| 摘要 |
PURPOSE:To increase the yield of thiophosgene by adding perchloromethyl mercaptan to a mixture of an aq. H2SO3 soln., an org. solvent and an acid in the presence of one or >=2 kinds of catalysts among S2Cl2, SCl2, an alkali iodide and I2 to cause a reaction. CONSTITUTION:From 0.4 to 9 pts.wt. of an org. solvent such as dichloromethane based on 1 pt.wt. of perchloromethyl mercaptan(PCMM), 0.1-6N concn. mixture of one or >=2 kinds of acids among HCl, H2SO4, etc., and a 0.5-3.0mol% of a mixture of one or >=2 kinds among S2Cl2, SCl2, an alkali metal iodide such as KI and I2 as catalyst based on PCMM are mixed into an aq. H2SO3 soln. at >=4wt.% concn. obtained by dissolving gaseous SO2 in the water in a reactor and having <=90wt.% saturation solubility. PCMM is added to the liq. mixture at 0-60 deg.C while agitating the mixture to cause a reaction. After PCMM is added, the mixture is aged for about 0.5-8hr, and thiophosgene is safely obtained in high yield. |
