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为制备高分子单体2,6-萘二甲酸,以自制的2-甲基6-丙酰基萘为原料,在自建的一套氧化反应装置中,以钴锰溴类物质为催化剂,经空气液相催化氧化得到了2,6-萘二甲酸.并对氧化反应的产物进行了FT-IR和HLPC-MS表征;对氧化反应的工艺条件进行了研究.结果表明,氧化反应的较佳条件为:反应时间30 min,物料的溶剂质量比为15∶1,反应温度210℃,反应压力2.2 MPa,催化剂中钴的质量分数为0.1%,合适的催化剂质量配比1∶2∶3.产物的收率可达68%,产物的纯度大于95%.
In order to prepare macromonomer 2,6-naphthalene dicarboxylic acid, self-made 2-methyl 6-propionyl naphthalene was used as raw material. In a self-built oxidation reaction device, The 2,6-naphthalene dicarboxylic acid was obtained by liquid-phase catalytic oxidation in air and FT-IR and HLPC-MS were used to characterize the oxidation reaction. The oxidation conditions were studied. The results showed that the oxidation reaction was better The conditions were: the reaction time was 30 min, the mass ratio of solvent to solvent was 15:1, the reaction temperature was 210 ℃, the reaction pressure was 2.2 MPa, the mass fraction of cobalt in the catalyst was 0.1% and the mass ratio of the catalyst was 1: 2: 3. The yield of the product can reach 68%, the purity of the product is more than 95%.