| 摘要 |
A process of treating dialkyl sulphoxides containing up to 6 carbon atoms to remove impurities, particularly those causing relatively high light absorbence at 270-300 mm comprises contacting a dialkyl sulphoxide with adsorptive carbon and separating the dialkyl sulphoxide from the carbon after contact and/or saturating dialkyl sulphoxide with an inert gas which will not interfere with the contemplated use of the dialkyl sulphoxide and which will impart to it lower light absorbence between 270-300 mm , when saturated therewith, than is imparted to the same dialkyl sulphoxide by saturation with air, by intimately contacting the dialkyl sulphoxide with the gas, thereby displacing the impurities into the atmosphere. Three main procedures may be adopted as follows: (a) the dialkyl sulphoxide is contacted with adsorptive carbon, rectified and the remaining portion of the distilland which would increase the 270-300 mm light absorbence of the distillate if allowed to distil over is separated as residue, (b) as in (a) above but following the separation the distillate is contacted with an inert gas to at least partially saturate the dialkyl sulphoxide and (c) contacting the dialkyl sulphoxide with adsorptive carbon, rectifying the dialkyl sulphoxide while maintaining the pressure below 80 mm. Hg. contacting the dialkyl sulphoxide, during rectification with an inert gas, separating the residue as in (a), relieving the pressure over the distillate to atmospheric and saturating the distillate with the inert gas. The contacting of the dialkyl sulphoxide with adsorptive carbon may be a multi-stage treatment, the carbon being filtered off at each stage. If an acid treated adsorptive carbon is used, the dialkyl sulphoxide should be treated with a base, such as an alkali or alkaline earth metal oxide, hydroxide or carbonate during or after the last carbon contact. In any case the acid impurities should be removed before distillation of the dialkyl sulphoxide. Dimethyl sulphoxide is preferred whilst suitable inert gases are nitrogen, carbon dioxide, helium, argon, petroleum ether, 1-butene, hydrogen, ethylene, propylene, ammonia and natural gas. Preferably a small stream of bubbles of the selected gas is introduced directly into the boiling distilland. In the case of dialkyl sulphoxides which contain odour-imparting impurities, the sulphoxide may be treated to remove such impurities at any time prior to the final rectification by contacting it with an immiscible extraction solvent. Suitable extraction solvents are petroleum ether, isooctane, hexane, kerosene and gasoline fractions of petroleum, dialkyl ethers preferably with water, aromatic hydrocarbons and halogenated hydrocarbons. |
