Patent GB-798453-A (GB)
Title: Process for separating normal paraffins from mixtures of hydrocarbons
Filed: 1954-09-23
Abstract: n-Paraffins are separated from mixtures thereof with non-straight chain hydrocarbons by treating the mixture with a solution of urea in a solvent (or so-called activator) which is substantially immiscible with the hydrocarbons, in the presence of an oil solvent which dissolves the hydrocarbons but not the urea, which does not form an adduct with urea and whose boiling point is below that of the activator, the activator and oil-solvent being nonsolvents for the adduct, separating the resulting paraffin-urea adduct by filtering or centrifuging, removing the oil solvent from the filtrate by distillation, whereupon the residual mixture breaks up into two layers, one consisting mainly of non-straight chain hydrocarbons and the other containing the bulk of the activator and decomposing the paraffin-urea adduct by heating it with the layer containing the bulk of the activator; this decomposition also yields two liquid layers, one consisting essentially of activator and urea which may be re-used for the formation of adduct, the other layer containing the separated n-paraffins.  The ratio of oil-solvent to activator is preferably such that the adduct formation occurs in a heterogeneous liquid system.  The activator may be water or an alcohol and the oil solvent may be a lower normal paraffin, a branched chain aliphatic or aromatic hydrocarbon or an organic halogen compound such as a chlorinated hydrocarbon, e.g. carbon tetrachloride, dichlorethane or methylene chloride.  Examples describe the removal of n-paraffins from a lubricating oil and from spindle oil by treating the mixed hydrocarbons with urea, methanol and methylene chloride in a highspeed mixer, centrifuging the product to remove the urea adducts, distilling the filtrate to remove the methylene chloride as an azeotrope with methanol part of which is used to wash the urea adduct and thereafter recycled with the remainder to the mixer, the stripped filtrate is passed to a settler, from which is withdrawn the oil layer of non-paraffinic hydrocarbons and the methanolic layer, the latter is heated at 80-100 DEG  C. with the urea-adduct to liberate the n-paraffins which are separated from the urea-enriched methanol which is recycled to the mixer.  The temperature in the mixer is held at adduct-forming level by vaporizing methylene chloride from the mixture by reducing the pressure.  Suitable apparatus is described for the process.ALSO:n-Paraffins are separated from oils containing both n-paraffins and non-straight chain hydrocarbons by treating the oil with a solution of urea in a solvent (a so-called activator) which is substantially immiscible with the hydrocarbons, in the presence of an oil solvent which dissolves the hydrocarbons but not the urea, which does not form an adduct with urea and whose boilingpoint is below that of the activator, the activator and oil-solvent being non-solvents for the adduct, separating the resulting n-paraffin urea adduct by filtering or centrifuging, removing the oil solvent from the filtrate by distillation wherein the residual mixture breaks up into two layers, one consisting mainly of nonstraight chain hydrocarbons and the other containing the bulk of the activator, and decomposing the paraffin-urea adduct by heating it with the layer containing the bulk of the activator; the decomposition mixture yields two layers, one consisting mainly of the n-paraffins and the other of a solution of urea in the activator which may be reused in the adduct formation.  The ratio of oil solvent to activator is preferably such that adduct formation is effected in a heterogeneous liquid system.  The activator may be water or an alcohol and the oil solvent a C1-5 n-paraffin, a branched-chain aliphatic or aromatic hydrocarbon or a halogenated hydrocarbon, especially a chlorinated hydrocarbon of the dewaxing type, such as carbon tetrachloride, methylene chloride or dichlorethane.  Examples describe the removal of n-paraffins from a lubricating oil and from spindle oil by treating the oils with urea, methanol and methylene chloride in a highspeed mixer, centrifuging the product to remove the urea adduct, distilling the filtrate to remove methylene chloride as its methanol azeotrope, part of which is used to wash the urea adduct and thereafter recycled with the remainder to the mixer, the stripped filtrate is passed to a settler from which is withdrawn the oil-layer of non-paraffinic hydrocarbons and the methanolic layer, the latter is mixed with the urea adduct and heated at 80-100 DEG  C. to liberate the n-paraffins which are removed and the residue of urea-enriched methanol and the latter is recycled to the mixer.  The temperature in the mixer is held at adduct forming level by vaporizing methylene chloride from the reaction mixture by reducing the pressure.  Suitable apparatus is described for the process.