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United States Patent 0 Ice Patented Nov 1 3,216,982 United States Patent 0 ice Patented Nov. 9, 1965 1 2 are halides of Groups IVa, Va or VIa metals such as 3,216,982 titanium tetrachloride, zirconium tetrachloride, vanadium CATALYSTS FOR POLYMERIZATIGN tetrachloride and titanium tetraiodide, and oxyhalides Adam Orzechowski, Waltham, and James C. Mac-Kenzie, such as vanadium oxychloride and chromium oxychlo Wellesley Hills, Mass, assignors to Cabot Corporation, ride. Boston, Mass, a corporation of Delaware The conditions under which reaction between the tran No Drawing. Filed Mar. 28, 1963, Ser. No. 268,589 The portion of the term of the patent subsequent to sition metal halide and the ?nely-divided inorganic solid Jan. 18, 1982, has been disclairned can be accomplished are subject to considerable varia 23 Claims. (Cl. 260—88.2) tion as explained in detail in Serial No. 2,861, for ex 10 ample. However, in order to obtain a catalyst com This invention relates to the polymerization and co ponent with exceptionally high activity and reproducible polymerization of mono-ole?ns and/or di-ole?ns such as character it has been found to be all important that the ethylene, propylene, butene-l, styrene, isoprene and buta ?nely-divided inorganic solid be essentially dry and anhy diene and includes within its scope improved catalysts drous (i.e. free of molecular water in any form) at the for the polymerization of the aforementioned classes of time it is brought into contact with the transition metal monomers. halide. In addition, it is recommended that said reaction This case is a continuation in part of copending ap be achieved so as to allow by-products of the reaction plications, Serial No. 2,861, ?led January 18, 1960, and (for example, HCl) to be eliminated from the reaction Serial No. 21,110, ?led April 11, 1960, both by Orze~ zone in order to insure that said reaction goes to com 'chowski and MacKenzie, and both now abandoned. 20 pletion. Generally, said reaction can be carried out by It is a principal object of the present invention to contacting said inorganic solid with said transition metal provide a process for the polymerization of mono-, di-ole halide, preferably in a solution thereof in an inert hydro ?ns and mixtures thereof. carbon medium, and maintaining the two reactants in It is another object of this invention to provide novel intimate contact for a period of time sufficient to effect catalysts for the polymerization of mono-, di-ole?ns and the desired chemical reaction resulting in the chemical mixtures thereof. bonding of the transition metal to the inorganic solid. Other objects of this invention will in part be obvious The length of time required to effect a given amount of and will in part appear hereinafter. such reaction and chemical bonding is largely dependent Said copending applications disclose catalyst com upon the temperature of the reaction mixture. Generally ponents suitable for use in the polymerization and co- ‘ speaking, ‘almost ‘any temperature between about 0° C. polymerization of mono- and di-ole?ns, which com and about 300° C. can 'be used satisfactorily, but room ponents comprise the product of the metathetical reac temperature to about 105° C. is generally de?nitely pre tion carried out under certain conditions between a ferred. Assuming provision is made for intimate con halide-type compound of a Group IVa, Va or VIa metal tact of the dry inorganic solid and the transition metal and hydroxyl groups on the surface of a ?nely-divided 35 halide, the minimum time required to accomplish the particulate inorganic solid. In accordance with the chemical reaction needed will vary from periods of about present invention, it has been discovered that excellent 10 hours at room temperature to periods of about 15 polymerization catalysts are obtained when said catalyst minutes at temperatures of 100° C. or over. Tempera components are combined, under suitable conditions, with tures higher than about 300° C., e.g. 500° C., are com certain organometallic compounds comprising germa 40 pletely needless and therefore of little or no interest. nium, tin or lead. Elimination of by-products of the reaction from the The polymerization and copolymerization of the mono reaction zone, i.e. the reaction medium, can be accom and/or di-ole?ns can be effected at suitable tempera plished in many ways, such as by sweeping the reaction tures within the range of from about -—25° C. to about vessel with an inert gas, by carrying out the reactionat 250° C., and pressures ranging upwardly from about su?iciently elevated temperatures to drive by-products atmospheric pressures to any desired maximum pressure, out of the reaction zone, i.e. usually out of the reaction for example, 30,000 p.s.i.g. or even higher pressures. medium, or by complexing or reacting said by-products Inorganic solids suitable for the purposes of the present with suitable substances such as tertiary arsines, tertiary invention generally include any inorganic compound phosphines, terpenes, terpinenes, tetrasubstituted hydra which is available in ?nely-divided particulate form with 50 zines, carbides such as calcium carbide, and other sub hydroxyl groups on the surface thereof. For example, stances such as sodium hydride which Will react orcom oxides such as alumina, zirconia and silica, silicates such plex with said by-products and thereby eliminate them. as chrysotile, and aluminates such as corundum are all Organometallic compounds suitable for the purposes generally suitable for the purposes of the present inven of the present invention are those compounds conforming tion. For best results, however (as explained in detail 55 to the empirical formula in said copending application Serial No. 2,861), inorganic solids having an average particle diameter of less than about 0.1 microns are de?nitely preferred. Halide-type compounds of Group IVa, Va or VIa 60 (hereinafter generally referred to as transistion metal wherein each R is chosen from the group consisting of halides) suitable for the purposes of the present inven monovalent hydrocarbon radicals, monovalent alkoxy tion, are compounds conforming to the general empirical radicals, monovalent aryloxy radicals, and the halogens; formula p is a number from 0 to 3; each H is a hydride radical; TOaXb 65 t is a number from 1 to 4; M is a quadrivalent metal wherein T is a metal of Groups IVa, Va or VIa (where chosen from the group consisting of germanium, tin the group numbers correspond to the Mendeleev Periodic and lead; and O is oxygen. System); 0 is oxygen; a is number from 0 to 2; each Speci?c examples of R groups for substitution in the X is any halogen; and b is a number from 1 to 6. above formula include methyl, 2-methyl-2-butenyl, n Examples of suitable compounds conforming to said 70 dodecyl, 4~cyclohexylethyl, methylnaphthylethyl, 2,2,1 general formula bicycloheptyl, tolyl, xylyl, xenyl, methoxy, isobutoxy, n T0,,Xb octyloxy, phenoxy and 1,2-naphthoxy. 3,216,982 3 4 Speci?c examples of compounds conforming to the catalyst utilized, the speci?c type of product desired, and formula: the extent of monomer conversion desired in any given run or pass over the catalyst. In general, this variable is readily adjustable to obtain the desired results. There follow a number of illustrative non-limiting ex amples: which are suitable for the purposes of the present inven tion are: trimethylstannane, (CH3)3SnH; triphenylstan Example 1 nane, (C6H5)3SnH; dimethylstannane, (CH3)2SnH2; tri ethylgermane, (CZH5)3GeH; triphenylgermane, To a 2000 milliliter, three neck, glass reaction vessel 10 there is added 20 grams of “Cab-O-Sil,” a pyrogenic (csHsl sGeH silica produced by Cabot Corporation, which has an av tri-a-naphthyl-germane, (a-C1°H7)3G€H; tri-n-hexylger erage particle diameter of 10 millimicrons and a hy mane, (n-CGH1’3)3GeH; di-i-propylgermane, droxyl group content on the surface thereof of about 1.5 15 milliequivalents per gram. To said reaction vessel there is added 1700 milliliters of benzene, and the resulting plumbane, PbH4', germane, Gel-I4; stannane, SnH4; 1,2 slurry is dried by being heated to, and maintained at, dihydrotetramethylstannoxane, (CH3) 2HSnOHSn(CH3) 2; the boiling point of benzene, i.e. about 80° C., for about and the like. 20 hours, while a water/benzene azeotrope is removed The catalysts of the present invention are formed when 20 from. the reaction vessel by periodic distillation until the product of the metathetical reaction (as described about 450 milliliters of distillate has been removed. The above) of hydroxyl groups in the surface of an inorganic vessel is then cooled and charged with 20 millimoles of solid and a transition metal halide is combined in an titanium tetrachloride. The contents of the vessel are inert environment with an organometallic compound at then continuously stirred, and maintained at re?uxing temperatures normally between about 0° C. and about temperature (about 80° C.) for about 6 hours while the 150° C. and at atmospheric pressure, although higher contents of the gas phase are swept by a stream of dry temperatures and pressures can be utilized. Thetem nitrogen. Subsequently, the extent of the reaction be peratures and/ or pressures that are most desirably utilized tween the titanium tetrachloride and the hydroxyl groups with any particular combination of components can be in the surface of the silica is determined by measuring readily determined bearing in mind that temperatures and/ the quantity of HCl that was removed by the dry nitrogen or pressures that cause substantial decomposition of either of the components of the catalyst should be avoided. stream and by testing the liquid contents of the vessel Using the catalysts of this invention, polymerization for the absence therein of titanium tetrachloride, and of mono-ole?n and/ or di~ole?n monomers can be accom said slurry is found to contain 20 milliatoms of titanium plished in the absence of liquids (other than the monomers chemically bound to the surface of said silica.
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