Patent GB-974298-A (GB)
Title: Improvements in the sulphonation and sulphation of organic compounds
IPC: C07C303/24
Filed: 1961-05-24
Abstract: <PICT:0974298/C1/1> <PICT:0974298/C1/2> A continuous process for sulphonating a sulphonatable organic compound comprises causing a liquid film of the organic compound to flow down the inside of a substantially vertical wall defining a reaction zone, forming a pressurized gaseous mixture of 1 part by volume sulphur trioxide to 5-50 parts of an inert gas, introducing this gaseous mixture into the reactor and impinging it upon the flowing film at a sufficient velocity to produce marked turbulence in the film and substantially instantaneous exothermic reaction of the sulphur trioxide and organic compound, but without producing pressure pulsations, and cooling the wall so as to cool the film to a temperature low enough to prevent formation of undesired coloured by-products but high enough to maintain the viscosity of the film low enough to permit the film to flow freely down the wall and to undergo the turbulence.  (The terms "sulphonating" and "sulphonatable" are used to include "sulphating" and "sulphatable" respectively).  The cooling of the film is controlled, preferably, such that the viscosity of the film is maintained at 1 to 20 cps.  The sulphonation process may be carried out in a tubular reactor or a plurality of such reactors. Fig. 2 represents a side elevational view of a suitable sulphonation apparatus comprising a single reactor tube 18.  Fig. 3 presents a more detailed view of the upper end of the reactor, where the reactants are introduced into the reaction zone.  The reactor tube is surrounded by heat exchange means comprising chambers 12c, 13c and 14c, through which steam or water may be circulated.  The film of sulphonatable material 40 is introduced into the reaction zone by means of the jet nozzle 29, and is impinged by blasts of the sulphur trioxide-inert gas mixture 41 emanating from the nozzle 31. The inert gas used with the sulphur trioxide may be dry air, nitrogen, carbon dioxide, carbon monoxide, sulphur dioxide, a halogenated paraffin or a low molecular weight paraffin, or a mixture thereof with other inert gases, such as hydrocarbon cracking by-products. Compounds suitable for sulphonation include phenols and alkyl-phenols; aromatic hydrocarbons such as those containing a benzene, naphthalene, phenanthrene or anthracene nucleus; aliphatic and cycloaliphatic alcohols; heterocyclic compounds such as thiophene and pyridine; olefins such as octene and decene; cycloolefins and their alkyl derivatives such as cyclohexene and ethylcyclohexene; ethers and esters such as phenyl methyl ether, methyl esters and the fatty acid glycerides; acids such as benzoic acid; and various derivatives of the above compounds containing substituents such as halo, nitro, amino, keto and carboxyl groups.  The compounds sulphonated in the examples are (1) dodecylbenzene (2) lauryl alcohol, the sulphated product being converted to the sodium salt (3) ethoxylated lauryl alcohol, the sulphated product being converted to the sodium salt and bleached with hydrogen peroxide (4) and (5) ethoxylated nonylphenol, the sulphated product being neutralized with ammonium hydroxide and (6) a mixture of methyl palmitate and methyl stearate, the product being a mixture of a -sulpho ester and a -sulpho carboxylic acid.