Manufacture of a titanium-containing component for catalysts of the Ziegler-Natta type

Claim 1

A process for the manufacture of a titanium-containing component of a catalyst for the homopolymerization and copolymerization of α-monoolefins of 3 to 6 carbon atoms by the Ziegler-Natta method, by milling together (a) a titanium-containing compound of the general formula TiCl.sub.3.nAlCl.sub.3 where n is a number from 0.01 to 1, and (b) an ester of a total of 2 to 34 carbon atoms, which has the general formula ##STR3## where R 1 is (I) alkyl of 1 to 16 carbon atoms or (II) phenylalkyl of a total of 7 to 23 carbon atoms, up to 5 hydrogen atoms of the phenyl radical being unsubstituted or substituted by alkyl of 1 to 5 carbon atoms, and R 2 is (I) hydrogen, (II) alkyl of 1 to 18 carbon atoms, (III) phenylalkyl of a total of 7 to 23 carbon atoms, up to 5 hydrogen atoms of the phenyl radical being unsubstituted or substituted by alkyl of 1 to 5 carbon atoms, (IV) phenyl or (V) alkylphenyl of a total of 7 to 23 carbon atoms, up to 5 hydrogen atoms of the phenyl radical being unsubstituted or substituted by alkyl of 1 to 5 carbon atoms, individual radicals R 2 being identical or different when more than one is present, wherein (1) a vibratory ball mill producing a milling acceleration of from 30 to 80 m.sec. -2 is employed, (2) the mill is first charged with the titanium-containing compound (a), after which it may or may not be operated in the absence of a diluent at from -50 to +100° C. over a period of from 50° to 100 hours, then (3) whilst milling at a grist temperature of from -50° to +80° C. an amount of the ester (b) which corresponds to a molar ratio of aluminum in the titanium-containing compound (a) to ester (b) of from 1:5 to 1:0.5 is added continuously or at intervals, in the absence of a diluent, at a rate of from 0.01 to 200 ml/min per 2.5 kg of titanium-containing compound (a), thereafter (4) whilst being milled, the grist is brought to from +10° to +100° C. and is kept in this temperature range until from 5 to 85% of the aluminum trichloride originally present in a bonded form in the titanium-containing compound (a) has been eliminated from the latter, after which (5) is desired, the product obtained in accordance with (4) is washed with at least 0.6 times its amount by weight of a hydrocarbon which is liquid at standard temperature and pressure and boils below 150° C. at standard pressure and is dried, and then (6) the product obtained in accordance with (4) or (4) and (5) is milled, in the absence of diluents, for a period of from 5 to 60 minutes at from -50° to -10° C.