甲基磺酸的制备及反应条件的考察.pdfVIP

甲基磺酸的制备及反应条件的考察 摘 要 甲基磺酸（MSA ）是一种有机强酸，常用作溶剂、烷基化和酯化反应的催化剂， 是重要的有机合成和医药中间体。近几年，MSA 在电镀工业中应有越来越广泛， 由于MSA 危害相对较少而且废水处理简单，并且可生物降解，不仅在环保方面具 有明显的优势，还具有许多其他优良特性，正逐步替代传统的氟硼酸和氟硅酸镀液。 因此，MSA 是一种很有发展前途的化工产品。 本论文采用硝酸直接氧化二甲二硫制备甲基磺酸。采用化学滴定分析方法分析 实中产物，尾气 NO 通过空气氧化后水吸收或者双氧水直接吸收。实验中考察了硝 酸浓度（40-70% ）、反应温度（50-100℃）和反应时间对甲基磺酸收率的影响。由 研究结果得到最佳反应条件为，硝酸浓度为 50-70%，反应温度 60-80℃之间得到的 甲基磺酸收率最高，而二甲二硫的转化率均可达到 100%。 硝酸氧化二甲二硫过程中硝酸可以循环利用，反应在常压和温度不高的条件下 进行，因此该方法具有运行成本低、废物排放少、节能环保的优点，具有很好的工 业应用前景。 关键词：甲基磺酸，氧化法，二甲二硫，滴定分析 I 甲基磺酸的制备及反应条件的考察 Abstract MSA is a kind of strong organic acid, commonly it was used as the catalyst in the solvent reaction, alkylate reaction and esterification ,and it is a major midbody of the organic synthesis and pharmaceutical. In recent years, MSA is use more and more extensinve in the electroplating industry. Since the MSA is little harmful and treated easylily and biodegradable, it is not only in environmental protection has obvious advantages, but also has many other fine features, are gradually replaced Traditional fluoride solution of boric acid and fluorosilicic acid. Therefore, MSA is a promising chemical products. This paper used nitric acid oxidation of methyl acid dimethyl disulfide. Titration analysis using chemical analysis of the real product, NO exhaust air through absorption of water or hydrogen peroxide after the direct absorption. Experiment inspected the concentration of nitric acid (40-70%), temperature (50-100 ℃) and reaction time on acid-yield impact. The results from the b