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机构地区:[1]中科纳米涂料技术(苏州)有限公司,江苏苏州215024 [2]苏州大学材料与化学化工学部,江苏苏州215123
出 处:《石油化工》2013年第9期1004-1008,共5页Petrochemical Technology
基 金:国家自然科学基金项目(21074085)
摘 要:以二氧六环和水为溶剂、以2-氯-4,6-二(2-萘氧基)-1,3,5-三嗪(CN TA)和1-羟基蒽醌(HYA)为原料,合成了新型三聚氯氰衍生物1-[4,6-双-(2-萘氧基)-2-[1,3,5]三嗪氧基]蒽醌(DNATA).考察了原料配比、碱的种类和用量、反应温度、反应时间等反应条件对DNATA收率的影响,得到了适宜的反应条件.实验结果表明,在NaOH作用下,在n(HYA)∶n(NaOH)∶n(CNTA)=1.1∶1.5∶1.0、反应温度90℃、反应时间72 h的优化条件下,DNATA收率达90.1%.采用FTIR、1H NMR、MS和元素分析等方法对DNATA的结构进行了表征.DNATA的熔点为198 ~ 200℃,DNATA的分解温度为350℃;在四氢呋喃中,最大吸收波长为331nm,摩尔吸光系数为4.96 × 103 L/(mol·cm),最大荧光波长为400 nm.A novel cyanuric chloride derivative 1-[4,6-bis-(2-naphthyloxy)-[1,3,5] triazine-2-yloxy] anthraquinone(DNATA) was synthesized from 2-chloro-4,6-bis-(2-naphthyloxy)-[1,3,5]triazine(CNTA) and 1-hydroxyanthraquinone(HYA) with water and dioxane as solvents.The effects of the mole ratio of the raw materials,type and dosage of bases,and reaction temperature and reaction time on the yield of DNATA were studied.Under the optimum reaction conditions of sodium hydroxide as the base,n(HYA) ∶ n(sodium hydroxide) ∶ n(CNTA) 1.1 ∶ 1.5 ∶ 1.0,reaction temperature 90 ℃and reaction time 72 h,the yield of DNATA reached 90.1%.The product structure was characterized by means ofFTIR,1H NMR,MS and elementary analysis.Its melting points is in the range of 198-200 ℃ and its decomposition temperature is 350 ℃.In tetrahydrofuran,its maximum absorption wavelength,mole extinction coefficient and maximum fluorescence emission wavelength are 331nm,4.96 × 103 L/(mol · cm) and 400 nm,respectively.
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