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 ether which contains a total of from 4 to 30 carbon atoms and has the general formula R.sup.1 -- O -- R.sup.2 where R 1 and R 2 are identical or different and each is open-chain alkyl of 1 to 15 carbon atoms, phenyl or alkylphenyl, where alkyl is of 1 to 8 carbon atoms, 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 0.5 to 100 hours, then (3) whilst milling at a grist temperature of from -50° to +80° C., an amount of the ether (b) which corresponds to a molar ratio of aluminum in the titanium-containing compound (a) to ether (b) of from 1:5 to 1:0.5 to 1:0.05 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 6 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) 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, then (6) the product obtained in accordance with (5) is dried and milled, in the absence of diluents, for a period of from 5 to 60 minutes at from -50 ° to +10° C., subsequently (7) the product obtained in accordance with (6) is suspended in from 0.5 to 60 times its amount by weight of a hydrocarbon which is liquid at standard temperature and pressure and boils below 150° C. at standard pressure, thereafter (8) the suspension obtained in accordance with (7) is mixed with the ether (b) in such amount that a molar ratio of titanium from the titanium-containing compound (a) to ether (b) of from 1:0.5 to 1:5 results and the batch is agitated vigorously for a period of at least 5 minutes at from 0° to 90° C., thereupon (9) the solid is isolated from the suspension obtained in accordance with (8) and is washed with at least an equal amount by weight of a hydrocarbon which is liquid at standard temperature and pressure and boils below 150° C. at standard pressure, and thereupon (10) the product obtained in accordance with (9) is dried and milled, in the absence of diluents, for a period of from 5 to 60 minutes at from -50° to +10° C.