PATENTS

3113.----- [RUHRCHEMIE, A. G.]  [Process for the Improved Production of Esterlike High-Molecular Compounds of Waxy Nature.]  German Patent Appl. R 111,074, R 593, filed Sept. 22, 1941, (Cl. IV d-12 o).  TOM Reel 36, bag 3,454, item 36, 5 pp.; Meyer Transl. PC-S-IV. vol. 1, ch. 5, 1948, p. 12.

High-boiling hydrocarbon mixtures from such sources as petroleum paraffin,, lignite paraffin, montan wax, or synthetic paraffin from CO hydrogenation are oxidized with N₂-containing gases with addition of nitrosyl H₂SO₄, and toward the end of the reaction polyvalent alcohols are slowly added to the reaction mass without any change in the temperature.  The alcohols may be partly or wholly substituted by alkyl-, aryl-, chlorine-, sulfate, phosphate-, or amine-groups.  After the alcohols are added. the reactants  are treated for 1-2 hr. with nitrous gases.  During or after the reaction, waxy, oily, or fatty substances containing carboxyl groups are added, especially those that occur as residues in the catalytic conversion of water gas to olefinic hydrocarbon mixtures.  Example:  2,500 gm. of hard paraffin obtained from the hydrogenation of CO and having a solidifying point of 91° are mixed with 500 cc. of nitrosyl H₂SO₄ and then exposed at a temperature of 122° for 14 hr. to an hourly flow of 3,000 N l. of ammonia combustion gases, which contain 8.5% NO and  5% O₂.  After 14 hr. the gas flow is reduced to 100 N l. per hr.  During the period of 110 minutes, 1,600 gm. of a synthetic C₁₃ alcohol, obtained by the catalytic conversion of water gas to C₁₂ olefins, are introduced dropwise.  After the reaction is completed, the reactants are washed with H₂O.  There are obtained 3,480 gm. of an ivory-colored, waxlike product having a saponification number of 115, a neutralization number of 4.5 and a hydroxyl number of 12.  An almost pure ester is obtained, containing only about 20% of unsaponifiable compounds.