以氨基磺酸为磺化剂制备樟脑磺酸的新工艺研究

Study on the New Technology of Preparing Camphorsulfonic Acid with Sulfamic Acid as Sulfonating Agent

为开发一种成本更低、收率更高、环境友好的樟脑磺酸制备工艺,尝试了大量磺化方法,最终发现合成樟脑粉在正庚烷溶剂中以氨基磺酸为磺化剂,在100℃~105℃、0.10 MPa的条件下的磺化效果最佳,收率为90.33%,含量为99.92%,熔点:201.2℃~201.5℃,硫酸盐含量≤0.20%,铁离子含量≤10 mg/kg,水分含量为0.25%。该工艺设备腐蚀性小,危险废物产生量少,符合工业化生产要求。

In order to develop a preparation process of camphorsulfonic acid with lower cost,higher yield and environmental friendliness,a large number of sulfonation methods were tried in this paper.It was finally found that the synthetic camphor powder was sulfonated with sulfamic acid in n-heptane solvent.The agent has the best sulfonation effect at 100℃~105℃and 0.10 MPa,the yield was 90.33%,the content was 99.92%,the melting point was 201.2℃~201.5℃,the sulfate was≤0.20%,the iron ion was≤10 mg/kg,the moisture was 0.25%.The process equipment was less corrosive and produced less hazardous waste,which met the requirements of industrial production.