对苯双偶氮乙酰乙酰苯胺的制备
毕业论关键字：对硝基苯胺，乙酰乙酰苯胺，重氮化反应，偶合反应
The preparation of double azo benzene acetoacetanilide
Abstract: In this study, use the para-nitroaniline (A), acetoacetanilide (B) supplied from enterprises as raw materials to synthesize high symmetry of double azo benzene acetoacetanilide pigment. Since para-nitroaniline has amino, prepare it to the corresponding diazonium salt. Acetoacetanilide with active hydrogen can do coupling reaction with diazonium salt to synthesize para-nitrobenzene azo acetoacetanilide (C). Reduce the nitro of compound by sodium sulfide to reach a single azo compound para-aminobenzene azo acetoacetanilide (D). Then make the corresponding diazonium salt of compound D with another acetoacetanilide further reaction to get the final product of double azo benzene acetoacetanilide (E). Use the infrared spectrum to characterize the intermediate and final products. The results show that the intermediate product preparation conditions: (1) diazotization of the feed ratio n(A): n(NaNO2)=1:1.5, the reaction temperature 0~5℃, reaction time 40 min, (2) reduction reaction of the feed ratio n(C): n(Na2S)=1:1.5, reduction time 12h, the yield 45.10%; final product preparation conditions: (1) diazotization of pH=2~3, the reaction temperature 0~5℃, reaction time 40 min, (2) coupling reaction of pH= 8~9, the reaction temperature 0~5℃, reaction time 90 min, the yield 52.12%.
Keywords: para-nitroaniline, acetoacetanilide, diazo reaction, coupling reaction
目 录
1 前言.1
1.1 颜料及有机颜料 1
1.1.1 颜料的概述及分类 1
1.1.2 有机颜料的概述及分类 1
1.2 偶氮颜料的概述 2
1.3 重氮化反应 2
1.3.1 重氮化反应及影响因素 3
1.3.2 重氮化反应的分析控制 4
1.3.3 重氮化合物 4
1.4 偶合反应 5
1.4.1 偶合反应概述 5
1.4.2 偶合反应的影响因素 5
1.4.3 偶合反应的分析控制 7
1.5 偶氮颜料的合成方法 7
1.6 乙酰基乙酰苯胺偶氮颜料的概述 9
1.7 本课题的研究内容及意义 9
1.7.1 研究内容 9
1.7.2 研究目的及意义 10
2 实验部分11
2.1 仪器和试剂 11
2.1.1 实验仪器 11
2.1.2 实验试剂 11
2.2 实验过程 12
2.2.1 对硝基苯胺重氮盐的制备 12