Patent GB-340001-A (GB)
Title: A prepared resin and method and apparatus for producing the same
IPC: C08F240/00
Filed: 1929-07-16
Abstract: Polymerized hydrocarbons.-A method of producing synthetic resins capable of being hardened to a hard amorphous solid, as distinct from an elastic caoutchouc-like material, comprises polymerizing a mixture of unsaturated hydrocarbons of varying degree of unsaturation as are present in a cracked distillate boiling below 180 DEG  C., said distillate being free from any substantial amounts of coumarone-indene constituents, by subjecting the mixture to the action of polymerizing or activitating agents of the type which will hydrolize with water to form acid (e.g. aluminium chloride), adding a compound containing a hydroxyl radicle and/or a neutralizing agent to the reaction mixture, and then distilling to remove volatile constituents and unacted-upon hydrocarbons from the resulting reaction products.  The cracked distillate is one containing a high proportion of unsaturated hydrocarbons, generally about 25 to 50 per cent, and mainly olefines and di-olefines, and the resins prepared are stated to be non-acid in reaction and unsaponifiable.  In addition to aluminium chloride <PICT:0340001/IV/1> as a polymerizing agent, the chlorides of metals as iron, boron, zinc, and tin are specified, and other compounds which may be used are benzene sulphonic acid, ethyl sulphate and aniline hydrobromide.  In operation the process described consists in polymerizing the cracked distillate, adding a water solution of alkali to neutralize the aluminium chloride present, and steam-distilling to remove the hydrocarbons not polymerized; the residue is then dissolved in a hydrocarbon solvent, such as benzol, alcohol or acetone is then added to precipitate the resin from the solution, and the precipitate dissolved and purified.  As shown, the distillate to be polymerized is fed through a pipe 30 into a container 10, provided with a cooling jacket 11, stirring mechanism 18, and condenser 20.  The distillate is stirred, pulverized aluminium chloride added from time to time, and the temperature maintained between 20 DEG  to 30 DEG  C.  After the conversion, the contents of the vessel 10 are transferred through a pipe 35 to a vessel 40 provided with a steam inlet pipe 41, a condenser coil 45 and a stirrer 43.  At the beginning of the distillation an excess of a water solution of alkali is added to neutralize the aluminium chloride.  After the steam distillation, the putty-like residue is dissolved in a hydrocarbon solvent and transferred through a pipe 55 to a vessel 62 equipped with a stirring mechanism 63.  Acetone or alcohol is then added through the pipe 65 to precipitate the resin, which forms the lower layer 68 and includes aluminium hydroxide and sodium chloride.  This layer is run into a vessel 72, provided with a reflux 77, benzol is added, and the vessel heated to effect solution of the resin. After filtering through a filter press 87 the resin solution is then distilled in a vessel 91 to recover the solvent, the residue being run into shallow pans 100 where the resin is allowed to cool and harden.  The resin may be further purified by suitable solvents to free it from some of the higher oils.