C2C(F)=C(F)C(F)=C(F)C=2F)C2C(F)=C(F)C(F)=C(F)C=2F)=C(F)C(F)=C(F)[C:13]=1F.[H][H]>[Ti].CCC(C)C.C1CCCCC1>[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH2:12]=[CH2:13]Participants
Procedure
Polymer is prepared in a 400 gallon (1500 L) agitated semi-continuous batch reactor, utilizing the process conditions set forth in the following Table Two. The reaction mixture consisted of approximately 250 gallons (950 L) of a solvent comprising a mixture of cyclohexane (85 weight percent) and isopentane (15 weight percent), and styrene. Prior to addition, solvent, styrene and ethylene are purified to remove water and oxygen. The inhibitor in the styrene is also removed. Inserts are removed by purging the vessel with ethylene. The vessel is then pressure controlled to a set point with ethylene. Hydrogen is added to control molecular weight. Temperature in the vessel is controlled to set-point by varying the jacket water temperature on the vessel. Prior to polymerization, the vessel is heated to the desired run temperature and the catalyst components: Titanium: (N-1,1-dimethylethyl)dimethyl(1-(1,2,3,4,5-eta)-2,3,4,5-tetramethyl-2,4-cyclopentadien-1-yl)silanaminato))(2-)N)-dimethyl, CAS# 135072-62-7, Tris(pentafluorophenyl)boron, CAS# 001109-15-5, Modified methylaluminoxane Type 3A, CAS# 146905-79-5, are flow controlled, on a mole ratio basis of 1/3/5 respectively, combined and added to the vessel. After starting, the polymerization is allowed to proceed with ethylene supplied to the reactor as required to maintain vessel pressure. In some cases, hydrogen is added to the headspace of the reactor to maintain a mole ratio with respect to the ethylene concentration. At the end of the run, the catalyst flow is stopped, ethylene is removed from the reactor, about 1000 ppm of Irganox* 1010 antioxidant is then added to the solution and the polymer is isolated from the solution. The resulting polymers are isolated from solution by either stripping by use of a devolatilizing extruder.
Workup
- customPolymer is prepared in a 400 gallon (1500 L)
- customare purified
- customto remove water and oxygen
- customThe inhibitor in the styrene is also removed
- customInserts are removed
- customby purging the vessel with ethylene
- additionHydrogen is added
- customPrior to polymerization
- temperaturethe vessel is heated to the desired run temperature
- additionadded to the vessel
- temperatureto maintain vessel pressure
- temperatureto maintain a mole ratio with respect
- concentrationto the ethylene concentration
- customethylene is removed from the reactor, about 1000 ppm of Irganox* 1010 antioxidant
- additionis then added to the solution
- customthe polymer is isolated from the solution
- customThe resulting polymers are isolated from solution by either stripping by use of a devolatilizing extruder
Sources & evidence
- ORD record
- ord-63fe2711ac124e1cbfcb2197795606e7
- Source dataset
- uspto-grants-2002_02
- Patent number
- US06344515B1
Reaction notes
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