Process for the separation of sulphuric acid from aqueous...

C - Chemistry – Metallurgy – 07 – C

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260/530.6

C07C 303/44 (2006.01) B01D 3/10 (2006.01) B01D 11/04 (2006.01) B01D 12/00 (2006.01) C01B 17/69 (2006.01) C01B 17/90 (2006.01) C07C 303/42 (2006.01) C07C 309/02 (2006.01) C07C 309/04 (2006.01)

Patent

CA 1297903

1. CASE 2437 "PROCESS FOR THE SEPARATION OF SULPHURIC ACID FROM AQUEOUS MIXTURES THEREOF WITH PARAFFIN-SULPHONIC ACIDS" Abstract The mixtures from which sulphuric acid must be separated according to the present invention are those which derive from the sulphoxidation of (C12-C18)-n- paraffins with SO2 and O2 in the presence of water and of U.V. light at a temperature comprised within the range of from 25 to 50°C, after the removal of n-paraffins, which separate spontaneously, and of SO2 excess, and after undergoing one of the following treatments: a) dehydration, by known systems of the residual mixture, at least until said mixture becomes cloudy (due to the formation of a biphasic system), extraction of not-sulphoxidated paraffins from the dehydrated, cloudy mixture, or from the supernatant phase of the biphasic system, with supercritical CO2, at a temperature comprised within the range of from 32°C to 80°C, under a pressure comprised within the range of from 75 to 350 bars, and with a CO2/paraffin- sulphonic acids weight ratio of from 1/1 to 50/1. b) addition of H2SO4 to the residual mixture, at least until said mixture becomes cloudy (due to the formation of a biphasic system), extraction with 2. supercritical CO2, from the cloudy mixture, or from the supernatant phase of the biphasic system, of the residual paraffins under such conditions as shown under (a); c) addition to the residual mixture of an aliphatic alcohol containing a number of carbon atoms lower than, or equal to, 4, preferably isopropanol, until a biphasic mixture is formed, extraction from said biphasic mixture of the residual paraffins, with supercritical CO2, under such conditions as reported under (a). The mixture of paraffin-sulphonic acids free, or substantially free, from paraffins, obtained by means of the above disclosed treatments from (a) to (c) (the "refined mixture") still contains, besides the paraffin- sulphonic acids, a considerable amount of H2SO4. In order to remove said sulphuric acid, according to the process of the present invention, the refined mixture is mixed with one or more halogenated solvent(s), possibly in mixture with H2SO4, in such way a separation being obtained of water and sulphuric acid from the refined mixture, and the residual mixture is finally submitted to evaporation, for the removal of the halogenated solvent(s), which are used again, concentrated paraffin-sulphonic acids being obtained.

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