Patent GB-413007-A (GB)
Title: Improvements in the manufacture and production of resins
IPC: C08F240/00
Filed: 1932-12-12
Abstract: Liquid unsaturated hydrocarbons or mixtures containing them are polymerized in presence of anhydrous inorganic agents of the Friedel-Crafts-type, the product dissolved in an organic oxygen-containing solvent boiling above 80 DEG  C., and solid fusible resins separated from the solution.  Polymerization may be effected as described in Specification 340,001.  Polymerizing agents specified are chlorides of aluminium, iron, zinc, tin, antimony, indium, titanium, boron fluoride, or an addition compound of aluminium chloride and an olefine, for example ethylene.  These are preferably removed from the polymerization products before further treatment, by the action of water or aqueous alkali, the residue being distilled, for example up to 300 DEG  C., first at ordinary pressure and later in vacuo, the distillate being worked up to motor fuels or lubricating oils. The residue is dissolved in the aforesaid solvents such as alcohols or ketones, particularly butyl or amyl alcohols, or mixtures of these, hexyl or heptyl alcohols, or cyclohexanol or cyclohexanone, if necessary while warming, and the solution treated with decolourizing agents such as carbon and, if desired, zinc dust. After filtering, the resin is separated by cooling, partially evaporating and cooling, or by adding a precipitant such as methyl or ethyl alcohol, acetone, or methyl ethyl ketone.  The resin may be separated in fractions by successive additions of small amounts of the precipitant liquid, or by successive evaporation and cooling steps.  The treatment with solvents and precipitants may be repeated or the resin dissolved in an oxygenfree solvent, such as benzene or petroleum ether, the solution decolourized, evaporated, and the residue fused in vacuo. The products may be employed in the manufacture of lacquers and artificial compositions.  The initial liquid hydrocarbons may be obtained by high temperature polymerization of gaseous unsaturated hydrocarbons, by cracking liquid paraffins, or by converting gaseous paraffins, obtained from natural gases or the hydrogenating cracking of mineral oils, coals or tars, into olefines in apparatus lined with silicon, and then polymerizing in similar apparatus, for example at 450--600 DEG  C. and 25 atmospheres.  Liquid olefines having a boiling range of 25--75 DEG  C. or 160--200 DEG  C. may, for example, be employed.  In an example, a benzine boiling up to 210 DEG  C. and made by polymerizing a cracking gas at 550 DEG  C. and 70 atmospheres is added to a solution of aluminium chloride-ethylene compound in a middle oil boiling at 200--300 DEG  C., obtained by distilling earlier batches from the polymerization, and containing about 5 per cent by weight of aluminium chloride calculated on the benzine.  The mixture is stirred and then heated to 100--120 DEG  C., aluminium chloride washed out, the liquid products distilled off and 1 part of the residue dissolved at 90 DEG  C. in 5 parts of isobutyl alcohol, animal carbon added and the solution filtered.  The resin is precipitated by cooling or addition of methanol.  It is purified by re-dissolving and precipitating, dissolving in petroleum ether, treating with bleaching earth, and finally fusing.  Liquid olefines obtained according to Specifications 336,234, and 376,397, [Class 2 (iii)], may be similarly employed.