Acrylic Acid → Prop-2-enoic acid--6-methylheptyl prop-2-enoate (1/1)

Participants

Reaction Conditions

Reaction Steps

A flask equipped with an agitator, condenser, nitrogen inlet tube and an addition funnel was charged with isooctyl acrylate (72.0 g), acrylic acid (8.0 g) and ethyl acetate (78.1 g). The mixture was heated to 60° C. with medium agitation and purged with nitrogen to remove oxygen. Lucidol 75 (0.07 g, available from Elf Atochem North America) premixed in ethyl acetate (3.0 g) was added to initiate reaction. The reaction temperature was maintained at 60° C. Ethyl acetate (1.5 g) was added to the polymer solution every 30 minutes until the conversion of isooctyl acrylate to polymer reached a minimum of 95%, typically 20-30 hours. An additional charge of Lucidol 75 (0.07 g) premixed with ethyl acetate (3.0 g) was added after 5 hours and nine hours reaction time. When 95% minimum reaction conversion was achieved, the resulting polymer solution was diluted with heptane to 20-23%, solids, cooled and drained. The inherent viscosity in ethyl acetate at 0.15 g/dl was measured at 1.7-2.0 dl/g. The inherent viscosity was measured by conventional means using a Canon-Fenske #50 viscometer in a water bath controlled at 27° C. to measure the flow time of 10 milliliters of the polymer solution. The test procedure and apparatus are described in detail in "Textbook of Polymer Science", F. W. Billmeyer, Wiley Interscience, Second Edition, 1971, pages 84 and 85.

Provenance & Evidence