Patent GB-828926-A (GB)
Title: Control of polymerization processes
IPC: C08F2/00
Filed: 1956-07-18
Abstract: <PICT:0828926/III/1> Polymerization reactions using a catalyst, in which the density of the product is greater than the monomer feed, are controlled by regulating the catalyst feed rate by the density of the effluent product.  Preferably the density recorder mounted in the polymer discharge line, is of hygrometric or Y-ray type and automatically controls the catalyst feed at the desired rate previously determined by calibration with the reactants, diluents, temperatures and pressures required.  Detailed information on the polymerization of olefine mixtures is given with graphs; the process may be applied to C3-C8 olefins, e.g. isobutylene or methyl-2-butene-1, alone or with added vinyl aromatics or multi-olefines.  Tri-polymers are also referred to. An apparatus consists of two reactors 1, 2, Fig. 1, provided with cooling jackets and stirrers, the first reactor having a feed 9 for the monomers and solvent, and a feed 10 for the catalyst. The partly polymerized product flows through an outlet 14 to the second reactor, where polymerization is completed.  A density-measuring device 15, mounted in the outlet 11 is previously calibrated to read density directly in terms of percentage conversion of the product, and is electrically connected to a solenoid 17 which actuates the valve admitting catalyst to the reactor.  A series of reactors may be employed in which the supply of catalyst is controlled in all stages except the last.  U.S.A. Specification 2,274,749 is referred to.ALSO:<PICT:0828926/IV (a)/1> Polymerization reactions using a catalyst in which the density of the product is greater than the monomer feed, are controlled by regulating the catalyst feed rate by the density of the effluent product.  Preferably a density recorder of the hygrometric or g -ray type is mounted in the polymer discharge line, and automatically controls the catalyst feed at a desired rate previously determined by calibration with the monomers, diluents, temperatures and pressures required.  An example is given compiling data and graphing a polymerization.  The process may be applied to polymerizing C3-C8 olefines alone or with added vinyl aromatic hydrocarbons, multi-olefines and other materials copolymerizable therewith, e.g. indene, acrylonitrile or other acrylate derivatives or vinyl ketones.  The following polymers are referred to: (a) copolymers of C4-C8 iso-olefines with styrene; (b) tri-polymers of C4-C8 olefines or iso-olefines with vinyl aromatics and a minor amount of isoprene, or 1,3-butadiene, (c) homopolymers of C4-C10 iso-olefines, e.g. polyisobutylene.  The catalyst may be of Friedel-Crafts type (preferably dissolved in methyl chloride, saturated hydrocarbons, CS2, or low-boiling organic fluorides), metal alkyls, or boron fluoride.  In the production of tri-polymers a minor amount of benzoyl peroxide or sodium perborate is added.  Emulsion polymerization is also referred to.  A suitable apparatus comprises two reactors 1, 2, Fig. 1, provided with cooling jackets and stirrers 5, the first reactor having a feed line 9 for monomers dissolved in a solvent, and a feed 10 for a solution of the catalyst.  The partially polymerized product flows through a line 14 to the second reactor where polymerization is completed.  A density measuring device 15, mounted in the outlet 11, is previously calibrated to read density directly in terms of percentage conversion of the product, and is electrically connected to a solenoid 17 which actuates the valve admitting catalyst solution to the reactor.  A series of reactors may be employed in which the supply of catalyst is controlled in all except the last stage.  An example is given in which the monomer feed is a 15% solution in methyl chloride of equal parts of styrene and iso-butylene, using a catalyst feed of aluminium chloride in methyl chloride.  U.S.A. Specification 2,274,749 is referred to.