摘要
选择邻硝基甲苯作为合成4-氨基-2-氯甲苯-5-磺酸(2B酸)的环保型反应溶剂,进行工艺改进研究。采用单因素分析考察了原料摩尔配比、反应温度、反应时间和溶剂用量等操作条件对产品收率和纯度的影响,确定了最优工艺条件为:mol2B油∶mol浓硫酸=1∶1.02,T=200℃,t=120 min,每克2B油对应的溶剂最佳用量为5 m L;该反应条件下产品收率为95.05%,产品纯度为99.92%。同时研究了溶剂重复使用对产品收率和纯度的影响,结果表明溶剂循环使用5次产品收率和纯度均分别在94.80%和99.50%以上,溶剂每次循环使用的回收率也均高于95.20%。
O-nitrotoluene was chosen as environmental-protection-type solvent to improve the synthesis process of 4-amino-2-ehlorotoluene-5-sulfonic acid （2B acid） in this paper. Effects of the molar ratio of raw material, reaction temperature, reaction time and solvent dosage on the product yield and purity were investigated by using the single factor experiment. As a result, the optimal process conditions were obtained in the following： mol2a lid： molso =1：1.02, T=200 ℃, t=120 rain and 5 mL o-nitrotoluene per gram of oil 2B, and the product yield and pu- rity were 95.05% and 99.92%, respectively, under the optimal process conditions. At the same time, the effect of the repeated use of o-nitrotoluene on the yield and purity of 2B acid were studied, the result showed that the yield, purity and recoveries of solvent were all above 94.80%, 99.50% and 95.20% respectively during the five recycling use of o-nitrotoluene.
出处
《苏州科技学院学报（工程技术版）》
CAS
2015年第3期5-8,41,共5页
Journal of Suzhou University of Science and Technology （Engineering and Technology）
基金
住房与城乡建设部科技开发项目(2011-K4-2)
苏州科技学院校研究生创新工程项目(SKCX14_066)
关键词
2B酸
磺化
工艺改进
2B acid
sulfonation
process improvement
