DE906487C - Process for the production of high-quality lubricating oils from high-molecular paraffins of the catalytic carbon dioxide hydrogenation - Google Patents

Description

Process for the production of high quality lubricating oils from high molecular weight Catalytic carbohydrate hydrogenation paraffins High-melting paraffins of any kind Origin can be processed in various ways on synthetic lubricating oils, the first step always being the production of olefin-rich hydrocarbon mixtures consists, which serve as the starting material for the polymerization. The necessary Olefins can be produced, for example, by cleavage. Here you get pretty much low boiling hydrocarbon mixtures; there are also not inconsiderable losses through gas formation and carbon deposition. Deliver during polymerization synthetic lubricating oils of this type are relatively low Viscosity.

Instead of splitting, the paraffins are already obtained by chlorination and subsequent elimination of chlorine converted into olefins, the elimination of chlorine was partially combined with the polymerization. Those from such olefins however, lubricating oils obtained from the chlorination products themselves did not show any satisfactory properties in terms of viscosity, viscosity pole height and pour point. In particular, it has so far not been possible to obtain lubricating oils, in spite of particularly high viscosity have a sufficiently low pour point.

It has been found that high-melting paraffins of the catalytic Caroxide hydrogenation with good yield on surprisingly high quality lubricating oils can be processed, if the chlorine addition and elimination of chlorine under conditions is working, which have not previously been used in this way and sequence. The accumulation of chlorine must be made according to the invention so that on the paraffins above their Melting point of elemental chlorine to the extent that it has an effect, up to per mole of paraffin a chlorine uptake of 0.9 to 1.5 moles of chlorine has taken place. The chlorinated paraffins obtained are then at 3oo to 400 'over one of silica (S102) and / or aluminum oxide (A1203) to conduct existing contact, which was previously longer than its sintering temperature was heated.

Due to the addition of chlorine under the conditions mentioned ur_d elimination results in unsaturated hydrocarbon mixtures, their olefinic Double bonds in an unforeseeable way are such that they Can be processed excellently well on lubricating oil. One receives in good yield Lubricating oils, which despite their relatively very high viscosity have a low Viscosity pole height and one that is sufficiently low for most purposes Possess pour point.

The production of lubricating oil can take place here with condensing agents known per se, for example with aluminum chloride, in the temperature range from 50 to 100 '. Because of the high viscosity of the resulting polymers, after the condensation has ended, they are diluted with heavy gasoline or other solvents, such as. B. with mineral spirits or chlorinated hydrocarbons (trichlorethylene), so that the polymerization layer can be separated from the contact residue with sufficient ease.

Further details can be found in the following exemplary embodiments. Embodiment 1 A soft paraffin from catalytic carbohydrate hydrogenation, which had a solidification point of 25 'and an average molecular weight of 268, was treated with gaseous chlorine at 90 to 10' until the resulting chlorination product contained 26.3% chlorine, which is a Chlorine uptake of 0.98 moles of chlorine per mole of paraffin corresponded. This chlorination is conducted at 35o ° with a space-time load of o, 0, containing 2 via a .geglühten at i25o ° contact of 94 ° / o S102 and 6 ° / o Al. For every 100 g of soft paraffin used, 98 g of an olefinic hydrocarbon mixture were obtained which had an iodine number of 122 and a residual chlorine content of 1.1%.

This olefin mixture was mixed with 5% anhydrous aluminum chloride and polymerized first for 6 hours at 50 ', then for a further 6 hours at 75' and finally again for 12 hours at 100 'with vigorous stirring. The reaction product obtained was diluted with hydrogenated heavy gasoline and left to stand for a long time. The polymer obtained was then separated from the aluminum chloride residue in order to treat it with 5% fuller's earth (trademark Tonsil) for a longer period of 100 to 120 minutes. The heavy gasoline and the portions boiling below 400 'were then distilled in vacuo. away. The end product was a lubricating oil with a viscosity of 93 'E (5o') while the viscosity pole height was 1.58 and the pour point was -22 °.

The soft paraffin used gave a yield of 70 % of the lubricating oil just identified. Embodiment 2 A paraffin from the catalytic carbon dioxide hydrogenation boiling above 300 °, which had an average molecular weight of 310 and a solidification point of 34 ', was chlorinated with constant stirring at 10' until the chlorination product contained 33.5% chlorine , which corresponded to a chlorine uptake of 1.4 moles of chlorine per mole of paraffin. The chlorination product obtained in this way was passed at 35 ° with a space-time loading of 0.2 over silica gel precipitated at 20 °, which in turn had been calcined for several hours at 120 '. This gave an olefinic hydrocarbon mixture which was almost free of chlorine and had an iodine number of 125.

This unsaturated hydrocarbon mixture was mixed with 5 ° / o anhydrous aluminum chloride, and then stir it vigorously for 24 hours to heat up to ioo '. The resulting polymerization product was with the the same volume of heavy petrol diluted. This was then separated by decanting Polymer from the contact oil layer and heated the former in a vacuum up to 400 ', with the heavy gasoline and the lower-boiling components distilling off. A high-quality lubricating oil with a viscosity remained as the distillation residue of 125 'E (5o'), a viscosity pole height of 1.60 and a pour point of -5 ° owned. From every 100 g of the paraffin used, 83 g of lubricating oil were obtained,

Claims (1)

PATENT CLAIM: A process for the production of high-quality lubricating oils from high molecular weight paraffins of the catalytic hydrocarbon hydrogenation, characterized in that the paraffins are treated with elemental chlorine at temperatures just above their melting point until the chlorine uptake reaches 0.9 to 1.4 moles of chlorine per mole of hydrocarbon whereupon the chlorinated paraffins obtained are dechlorinated between 300 and 400 ° via lumpy contacts containing S'02 and / or Al203, which were heated to temperatures above the sintering temperature before the treatment, and the dechlorinated products are polymerized between 50 and 100 ° with aluminum chloride , whereby the polymer layer is diluted with heavy gasoline or other solvents to separate the polymer layer. References: U.S. Patents Nos. 1 955 26o, 1 970 402, 2 077 78 1 , 2 0 82 2 0 3, 2 094 593; Soc. of Automotive Engineers 1931, pp. 40 to 44; Ind. And Eng. Chemistry 1931, pp. 604-611.