Methyl Methacrylate → HCID 197116, compound

Participants

Reaction Steps

Methacrylic acid (0.1 mol) and hexaethyldititanoxane (0.05 mol) were dissolved in xylene and subjected to reaction. The water that formed as the reaction proceeded was removed together with the solvent by distillation. The by-product of the reaction was distilled off under vacuum and the residue was dried under vacuum to obtain triethyltitanyl methacrylate (m.p. 89° C.; yield, 54%). This triethyltitanyl methacrylate and methyl methacrylate were put into a round-bottom flask at a molar ratio of 1:1 and xylene was added to achieve a concentration of ca. 50%. Benzoyl peroxide (1 mol % of the sum of the triethyltitanyl methacrylate and methyl methacrylate) dissolved in xylene was charged into a dropping funnel. After equipping the flask with this funnel, the benzoyl peroxide solution was dripped in an amount of about 10% of the total quantity of the solution. Thereafter, the flask was heated to the reflux temperature and the remaining polymerization initiator was slowly added dropwise until the reaction was completed in 8 hours. After the reaction, the content of the flask was added to n-hexane and subjected to re-precipitation. The resulting precipitate was recovered and dried to obtain a solid product. This solid product was dissolved in ethanol, added slowly to ice water and subjected to re-precipitation. The precipitate was recovered and dried to obtain poly(triethyltitanyl methacrylate-methyl methacrylate). Yield, 75%, Mn, 35,000; Mw/Mn=2.2, IR (ν cm-1), 1720, 1710, 1160, 1100, 720; atomic absorption spectrum (Ti content), 14.80 (found) and 14.95 (calculated).

Provenance & Evidence