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以固体酸为催化剂,4,4’-二氟二苯甲酮与苯胺脱水缩合,合成了N-(双(4-氟苯基)亚甲基)苯胺.比较了不同固体酸催化剂H型ZSM-5、Na型ZSM-5、介孔分子筛MCM-41(Al)及强酸型离子交换树脂Amberlyst 15的催化效果.使用比表面、NH3-TPD对催化剂进行了表征,并与催化效果关联.考察了催化剂用量、原料摩尔比、浓度及溶剂等反应条件对产物收率的影响.产物通过熔点、核磁共振谱进行了表征.结果表明,HZSM-5固体酸催化剂具有优异的催化作用.在优化条件下,以对二甲苯为反应溶剂和脱水剂,4,4’-二氟二苯甲酮0.1 mol,苯胺0.2 mol,催化剂用量2.0 g,反应24 h,产物收率达91%.此外,催化剂易于分离,能够重复使用多次.
N, N-bis (4-fluorophenyl) methylene) aniline was synthesized by the dehydration condensation of 4,4’-difluorobenzophenone with aniline using solid acid as the catalyst.Compared with different solid acid catalysts, H type ZSM -5, Na-type ZSM-5, mesoporous molecular sieve MCM-41 (Al) and strong acid ion-exchange resin Amberlyst 15. The catalysts were characterized by specific surface and NH3-TPD and correlated with the catalytic effect. The effects of reaction conditions, such as the amount of catalyst, the molar ratio of raw materials, the concentration of the raw materials and the reaction conditions on the yield of the product were investigated. The product was characterized by means of melting point and nuclear magnetic resonance spectroscopy. The results showed that HZSM-5 solid acid catalyst had excellent catalytic activity, , With p-xylene as the reaction solvent and dehydrating agent, 0.1 mol of 4,4’-difluorobenzophenone and 0.2 mol of aniline, the amount of catalyst was 2.0 g and the reaction time was 24 h, the yield of product was 91% .In addition, the catalyst Easy to separate, can be reused many times.