塗膜の劣化に関する研究-4-トール油脂肪酸,米ヌカ油脂肪酸ウレタン化油塗膜の劣化
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The authors carried out out door degradation test of the films of some urethane oils. The urethane oil was synthesized by the reaction of TDI (Tolylene-di-isocyanate) with partial fatty acid ester of pentaerythritol. Authors synthesized the tall penta 3 : 1 urethane oil as follows : One mol of distillated grade tall oil fatty acid was reacted with 1/3 mol of pentaerythritol at 200°:C for 2 hours and at 230°:C for 4 hours. Then the product was reacted with stoichiometrical TDI in the presence of Pb 0. 4% and Co 0. 05% catalyst at 60°:C for 30 min, at 70°:C for 30 min and at 80°:C for 30 min.<BR>Tall penta 2 : 1 urethane oil, alkali isomerized tall penta 3 : 1 urethane oil and rice penta 2 : 1 urethane ell were also synthesized.<BR>Changes of IR spectra of the films of these urethane oils were measured as follows : Sample was coated on a polyethylene 20υ film at the thickness of about 25 υ. The coated film was fixed on a frame of polyvinyl chloride resin, then IR spectrum was measured by a double beam type IR spectrophotometer, putting another not coated polyethylen film in the position of compensate cell. Then the coated film was exposed for 10 months, and the spectrum was measured at intervals.<BR>Changes of weights, hardness and gloss were measured of the films coated on a glass plate, and flexibility was also measured on the films coated on a tin plate.<BR>Discussion : Nonexposed tall penta 3 : 1 urethane oil film had absorption peak at 3300 cm- (OH and NH), 2926 cm- (CH<SUB>2</SUB>), 1725 cm- (urethane carbonyl and ester carbonyl), 1600 cm- (benzene ring), 1525 cm- (amide), 1230 cm- (amide 1ff +ester), 1175 cm- (ester C-O-C), 1065 cm- (carbamate C-O-C), 1035 cm- (pentaerythritol skeletal), 815 cm- (1, 2, 4 trisubstituted benzen C-H out of plane) and 770 cm- (1, 2, 3 trisubstituted. benzen C-H out of plane) and 730 cm- (CH<SUB>2</SUB> rocking). Optical density changes of these absorption on exposing were plotted to the lapse of month. Decreasing speeds of 1725 cm-, 1525 cm-, and 1230 cm-were almost equal to the decreasing speed of the weight of glass plate film. Therefore it must be said that urethane part of the film was unchanged on exposing. Optical density of 3300 cm-, 1050 cm-, 1175 cm-decreased more slowly than the weight, which seems that OH and ester group increased on exposing. That of 2926 cm-decreased much more rapidly than the weight loss, which seems that CH<SUB>2</SUB> part diminished quickly on exposing.<BR>Tests of tall penta 2 : 1 urethane oil, alkali-isomerized tall penta 3 : 1 urethane oil and rice penta 2 : 1 urethane oil gave same results.<BR>Gloss of each oil films was lost down to about 60% after 1 month exposing and was unchanged after that time. Hardness (Sword hardness) of comparatively soft film increased to about 20 gradually. But the films lost flexibility inversely after exposing.
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