有机颜料黄系列的合成与改性研究

【作者】 王琦；

【导师】 鲁波； 陈志荣；

【作者基本信息】 浙江大学 ， 化学工程， 2006， 硕士

【摘要】 有机颜料黄系列是有机颜料中应用最广泛的一类重要的颜料。有机颜料黄12、有机颜料黄13、有机颜料黄83是有机颜料黄系列中最常用的三种颜料。本文以3,3′—二氯联苯胺为原料,通过重氮化反应、偶合反应和颜料化后处理的方法来合成这三种有机颜料。通过测试有机颜料在油墨中应用性能,对其性能的影响因素进行分析,对这三种有机颜料的合成工艺条件进行的优化研究结果表明在重氮化反应中搅拌转速要控制在300rpm以上,温度在5～10℃,滴加时间为40分钟,亚硝酸钠与原料3,3′—二氯联苯胺的摩尔比为1.2:1,酸量在2.4mol/L。在有机颜料黄12和有机颜料黄13的偶合反应中搅拌转速都要控制在600rpm以上,滴加时间在50分钟左右,pH值在5左右,温度在5～10℃。在合成有机颜料黄83偶合反应中搅拌转速要控制在600rpm以上,在低温反应阶段滴加时间在40～50分钟,pH值在5左右,温度在5～10℃,在高温反应阶段滴加时间在90分钟,温度在70℃。 本文通过对有机颜料中含有杂质对其应用性能影响的分析,结合反应机理,对杂质的构成和产生过程进行了推断。 对于有机颜料的应用性能与有机颜料晶体物理形态的关系,运用扫描电镜、X射线衍射等分析手段对颜料晶体粒径、晶体形貌与有机颜料的应用性能进行研究分析,表明颜料性能不仅与晶体形貌有关,也与颜料晶体的粒径分布有关。更多还原

【Abstract】 The series of organic yellow pigment are the most important kind of pigments. And yellow pigment 12, yellow pigment 13,and yellow pigment 83 are most widely used of the series of organic yellow pigment. The yellow pigment 12, 13, and 83 are synthesized by 3,3’-dichlorobenzidine through diazotization reaction, and the couple reaction. The influencing factors of the performance of pigment are studied by testing the applied performance of the pigment in printing ink. And when the diazotization reaction happens under the conditions that the agitated speed more than 300 rpm, the temperature is between 5℃ and 10℃, 3,3’-dichlorobenzidine is added in 40 minutes, the concentration proportion of nitrous sodium and 3,3’-dichlorobenzidine is 1.2: 1, and the acid concentration is 2.4mol/L, the pigment shows greater applied performance than those prepared under other conditions. And when the couple reaction happens under the condition that the agitated speed more than 600 rpm, the diazo salt is added in 50 minutes, the temperature is between 5℃ and 10℃, and pH is 5, the yellow pigment 12 and 13 show greater performance. When the yellow pigment 83 is synthesized, the agitated speed is controlled more than 600 rpm, and the diazo salt is added in 40-50 minutes during the low temperature 5~10℃, and pH is 5, when the temperature is 70℃, the diazo salt is added in 90 minutes.The impurity affects the applied performance of the pigment, the constitute of the impurity and the second reaction are concluded by analyzing the reaction mechanism.SEM and XRD are used to analyzing the relation between the applied performance of organic pigment and the crystal modality. The conclusion is that the applied performance is not only affected by the crystal modality, but also by the distribution of the particulate size.更多还原