【作者】 何广科；

【导师】 陈钟秀；

【作者基本信息】 浙江大学 ， 应用化学， 2005， 硕士

【摘要】 2-磺酸-4-(β-乙基砜硫酸酯)苯胺为制备水溶性双活性染料的重要中间体,该产品的研制国内文献未见报导。本文研究了合成上述中间体的两步关键反应,即乙酰苯胺发生氯磺化反应合成对乙酰氨基苯磺酰氯和对氨基苯基-β-羟乙基砜硫酸酯(对位酯)合成最终产品的生产工艺。本文确立了乙酰苯胺氯磺化的最佳工艺条件,乙酰苯胺与氯磺酸的摩尔比为1:3. 8,反应温度为60℃,反应时间为2. 5小时,催化剂A的用量为1. 6克(乙酰苯胺20. 3克)。乙酰苯胺与磺化助剂的摩尔比为1:0. 45时,摩尔产率可达96. 09%;乙酰苯胺与磺化助剂的摩尔比为1:0. 35时,经济成本最佳,摩尔产率为90. 24%。本文也确立了以对位酯为原料,依次进行磺化、水解和酯化反应,即得产品2-磺酸基-4-(β-乙基砜基硫酸酯)苯胺,其摩尔产率以氨基值为基准计算,为98. 55%,比文献值高2. 55%。其最佳反应条件为:对位酯与发烟硫酸的摩尔比为1:2. 7,发烟硫酸的滴加温度为10-15℃,磺化、水解和酯化的反应温度分别为130、 124和140℃,磺化、水解和酯化的反应时间分别为5. 0、 11. 5和25小时。更多还原

【Abstract】 1-Aminobenzene-4-( β -sulphatoethylsulphone)-2-sulfonic acid is often applied to producing bifunctional-soluble reactive dyes and is an important dye intermediate. Two steps play a great role in the process of its preparation, one is chlorosulfonation reaction of acetanilide, the other is sulfonation of l-aminobenzene-4- P -sulphatoethylsulphone.The optimal reaction conditions of synthesizing p-acetanmidobenzenesufonyl chloride have been studied in the paper. In the reaction conditions, the mol ratio between acetanilide and chlorosulfonic acid is 1:3.8; the reaction temperature is 60℃; the reaction time is 2.5 hours; the usage of catalyst A is 1.6 gram. When the mol ratio between acetanilide and sulfonation agent equals 1:0.35, the mol yield is 90.24% and the productive cost is more economical; when the mol ratio between acetanilide and sulfonation agent is less than 1:0.35, the mol yield will be higher than 96.09% .l-Aminobenzene-4- β -sulphatoethylsulphone(para-ester) can be used as raw material to produce the target product l-aminobenzene-4-( β -sulphatoethylsulphone)-2-sulfonic acid through sulfonation and hydrolysis and esterification reactions. The mol yield is 89.95 % and 98.55 % on the basis of ester-group value and amino-group value respectively. The optimal reaction conditions are as follows: the mol ratio between oleum containing by weight of 50% and para-ester is 2.7:1; the addition temperature of oleum is 10-15℃; the temperature of sulfonation and hydrolysis and esterification reactions is 130 ℃ and 124℃ and 130℃ respectively, and their reaction time is 5 hours and 11.5 hours and 25 hours in turn.更多还原