Acrylic Acid → Acrylic Acid Trimethylolpropane Triacrylate

Participants

Reaction Steps

To a three neck round bottom glass flask, equipped with a mechanical stirrer and a thermocouple with a nitrogen inlet at the side of the inlet-tube was added 70.38 g of 20% caustic (0.353 mol) and 15.63 g water. Next, 26 g of acrylic acid (0.36 mol) were added slowly via a dropping funnel. After the mixture was cooled to room temperature, 0.28 g of a 40 wt. % active solution of Versenex 80 (diethylene glycol triamine pentaacetate from Aldrich) were added. Then 0.8 g trimethylolpropane triacrylate (TMPTA) were dissolved in 13.75 g acrylic acid (0.19 mol) and added to the reaction flask. The dropping funnel was taken off and the opening was covered by a septum. An amount of 0.2 ml of a 0.1% solution of FeSO4x7H2O was added by a syringe through the septum, followed by 0.635 ml of a 10% Na2S2O8 solution. The reaction started immediately. A gel formed. After the temperature peaked the flask was heated for another hour at 70° C. using a heating mantle. Then the aqueous gel was removed and was minced in a lab grinder. One portion was heated in a vacuum oven for 2 hours at 170° C. and a second portion was heated for several hours at 220° C. The products were ground and sieved with 30 mesh (595 μm) and 50 mesh (297 μm) sieves.

Provenance & Evidence