Isopropanol → Benzene, ethenyl-, polymer with 1,3-butadiene

HRID 2208624Notes

Reaction equation

HRID 2208624 reaction equation
[CH2:1]=[CH:2][CH:3]=[CH2:4].C([Li])CCC.[CH2:10]=[CH:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(O)(C)C>CCCCCC>[CH2:10]=[CH:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[CH2:1]=[CH:2][CH:3]=[CH2:4]

Participants

6

Reactant 4

HCID 3776IsopropanolHCID 7501StyreneHCID 78451,3-ButadieneHCID 178418339Butyllithium

Product 1

HCID 62697Benzene, ethenyl-, polymer with 1,3-butadiene

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent5×

Procedure

Under nitrogen to a dry 2-gallon reactor was added 1364 g of hexane, 2410 g of 21.6% butadiene solution in hexane, followed by 3.83 mL of 1.6 M butyl lithium solution in hexane. After the polymerization was carried out for 2 h at 60° C., 3.83 mL of 1.6 M 2,2-bis(2′-tetrahydrofuryl)propane solution in hexane was added to the solution, followed by 278 g of 33.0% styrene solution in hexane. After 1 h, the polymer cement was poured into isopropanol containing BHT and the coagulated polymer was dried by a drum-drier. The molecular weight of the (Bd-b-St block) polymer was determined by GPC. It was found: Mn=101,291; Mw=107,745; Mw/Mn=1.06. The vinyl content is 8.8% (Bd=100%) and the styrene content is 15.1%, both determined by 1H NMR. The vinyl content is based upon Bd being equal to 100%.

Workup

  1. waitAfter 1 h
  2. customthe coagulated polymer was dried by a drum-drier

Sources & evidence

ORD record
ord-db27a9a403764ad8af9b860d1960be05
Source dataset
uspto-grants-2016_06
Patent number
US09376508B2

Reaction notes

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