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在浓硫酸和3-巯基丙酸催化下,3′-三氟甲基苯基-2,2,2-三氟苯乙酮(1)和甲苯于40～50℃下缩合反应8 h,制得中间体-1,1-二(4-甲基苯基)-1-(3′-三氟甲基苯基)-2,2,2-三氟甲基乙烷(2),继而在光照和N-溴代丁二酰亚胺促进下,将中间体氧化得到二羧酸-1,1-二(4-羧基苯基)-1-(3′-三氟甲基苯基)-2,2,2-三氟甲基乙烷(3),二步反应总收率为77.4%.采用Yamazaki体系,3和9,9-二[(4-氨基苯氧基)苯基]呫吨进行溶液亲核缩聚反应,制得了一种高分子量的(数均分子量为43000,分子量分布为1.8)新型含三氟甲基和呫吨结构的聚酰胺.该聚酰胺为非晶态结构并具有良好的透光率(λcutoff=330 nm),其玻璃化转变温度(Tg)为242℃,在氮气气氛中5%的热失重温度(Td5)为465℃,800℃时的残炭率为50%.聚合物易溶于N,N-二甲基乙酰胺(DMAc)、N-甲基吡咯烷酮(NMP)、间甲酚、吡啶(Py)和四氢呋喃(THF)等有机溶剂中,并可浇注得到韧性好和透明的薄膜,其拉伸强度为85 MPa,拉伸模量为2.0 GPa,断裂伸长率为10%.同时,该聚合物的体积电阻、表面电阻和介电常数分别为2.85×1015Ωcm,4.23×1014Ω和3.55(100 Hz),呈现了良好的电绝缘性能.
In the presence of concentrated sulfuric acid and 3-mercaptopropionic acid, 3’-trifluoromethylphenyl-2,2,2-trifluoroacetophenone (1) was condensed with toluene at 40-50 ° C for 8 h to give 1,1-bis (4-methylphenyl) -1- (3’-trifluoromethylphenyl) -2,2,2-trifluoroethane (2) Oxidation of the intermediates by light irradiation and N-bromosuccinimide gave dicarboxylic acid 1,1-bis (4-carboxyphenyl) -1- (3’-trifluoromethylphenyl) - 2,2,2-Trifluoromethylethane (3) was obtained in 77.4% of the total yield in two steps using Yamazaki system with 3 and 9,9-bis [(4-aminophenoxy) phenyl] Ton solution nucleophilic polycondensation reaction to obtain a high molecular weight (number average molecular weight of 43000, a molecular weight distribution of 1.8) containing trifluoromethyl and xanthene structure of the polyamide polyamide is amorphous and Has a good light transmittance (λcutoff = 330 nm), a glass transition temperature (Tg) of 242 ° C., a 5% weight loss temperature (Td5) of 465 ° C. in a nitrogen atmosphere, 50%. The polymer is easily soluble in organic solvents such as N, N-dimethylacetamide (DMAc), N-methylpyrrolidone (NMP), m-cresol, pyridine and tetrahydrofurane (THF) Pouring good toughness And a transparent film having a tensile strength of 85 MPa, a tensile modulus of 2.0 GPa and an elongation at break of 10%, and at the same time, the volume resistance, the surface resistance and the dielectric constant of the polymer were 2.85 × 10 15 Ωcm, 4.23 × 1014Ω and 3.55 (100 Hz), showing good electrical insulation properties.