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以邻苯二甲酸酐、尿素、六水合四氯化锡为原料,氯化铵为催化剂,采用固法合成二氯酞菁锡(Ⅳ),并用元素分析、IR、XPS、XRD进行表征。考察了反应物配比、催化剂、反应温度和时间对产率的影响,寻找出最佳合成条件为n(邻苯二甲酸酐)∶n(尿素)∶n(六水合氯化锡)=5∶15∶1,以钼酸铵和氯化铵为催化剂,加入反应器中,用水蒸汽冷凝回流,在150℃反应1h后,升温到260℃,继续反应1h,收率达到70.70%。
The phthalic anhydride, urea and tin tetrachloride hexahydrate were used as raw materials and ammonium chloride was used as catalyst to synthesize tin dichlorophthalocyanine (Ⅳ) by solid method and characterized by elemental analysis, IR, XPS and XRD. The effects of the ratio of reactants, catalyst, reaction temperature and time on the yield were investigated. The optimal synthesis conditions were n (phthalic anhydride): n (urea): n (tin chloride hexahydrate) = 5 : 15: 1, ammonium molybdate and ammonium chloride as catalyst, added to the reactor, condensed with water vapor reflux, at 150 ℃ for 1h, heated to 260 ℃, the reaction was continued for 1h, the yield was 70.70%.