Methacrylic Acid → Methyl methacrylate isobornyl methacrylate methacrylic acid

Participants

Reaction Conditions

Reaction Steps

560.0 g of methyl ethyl ketone were placed in a 2 L three-necked flask equipped with a mechanical stirrer, a thermometer, a reflux condenser tube, and a nitrogen gas inlet tube, and heated to a temperature of 87° C. While maintaining the contents inside the reaction vessel in a refluxed state (thereafter, refluxing was continued until the reaction was completed), to this reaction vessel, a mixed solution of 278.4 g of methyl methacrylate, 243.6 g of isobornyl methacrylate, 58.0 g of methacrylic acid, 108 g of methyl ethyl ketone, and 2.32 g of “V-601” (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise at a constant speed so that the dropwise addition was completed in two hours. After the dropwise addition was completed, the resulting mixture was stirred for one hour. Thereafter, a solution of 1.16 g of “V-601” and 6.4 g of methyl ethyl ketone was added and the resulting mixture was stirred for two hours (process (1)). Subsequently, the process (1) was repeated for four times. Then, a solution of 1.16 g of “V-601” and 6.4 g of methyl ethyl ketone was further added, and stirring was continued for 3 hours. After completion of the polymerization reaction, the temperature of the resulting solution was lowered to 65° C. and then, 163.0 g of isopropanol were added thereto and the resulting mixture was cooled while leaving it standing still. In this way, a solution of a methyl methacrylate/isobornyl methacrylate/methacrylic acid copolymer (=48/42/10 [mass ratio]) was obtained.

Provenance & Evidence