반응 #491488
ord-a6b6d4a3ad4d4908b848fb8c47d04271
반응 조건
후처리
- 1기타In a 250 mL, round bottom 3-neck flask equipped with a condenser
- 2workup.WAITthe reaction temperature was kept at 110° C. for 5 hours
- 3온도After the reaction mass was cooled to 60° C.
- 4기타The solution was precipitated into 300 mL of hexane
- 5여과After filtration
- 6세척washing with ethyl acetate (100 mL×3×)
- 7기타drying in vacuum
실험 절차
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.