Reaction equation
C[C@H:2]1[CH2:30][O:29][C@@:5]2(O[C@H:8]3[CH2:10][C@H:11]4[C@@H]5CC=C6C[C@@H](O)CC[C@]6(C)[C@H]5CC[C@:12]4(C)[C@H:7]3[C@@H:6]2C)[CH2:4][CH2:3]1.[OH-].[K+].C(OCC(CC)CCCC)C1[O:36]C1>C1(C)C=CC=CC=1>[CH2:6]([CH:5]([O:29][CH2:30][CH3:2])[CH:4]1[O:36][CH2:3]1)[CH2:7][CH2:8][CH2:10][CH2:11][CH3:12]Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 60 °C
Procedure
In a 250 mL, round bottom 3-neck flask equipped with a condenser, a nitrogen in/out let, a mechanical stirrer, a thermo-watch, and a heating mantle, a mixture of 30 g of 35,000 Mw PEG and toluene (80 mL) was heated to 60° C. At this temperature, KOH (0.77 g, 0.02 mol, in 1 g of water) was added and the reaction mixture was stirred for 1 hour. 2-Ethyl hexyl glycidyl ether (1.91 g, 0.02 mole) was added and the reaction temperature was kept at 110° C. for 5 hours. After the reaction mass was cooled to 60° C., toluene (80 mL) was further added. The solution was precipitated into 300 mL of hexane. After filtration and washing with ethyl acetate (100 mL×3×) and drying in vacuum, a white polymer (31 g) was obtained. 1H NMR showed 5.2% hydrophobe incorporation. The Brookfield viscosity of a 5% aqueous solution of this oligomer was >200,000 cps (BF LV, S-63, 0.3 rpm at 25° C.). Paint performance: SG10 M (standard formulation). TE %=0.11, Viscosity Loss upon Tinting (VLT)=−24 KU. For UCAR 379 G, TE %=0.28, VLT=−30 KU.
Workup
- customIn a 250 mL, round bottom 3-neck flask equipped with a condenser
- waitthe reaction temperature was kept at 110° C. for 5 hours
- temperatureAfter the reaction mass was cooled to 60° C.
- customThe solution was precipitated into 300 mL of hexane
- filtrationAfter filtration
- washwashing with ethyl acetate (100 mL×3×)
- customdrying in vacuum
Sources & evidence
- ORD record
- ord-a6b6d4a3ad4d4908b848fb8c47d04271
- Source dataset
- uspto-grants-2014_06
- Patent number
- US08748542B2
Linked notes
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