Preparation of chlorosulfonic acid
Preparation of chlorosulfonic acid from sulphur trioxide and hydrochloric acid
To the round bottom flask fitted with gas inlet tube and condenser 200 g oleum (containing 38-40% free sulphur trioxide) is placed. To the bottom of the reaction flask, a current of dry hydrochloric acid is bubbled in. When absorption of the hydrochloric acid stops, the product is distilled. The distilled chlorosulfonic acid is generally slightly colored. Further purification could be performed by redistillation. The yield is almost theoretical. It is a colorless liquid which boils at 153-156° C with partial decomposition.
The war gases chemistry and analysis, by M. Sartory, 256, 1939.
Preparation of chlorosulfonic acid from sulfuric acid and phosphorus pentachloride
Thirty millilitres of concentrated sulfuric are mixed with an equal volume of 15-20% oleum and 100 g of the mixture is transferred to a 500 ml round ground-glass flask under the hood. Seventy-five grams of phosphorus pentachloride are added in small portions from a porcelain or glass spatula; the reaction mixture warms up and large quantities of hydrogen chloride escape. When all phosphorus pentachloride has been added, the solution is gently heated until the evolution of hydrogen chloride has ceased; care must be taken not to overheat it; otherwise some product may be lost through volatilization. The material is then distilled, using an air condenser, until the temperature of the vapor reaches 165° C; the receiver consists of a 250 ml round flask protected from moisture. As the acid attacks cork and rubber readily an all-glass apparatus must be used. The crude product is redistilled from the receiver and the colorless liquid is collected at 149-154°C; pure chlorosulfonic acid boils at 153 °C and must be kept in tightly sealed all-glass vessels. Yield 60-75 g.
Inorganic laboratory preparations, by G. G. Schlessinger, 139-140, 1962
Chlorosulfuric acid, CHLOROSULFONIC ACID, Chlorosulphuric acid, Sulfuric chlorohydrin, 7790-94-5, Chlorosulphonic acid, sulfurochloridic acid, Monochlorosulfuric acid, Sulfonic acid, monochloride, HSDB 909, EINECS 232-234-6, UN1754, sulfochloride, chloranesulfonic acid, chloro sulfonic acid, chloro sulfuric acid, Chloridosulfonic acid, Chloridosulfuric acid, Chlorinesulfonic acid, chloro sulphonic acid, sulfurochloridoic acid, Chloridosulphonic acid, Chlorinesulphonic acid, AC1L2NKP, AC1Q3VQI, AC1Q7DNB, UNII-2O9AXL1TJ4, 2O9AXL1TJ4, 26388_FLUKA, CTK2H7597, MolPort-000-872-004, XTHPWXDJESJLNJ-UHFFFAOYSA-N, 571024_SIAL, SBB040847, AKOS000269020, KB-48888, LS-53025, C1788, monochlorosulfuricacid;sulfonicacid,monochloride, 3B4-1619, I04-1469, Chlorosulfonic acid (with or without sulfur trioxide), Chlorosulfonic acid (with or without sulfur trioxide) [UN1754] [Corrosive], Chlorosulfonic acid (with or without sulfur trioxide) [UN1754] [Corrosive], 127529-03-7