Potassium Hydroxide → Diglycidyl ether

Temperature

60 °C

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 10,000 Mw PEG and toluene (80 mL) was heated to 60° C. At this temperature, KOH (1.52 g, 0.04 mol, in 1.5 g of water) was added and the reaction mixture was stirred for 1 hour. Dodecyl glycidyl ether (5.81 g, 0.024 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 (31.8 g) was obtained. 1H NMR showed 11% hydrophobe incorporation. The Brookfield viscosity of a 5% aqueous solution of this oligomer was >400000 cps (BF LV, S-63, 0.3 rpm at 25° C.). Paint performance: SG10 M (standard formulation). The material was not soluble in this paint. For UCAR 379 G, TE %=0.52, VLT=−17 KU.

1. customIn a 250 mL, round bottom 3-neck flask equipped with a condenser
2. waitthe reaction temperature was kept at 110° C. for 5 hours
3. temperatureAfter the reaction mass was cooled to 60° C.
4. customThe solution was precipitated into 300 mL of hexane
5. filtrationAfter filtration
6. washwashing with ethyl acetate (100 mL×3×)
7. customdrying in vacuum

ORD record

ord-8b5ed05764284242b288dcb9024a33f9

Source dataset

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08748542B2