Potassium Chloride → Styrene/butadiene pyrrolidinoethyl styrene

Participants

Reaction Steps

In this experiment, an emulsion styrene/butadiene/pyrrolidinoethyl styrene (PES) terpolymer was prepared in a larger reactor. In the procedure utilized, 40.1 lbs. of soft water, 33 grams of sodium naphthalenesulfonate-formaldehyde dispersant (Daxad 14B from Hampshire Chemical Co., 47.5% active), 25.5 grams of potassium chloride, 767 grams of disproportionated rosin acid (potassium salt, 20% solution in water at pH 9.5), 2927 grams of C14-18 and C16-18 unsaturated mixed fatty acids (potassium salt, 10% solution in water at pH 9.5), and 5.82 grams of tripotassium phosphate were charged into a 10-gallon stainless steel reactor. Prior to charging to the reactor, the pH of the solution was adjusted to 10.2-10.8 with 20% potassium hydroxide. Next, 440 grams of soft water, 1.26 grams of ethylenediaminetetraacetic acid, ferric sodium complex (Akzo Nobel Chemicals Co.), and 7.75 grams of sodium formaldehyde sulfoxylate were added. Then, 3245 grams of styrene, 59.8 grams of PES (92% purity by GC), and 16.0 grams of tertiary dodecylmercaptan were added. The reactor was evacuated for 15 minutes, and 7700 grams of 1,3-butadiene was added. At 10° C., 10 grams of pinane hydroperoxide (55% active) was added. The emulsion polymerization was initiated at a temperature of 10° C. with the reactor being agitated at a speed of 250 rpm with two AFT blades. After 6.25 hours and about 65% conversion, the polymerization was shortstopped with a solution of 880 grams of soft water and 44 grams of isopropylhydroxylamine (15% active).

Provenance & Evidence