混合溶剂法合成4-氨基萘-1-磺酸钠的研究

摘要

Study on the liquid sulfonation of 1-naphthylamine in mixed solvent of o-dichlorobenzene anddurene was conducted. Sodium 4-aminonaphthalene-l-sulfonate was prepared through ammonium sali-fying by 1-naphthylamine and sulfuric acid, transposition sulfonation and neutralization with Na2CO3 in the presence of o-dichlorobenzene and durene. Effects of the sulfonation reaction time, the mass of durene, recycle times of mother liquor were investigated. The optimum conditions were found as follows: 35. 8 g 1-naphthylamine, 33. 6 g 80% sulfuric acid, 120 mL o-dichlorobenzene, 60 g durene and sulfonation time 5 h, with the yield of sodium 4-amino naphthalene-1-sulfonate of 93. 1%.%研究了邻二氯苯-均四甲苯混合溶剂中1-萘胺的液相磺化.在邻二氯苯-均四甲苯混合溶剂的存在下,1-萘胺和硫酸经过铵盐化、高温转位磺化、加Na2 CO3中和成盐可以制备4-氨基萘-1-磺酸钠.考察了不同磺化反应时间、均四甲苯添加量、母液套用对反应的影响.较佳工艺条件为:1-萘胺35.8g,质量分数80％硫酸33.6 g,邻二氯苯120 mL,均四甲苯60 g,磺化时间5h,4-氨基萘-1-磺酸钠收率可达93.1％.