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Titanium trichloride catalyst and process for the production thereof

Assignee: Tonen General Sekiyu KK
•
Filing: 1979-02-09
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Granted: 1980-01-08
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Expires: 1999-02-09
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Abstract

Abstract A titanium trichloride catalytic complex is produced by reducing titanium tetrachloride with an organo-metal compound and then treating the resulting reduced solids product with a chlorinated saturated hydrocarbon having two carbon atoms in the presence of a complexing agent. The resulting titanium trichloride complex composition, when employed as a co-catalyst with an organo-metal compound for Ziegler-type catalysts in polymerization of alpha -olefins, results in uniform polymer grains with unexpectedly high polymerization activity and high stereoregular polymer yielding ratios.

Inventors

  • 👤 Hiroshi Ueno
  • 👤 Naomi Inaba
  • 👤 Tukuo Makishima
  • 👤 Koh Watanabe
  • 👤 Shozo Wada

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-26 13:20
CPC Classifications
C; C08; C08F; C08F10/00

Claims Analysis

Total Claims: 39
Claim 1
Independent Claim 137 words
A process for the production of a titanium trichloride catalyst comprising: reducing titanium tetrachloride with an organo metal compound of the formula R n AlX 3-n wherein R is an alkyl or aryl group having 1 to 18 carbon atoms, X is a halogen atom, and n is a numeral within the range of 1≦n≦3, at a temperature of from about -50° to about +30° C. to produce a reduced solids product; contacting said reduced solids product with a chlorinated saturated hydrocarbon having 2 carbon atoms in the presence of a complexing agent selected from an aliphatic ether compound having 4 to 16 carbon atoms at an elevated temperature of about 60° C. to about 100° C. for about 1 to about 10 hours; and recovering the resulting treated reduced solids product as a titanium trichloride catalyst.
Claim 2
Dependent Claim 137 words
A process for the production of a titanium trichloride catalyst comprising: reducing titanium tetrachloride with an organo metal compound of the formula R n AlX 3-n wherein R is an alkyl or aryl group having 1 to 18 carbon atoms, X is a halogen atom, and n is a numeral within the range of 1≦n≦3, at a temperature of from about -50° to about +30° C. to produce a reduced solids product; contacting said reduced solids product with a chlorinated saturated hydrocarbon having 2 carbon atoms in the presence of a complexing agent selected from an aliphatic ether compound having 4 to 16 carbon atoms at an elevated temperature of about 60° C. to about 100° C. for about 1 to about 10 hours; and recovering the resulting treated reduced solids product as a titanium trichloride catalyst.
Claim 3
Dependent Claim 57 words
The process of claim 1, wherein said reduced solids product is contacted with the chlorinated hydrocarbon in a ratio of about 0.2 to about 3.0 mols chlorinated hydrocarbon per 1 gram atom of titanium, and with said complexing agent at a ratio of about 0.1 to about 2.5 mols complexing agent per 1 gram atom of titanium.
Claim 4
Dependent Claim 22 words
The process of claim 1, wherein the reduced solids product is contacted with a mixture of the chlorinated hydrocarbon and complexing agent.
Claim 5
Dependent Claim 17 words
The process of claim 1, wherein the reduced solids product is first mixed with the chlorinated hydrocarbon.
Claim 6
Dependent Claim 44 words
The process of claim 1 wherein the reduced solids product is first mixed with the complexing agent at an elevated temperature of about 20° to about 90° C. for about 30 minutes to about 3 hours prior to the addition of said chlorinated hydrocarbon.
Claim 7
Dependent Claim 26 words
The process of claim 5, wherein the reduced solids product is separated from the complexing agent after mixture therewith and then mixed with the chlorinated hydrocarbon.
Claim 8
Dependent Claim 23 words
The process of claim 1, wherein the complexing agent is an ether selected from di-n-butyl ether, di-n-amyl ether, diisoamyl ether, or mixtures thereof.
Claim 9
Dependent Claim 19 words
The process of claim 1, wherein the chlorinated hydrocarbon is selected from hexachloroethane, pentachloroethane, tetrachloroethane, dichloroethane, and mixtures thereof.
Claim 10
Dependent Claim 11 words
The process of claim 8, wherein said chlorinated hydrocarbon is hexachloroethane.
Claim 11
Dependent Claim 11 words
The process of claim 8, wherein said chlorinated hydrocarbon is pentachloroethane.
Claim 12
Dependent Claim 11 words
The process of claim 8, wherein said chlorinated hydrocarbon is tetrachloroethane.
Claim 13
Dependent Claim 11 words
The process of claim 8, wherein said chlorinated hydrocarbon is dichloroethane.
Claim 14
Dependent Claim 131 words
A process for producing a titanium trichloride catalyst comprising: (a) reducing titanium tetrachloride with an alkylaluminum chloride compound having from 2 to 6 carbon atoms at a temperature of about -50° C. to about +30° C. for about 30 minutes to about 3 hours to produce a brown to red violet reduced solids product containing β-type TiCl 3 ; (b) contacting said reduced solids product with a chlorinated saturated hydrocarbon having 2 carbon atoms in the presence of a complexing agent selected from an aliphatic ether compound having 4 to 16 carbon atoms at an elevated temperature of about 60° C. to about 100° C. for about 1 hour to about 10 hours; and (c) recovering the resulting treated reduced solids product formed in step (b) as said titanium trichloride catalyst.
Claim 15
Dependent Claim 131 words
A process for producing a titanium trichloride catalyst comprising: (a) reducing titanium tetrachloride with an alkylaluminum chloride compound having from 2 to 6 carbon atoms at a temperature of about -50° C. to about +30° C. for about 30 minutes to about 3 hours to produce a brown to red violet reduced solids product containing β-type TiCl 3 ; (b) contacting said reduced solids product with a chlorinated saturated hydrocarbon having 2 carbon atoms in the presence of a complexing agent selected from an aliphatic ether compound having 4 to 16 carbon atoms at an elevated temperature of about 60° C. to about 100° C. for about 1 hour to about 10 hours; and (c) recovering the resulting treated reduced solids product formed in step (b) as said titanium trichloride catalyst.
Claim 16
Dependent Claim 14 words
The process of claim 13, wherein said alkylaluminum chloride compound contains diethyl aluminum chloride.
Claim 17
Dependent Claim 19 words
The process of claim 14, wherein the chlorinated hydrocarbon is selected from hexachloroethane, pentachloroethane, tetrachloroethane, dichloroethane, and mixtures thereof.
Claim 18
Dependent Claim 27 words
The process of claim 15, wherein the complexing agent is an ether selected from the group consisting of di-n-butyl ether, di-n-amyl ether, diisoamyl ether, and mixtures thereof.
Claim 19
Dependent Claim 52 words
The process of claim 16, wherein said reduced solids product is contacted with said chlorinated hydrocarbon and said ether in an amount of from about 0.2 to about 3.0 mols chlorinated hydrocarbon per 1 gm atom of titanium, and about 0.1 to about 2.5 mols ether per 1 gm atom of titanium.
Claim 20
Dependent Claim 41 words
The process of claim 17, wherein said reduced solids product is contacted with said chlorinated hydrocarbon in the presence of said ether at an elevated temperature of about 65° C. to about 90° C. for about 1 to about 10 hours.
Claim 21
Dependent Claim 11 words
The process of claim 18, wherein the chlorinated hydrocarbon is hexachloroethane.
Claim 22
Dependent Claim 11 words
The process of claim 18, wherein the chlorinated hydrocarbon is pentachloroethane.
Claim 23
Dependent Claim 11 words
The process of claim 18, wherein the chlorinated hydrocarbon is tetrachloroethane.
Claim 24
Dependent Claim 11 words
The process of claim 18, wherein the chlorinated hydrocarbon is dichloroethane.
Claim 25
Dependent Claim 11 words
The titanium trichloride catalyst produced by the process of claim 19.
Claim 26
Dependent Claim 11 words
The titanium trichloride catalyst produced by the process of claim 20.
Claim 27
Dependent Claim 11 words
The titanium trichloride catalyst produced by the process of claim 21.
Claim 28
Dependent Claim 11 words
The titanium trichloride catalyst produced by the process of claim 22.
Claim 29
Dependent Claim 166 words
An improved Ziegler-type catalyst composition adaptable for use in an α-olefin polymerization, 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) reducing titanium tetrachloride with an organo metal compound of the formula R n AlX 3-n wherein R is an alkyl or aryl group having 1 to 18 carbon atoms, X is a halogen atom, and n is a numeral within the range of 1≦n≦3, at a temperature of from about -50° to about +30° C. to produce a reduced solids product; (ii) contacting said reduced solids product with a chlorinated saturated hydrocarbon having 2 carbon atoms in the presence of a complexing agent selected from an aliphatic ether compound having 4 to 16 carbon atoms at an elevated temperature of about 60° C. to about 100° C. for about 1 to about 10 hours; and (iii) recovering the resulting treated reduced solids product as a titanium trichloride catalyst.
Claim 30
Dependent Claim 166 words
An improved Ziegler-type catalyst composition adaptable for use in an α-olefin polymerization, 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) reducing titanium tetrachloride with an organo metal compound of the formula R n AlX 3-n wherein R is an alkyl or aryl group having 1 to 18 carbon atoms, X is a halogen atom, and n is a numeral within the range of 1≦n≦3, at a temperature of from about -50° to about +30° C. to produce a reduced solids product; (ii) contacting said reduced solids product with a chlorinated saturated hydrocarbon having 2 carbon atoms in the presence of a complexing agent selected from an aliphatic ether compound having 4 to 16 carbon atoms at an elevated temperature of about 60° C. to about 100° C. for about 1 to about 10 hours; and (iii) recovering the resulting treated reduced solids product as a titanium trichloride catalyst.
Claim 31
Dependent Claim 69 words
The improved Ziegler-type catalyst composition of claim 27, wherein, in said process for producing said titanium trichloride catalyst, said reduced solids product is contacted with the chlorinated hydrocarbon in a ratio of about 0.2 to about 3.0 mols chlorinated hydrocarbon per 1 gram atom of titanium, and with said complexing agent at a ratio of about 0.1 to about 2.5 mols complexing agent per 1 gram atom of titanium.
Claim 32
Dependent Claim 35 words
The improved Ziegler-type catalyst composition of claim 28, wherein, in said process for producing said titanium trichloride catalyst, the complexing agent is an ether selected from di-n-butyl ether, di-n-amyl ether, diisoamyl ether, or mixtures thereof.
Claim 33
Dependent Claim 31 words
The improved Ziegler-type catalyst composition of claim 29, wherein, in said process for producing said titanium trichloride catalyst, the chlorinated hydrocarbon is selected from hexachloroethane, pentachloroethane, tetrachloroethane, dichloroethane, and mixtures thereof.
Claim 34
Dependent Claim 53 words
The improved Ziegler-type catalyst composition of claim 30, wherein, in said process for producing said titanium trichloride catalysts said reduced solids product is contacted with said chlorinated hydrocarbon in the presence of said ether at an elevated temperature of about 65° C. to about 90° C. for about 1 to about 10 hours.
Claim 35
Dependent Claim 23 words
The improved Ziegler-type catalyst composition of claim 31, wherein, in said process for producing said titanium trichloride catalyst, said chlorinated hydrocarbon is hexachloroethane.
Claim 36
Dependent Claim 23 words
The improved Ziegler-type catalyst composition of claim 31, wherein, in said process for producing said titanium trichloride catalyst, said chlorinated hydrocarbon is pentachloroethane.
Claim 37
Dependent Claim 23 words
The improved Ziegler-type catalyst composition of claim 31, wherein, in said process for producing said titanium trichloride catalyst, said chlorinated hydrocarbon is tetrachloroethane.
Claim 38
Dependent Claim 23 words
The improved Ziegler-type catalyst composition of claim 31, wherein, in said process for producing said titanium trichloride catalyst, said chlorinated hydrocarbon is dichloroethane.
Claim 39
Dependent Claim 24 words
The improved Ziegler-type catalyst composition of claim 27, wherein, said organometal compound co-catalyst is selected from monoalkylaluminum dichloride, dialkylaluminum monochloride, trialkylaluminum or mixtures thereof.

References Cited (Backward Citations)

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1983-01-07 1983-07-09 1984-01-08 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1987-01-07 1987-07-09 1988-01-08 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1991-01-07 1991-07-09 1992-01-08 $7700.00 Window Closed / Lapsed

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