Water → Buta-1,3-diene;methyl 2-methylprop-2-enoate;styrene

Participants

Reaction Conditions

Reaction Steps

A methyl methacrylate-styrene-butadiene multi-stage graft copolymer was prepared as follows. Initially, 1.36 grams of potassium persulfate was dissolved in 98.64 grams of distilled water. Then, 0.68 gram of sodium formaldehyde sulfoxylate (Hydrosulfite AWC PEA) was weighed into a 100 ml. volumetric flask and brought up to volume with distilled water. Into a three-neck flask was weighed 65.94 grams of 45.5% of a carboxylated SBR latex with 39% bound styrene (Polysar 6500-LS, Polysar Ltd.) and 34.0 grams of styrene. The three-neck flask was then set up on a hotplate/stirrer and a thermometer, a reflux condenser and a stopper were inserted in the necks. Nitrogen was then hooked up to the thermometer side of the flask and the hose from the reflux condenser was vented to the hood. After agitation was begun, the flask was gently purged with nitrogen for 5 minutes. Then, 10 ml. of the sodium formaldehyde sulfoxylate solution and 10 ml. of the potassium persulfate solution were added to the flask. The flask was then heated to a temperature of about 80° C. while stirring. After the temperature reached 80° C., the heat was turned off and the temperature was allowed to cool down to about 40° C. while still stirring. Then, 35.0 grams of methyl methacrylate and 0.35 gram of 1,3-butylene dimethacrylate (Rocryl 970) were weighed into a cylindrical separatory funnel which was placed on the flask and the contents added. After addition of 10 ml. of the sodium formaldehyde sulfoxylate solution and 10 ml. of the potassium persulfate solution, the flask was heated to a temperature of about 80° C. The reaction was allowed to proceed at a temperature of about 70°-80° C. for 1 hour. After 1 hour, the heat was turned off and the mixture was allowed to cool to about 40° C. The mixture was then removed from the flask and dried. The product was a multi-stage graft copolymer comprising a hard portion with about 35 percent by weight of cross-linked methyl methacrylate grafted onto about 35 percent by weight of styrene grafted onto a rubbery portion with about 30 percent by weight of styrene-butadiene copolymer.

Provenance & Evidence