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用以邻二氯苯为溶剂的液相磺化法代替固相烘焙磺化法,在表面活性剂Tween-60和邻二氯苯存在的条件下,1-萘胺和硫酸经铵盐化、转位磺化、加碱(Na2CO3)成盐合成了1-氨基-4-萘磺酸钠。考察了不同有机溶剂、磺化反应时间、表面活性剂、母液套用对反应的影响。得到的最佳工艺条件为:1-萘胺35.8 g、w(H2SO4)=80%的硫酸33.6 g、邻二氯苯150 mL、Tween-60 1.5 g,磺化反应时间6 h,在该条件下1-氨基-4-萘磺酸钠收率可达90.6%。
Using o-dichlorobenzene as solvent instead of the solid-phase sulfonation sulfonation method, 1-naphthylamine and sulfuric acid were ammonium salified in the presence of surfactant Tween-60 and o-dichlorobenzene, Translocation sulfonation, alkali (Na2CO3) salt synthesis of 1-amino-4-naphthalene sulfonate. The effects of different organic solvents, sulfonation time, surfactant and mother liquor on the reaction were investigated. The optimal conditions were obtained as follows: 35.8 g of 1-naphthylamine, 33.6 g of sulfuric acid with w (H2SO4) = 80%, 150 mL of o-dichlorobenzene, 1.5 g of Tween-60 and 6 h of sulfonation reaction. Under 1-amino-4-naphthalene sulfonate yield up to 90.6%.