Acrylamide → Acrylonitrile Acrylamide 2-Hydroxyethyl Acrylate

Beteiligte Stoffe

Reaktionsschritte

250 ml of a warm 14.2 lbs/gallon Calcium Bromide solution (Baroid Drilling Fluids) is placed in an Erlenmeyer flask. 4.938 grams of acrylamide (Aldrich, 99%) is allowed to dissolve. This solution is then placed in a sep funnel and 7.7457 grams (9.61 ml) of acrylonitrile (Aldrich, 99%), 16.135 grams (15.96 ml) of 2-hydroxyethyl acrylate (Aldrich, 96%), and 0.5618 grams (0.540 ml) of diethylene glycol diacrylate (Monomer-Polymer & Dajac Laboratories, Catalogue No. 7945) are added. N2 is bubbled through the solution for 30 minutes. In a 40 dram glass vial, 0.378 grams of V-50 Azo initiator (Wako Chemicals USA, Inc.) is added to 28 ml of DI water and allowed to dissolve. 12.5 ml of the V-50 solution is then added to the calcium bromide solution and the solution is degassed for an additional 15 minutes. In a 500 ml baffled three necked reaction vessel, 400 ml of Norpar-12 (Exxon), with 0.75 g of Span 80 (sorbitan monooleate, ICI Americas, Inc.), is degassed for 45 minutes, while the norpar is being stirred with a six bladed R100 impeller, at 560 RPM. The calcium bromide solution is then added to the norpar solution, which is still being stirred, and the reaction runs for 15-18 hours, at approximately 70° C.

Herkunft & Nachweise