Sulfuric Acid → Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

A glass-made vessel equipped with a reflux condenser, a dropping funnel, a thermometer, a nitrogen blowing-in nozzle and a stirrer was charged with 5 parts of PVA having a mercapto group at only one end thereof (PVA-3: degree of polymerization of 550, degree of hydrolysis of 88.3 mol %, mercapto group content of 3.3×10-5 equivalent/g) and 90 parts of ion-exchanged water, and the PVA was completely dissolved in the water at 95° C. The resultant aqueous solution of the PVA was adjusted to pH=4 with dilute sulfuric acid, and incorporated, under stirring at 150 r.p.m., with 10 parts of methyl methacrylate, 10 parts of n-butyl acrylate and 0.1 part of n-dodecyl mercaptan. Then, the reaction system was replaced with nitrogen, and the temperature in the system was raised to 70° C. Subsequently, emulsion polymerization was initiated by adding to the system, 5 parts of aqueous solution of potassium persulfate having a concentration of 1%. To the system were continuously added the mixture of 40 parts of methyl methacrylate, 40 parts of n-butyl acrylate and 0.4 part of n-dodecyl mercaptan over a period of 2 hours. The polymerization was finished at the time when a conversion of 99.5% was achieved after 3 hours from the start of the polymerization. As a result, there was obtained a stable emulsion of methyl methacrylate/n-butyl acrylate copolymer having a solid concentration of 52.0%. Thereafter, the procedure in Example 1 was repeated to produce the synthetic resin powder except that the emulsion thus obtained was used. The results of evaluation of the powder are given in Tables 3 and 4.

Herkunft & Nachweise