摘要
以邻硝基氯苯为原料,经亚硫酸氢钠亲核置换磺化,Pd/C催化加氢还原得到邻胺基苯磺酸,并对各步反应的影响因素进行了研究。结果表明:在反应时间为5h、反应温度60～65℃以及原料亚硫酸氢钠与邻硝基氯苯物质的量比为1.1:1时,中间体邻硝基苯磺酸收率可达86.1%。反应时间为12h、反应温度为75℃、氢气压力为0.8MPa、Pd/C用量为硝基物质量的1%时,邻胺基苯磺酸的收率达92.1%,产品纯度达98.95%,熔点300℃。与传统工艺相比,该工艺可以避免三废污染、降低生产消耗,有利于工业化生产。
O-aminobenzene sulfonic acid was synthesized from o-nitro chlorobenzene,by sulfonation with sodium bisulfite,and reducing reaction with Pd/C.The influences of all reaction factors were investigated respectively.Results showed that the yield of intermediate o-nitrobenzenesulfonic acid was 86.1% when the reaction time was 5 h,reaction temperature was 60-65 ℃,and material ratio of sodium bisulfite and o-nitro chlorobenzene was 1.1:1.The yield of o-aminobenzene sulfonic acid was 92.1% when the reaction time was 12 h,reaction temperature was 75 ℃,pressure of H2 was 0.8 MPa,and the mass of Pd/C was 1% of o-nitrobenzenesulfonic acid.The purity of o-aminobenzene sulfonic acid was 98.95%,and the melting point was 300 ℃.This method can avoid the pollution of three wastes,reduce consumptions and is more advantageous to industrialization comparing with the traditional process.
出处
《化工生产与技术》
CAS
2009年第4期23-24,共2页
Chemical Production and Technology
关键词
邻硝基氯苯
邻氨基苯磺酸
磺化
还原反应
o-nitro chlorobenzene
o-aminobenzene sulfonic acid
sulfonation
reducing reaction
