节点文献
1-氨基-2-萘酚-4-磺酸的合成工艺研究
A Study on the Synthetic Process of 1- Amino-2-naphthol-4-sul-fonic acid
【摘要】 以 β 萘酚为原料 ,在水 醇混合溶剂存在下 ,经亚硝化、加成、磺化制得 1 氨基 2 萘酚 4 磺酸 ,考察了原料配比、混合溶剂配比、反应时间、反应温度及过滤等因素对反应的影响 ,确定了优惠工艺条件。亚硝化条件 :n(酚 )∶n(亚硝酸钠 )∶n(硫酸 ) =1∶1∶0 5 ,以 10 gβ 萘酚计 ,有机溶剂异丙醇用量 15ml,混合溶剂配比V(水 )∶V(异丙醇 ) =(1~ 1 5 )∶1。亚硝化完毕后将物料过滤 ,水洗。加成反应时间控制在 6h ,n(酚 )∶n(亚硫酸氢钠 ) =1∶2 ,碘化反应时间6h ,温度 5 0~ 6 0℃。在此条件下 ,收率达到 72 1%。
【Abstract】 With water-alcohol as solvent, 1-amino-2-naphthol-4-sulfonic acid was prepared from β-naphthol by nitrosotion, addition, and sulphonation. The effects of ratio of reagents ,water-alcohol ratio, reaction time, reaction temperature, and filtration on reaction was investigated. The optimum reaction conditions are as follows; ①nitrosotion n(β-naphthol):n(NaNO2):n(H2SO4)=1∶1∶0.5,volume of solvent isopropanol 15 ml according to w (β-naphthol)=10g,V(H2O) ∶V(isopropanol)=(1~1.5) ∶1,filtering and washing after nitrosotion;②addition reaction time 6 h, n(β-naphthol) ∶n(NaHSO3)=1∶2; ③sulphonation reaction time 6 h, temperature 50~60?℃. Under optimum conditions the yield of 1,2,4-acid is 72.1%.
- 【文献出处】 精细化工中间体 ,Fine Chemical Intermediates , 编辑部邮箱 ,2003年05期
- 【分类号】O625.7
- 【被引频次】7
- 【下载频次】375