Trivalent titanium component prepn. for Ziegler-Natta catalyst system - by grinding titanium tri:chloride complex with ester and reacting with alcohol

摘要

In the prepn. of a new Ti(III)-component, (1), for Ziegler-Natta catalyst systems, a Ti-contg. cpd., (A), having formula TiCl3.nAlCl3 (where n is 0.01-1) is ground with a 2-34C ester, (B), having formula R1-O-CO-R2 or R1-O-CO-CR2=CHR2 (where R1 is 1-16C alkyl or 7-23C phenyl-alkyl in which the Ph gp. is opt. substd. by up to 5 1-4C alkyl gps.; R2 is H, 1-18C alkyl, 7-23C phenyl- alkyl or 7-23C alkyl-phenyl in which Pb is opt. substd. by up to 5 1-4C alkyl gps.). Specific grinding conditions are used. (B) is added to (A) in quantities corresponding to molar ratio Ti in (A) : (B) 1 : 1.5 to 1 : 0.01. A suspension of (i) 1 pt.wt. prod.; (ii) 0.5-20 pts.wt. hydrocarbon, (C), liq. under normal conditions and boiling below 150 deg.C; and (iii) a 1-20C alcohol, (D), having formula X(OH)y (where y is 1 or 2 and X is an aromatic, satd. aliphatic or cycloaliphatic hydrocarbyl gp.) is prepd. D-quantity is such as to set up molar ratio Ti in (A) : (D) 1 : 0.01 to 1 : 2. The suspension is then strongly stirred 5-120 min. at 40-140 deg.C and then cooled to 15-25 deg.C. The suspension is opt. mixed with an Al-contg cpd. (E) having formula Al(R8)x(Y)3-x (where x is 1-3; Y is Cl or R8; R8 is 1-12C alkyl). Quantities are such as to set up molar ratio OH gps. from (D) : alkyl gps. in (E) 1 : 0.005 to 1 : 2. The solid sepd. from the suspension is opt. washed with a hydrocarbon, liq. under normal conditions and boiling below 150 deg.C, and dried, to recover (I). The catalyst systems are used in 2-6C alpha-mono-olefin (co)polymerisation. Stereoregular polymers are obtd. in high yields. Fine grain proportion is reduced.