# US 4,395,358 A · Titanium trichloride catalyst complex and process for the production thereof > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 4,395,358 A - Document ID: US4395358A - Status: Granted - Kind: A - Application number: 06/208,212 - Filed: 1980-11-19 - Granted: 1983-07-26 - Earliest claimed: 1977-06-30 - Assignees: Exxon Research & Engineering Co. - Inventors: Harry J. Wristers - Web page: https://patentgrep.com/patent/US4395358A ## CPC - C08F 10/00: Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond - C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS ## Abstract A titanium trichloride catalyst complex is produced by reducing titanium tetrachloride with an organo-metal compound and then activating the resulting reduced solids by treatment with a chlorinated hydrocarbon and titanium tetrachloride in the presence of a Lewis base complexing agent. The employment of the chlorinated hydrocarbon and titanium tetrachloride in the presence of the Lewis base complexing agent unexpectedly produces a synergistic effect whereby activating conditions, e.g., temperature, time and TiCl.sub.4 concentration can be employed resulting in a titanium trichloride complex having superior alpha-olefin polymerization properties as compared to titanium trichloride catalyst complexes obtained by treatment under the same conditions in the absence of either titanium tetrachloride or chlorinated hydrocarbon. Moreover, unexpectedly high yields of activated catalyst can be recovered without loss of activity. ## Claims ### Claim 1 An improved catalyst composition adaptable for use in a stereopolymerization of alpha-olefins comprising: (a) an organometal compound co-catalyst, in contact with; (b) a titanium trichloride composition catalyst, said titanium trichloride catalyst being produced by a process comprising: (i) in a reduction step, contacting titanium tetrachloride with an organo metal compound of the formula R.sub.n AlX.sub.3-n, wherein R is a group having 1 to 18 carbon atoms selected from alkyl or aryl, X is a halogen and n is a numeral within the range of 1.ltoreq.n.ltoreq.3 at about -50.degree. C. to about 100.degree. C. in an inert diluent to obtain a reduced solids product; (ii) in an activation step, contacting the reduced solids of (a) with a chlorinated hydrocarbon and a titanium tetrachloride in the presence of a Lewis base complexing agent, said chlorinated hydrocarbon, titanium tetrachloride and Lewis base complexing agent, respectively, being present in amounts of about 0.1 to about 10 mols chlorinated hydrocarbon, about 0.1 to about 2.0 mols titanium tetrachloride and about 0.1 to about 2.0 mols Lewis base complexing agent per one mol of titanium trichloride in such reduced solids of (a), and said titanium tetrachloride being in a concentration of about 2 to about 15 volume percent at an elevated temperature within the range of from about 50.degree. C. to about 150.degree. C. for about 5 minutes to about 10 hours until a crystal conversion of the reduced solids product of (a) is obtained; and (iii) in a recovery step, recovering the resulting activated reduced solids product as said titanium trichloride catalyst complex in high yield. ### Claim 2 (depends on 1) The improved catalyst composition of claim 1, wherein, in said process for producing said titanium trichloride catalyst, said activation step (ii) is carried out under conditions of elevated temperature, time and titanium tetrachloride concentration such that the recovered titanium trichloride catalyst complex of (iii) has alpha-olefin polymerization properties superior to titanium trichloride catalyst complexes obtained by treating the reduced solids of (i) under the same conditions of elevated temperature and time in the absence of said titanium tetrachloride or said chlorinated hydrocarbon. ### Claim 3 (depends on 1) The improved co-catalyst composition of claim 1, wherein in said process for producing said titanium trichloride catalyst, said activation step (ii) is carried out under conditions of elevated temperature, time and titanium tetrachloride concentration such that the activated reduced solids recovered in step (iii) is greater than the amount of titanium trichloride catalyst complexes obtained by treating the reduced solids of (i) under the same conditions of elevated temperature and time in the absence of said titanium tetrachloride. ### Claim 4 (depends on 1) The improved catalyst composition of claim 1, wherein, in said process for producing said titanium trichloride catlayst, the chlorinated hydrocarbon is selected from chlorinated saturated hydrocarbons, chlorinated unsaturated hydrocarbons or mixtures thereof, said chlorinated hydrocarbons having from 1 to 8 carbon atoms per molecule. ### Claim 5 (depends on 4) The improved catalyst composition of claim 4, wherein, in said process for producing said titanium trichloride catalysts said chlorinated hydrocarbon is one having a stable chlorine-carbon bond. ### Claim 6 (depends on 1) The improved catalyst composition of claim 1, wherein, in said process for producing said titanium trichloride catalyst, said Lewis base complexing agent is an ether selected from the group consisting of n-butyl ether, p-methyl anisole, di-iso-pentyl ether, di-n-pentyl ether, di-n-hexyl ether, anisole, propyl phenyl ether, and mixtures thereof. ### Claim 7 (depends on 6) The improved catalyst composition of claim 6, wherein in said process for producing said titanium trichloride catalyst, said chlorinated hydrocarbon is hexachloroethane. ### Claim 8 (depends on 7) The improved catalyst composition of claim 7, wherein in said process for producing said titanium trichloride catalyst, said hexachloroethane and said ether compound are respectively present in an amount of about 0.5 to about 1.0 mol ether and an amount of from about 0.7 to about 2.0 mol hexachloroethane, respectively, per one mol of titanium trichloride in said reduced solids of (i). ### Claim 9 (depends on 8) The improved catalyst composition of claim 8, wherein, in said process for producing said titanium trichloride catalyst, said activation steps (ii) is carried out at an elevated temperature within the range of from about 60.degree. C. to about 85.degree. C. ### Claim 10 (depends on 1) The improved catalyst composition of claim 1, wherein said organometal compound co-catalyst is selected from monoalkylaluminum dichloride, dialkylaluminum monochloride, trialkylaluminum or mixtures thereof.