US4246135A
Expired / Lapsed
US
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Olefin polymerization catalyst
Assignee: Sumitomo Chemical Co Ltd
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Filing: 1979-05-23
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Granted: 1981-01-20
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Expires: 1999-05-23
Abstract
Abstract A process for producing a solid titanium trichloride catalyst which comprises at a temperature of -40 DEG C. to 40 DEG C. mixing titanium tetrachloride with an organo-aluminum compound of the formula (I): AlRnX3-n (I) wherein R has up to 10 carbon atoms and is an aliphatic hydrocarbon group which may be straight chain, branched chain or cyclic, or an aromatic hydrocarbon group; X is a halogen atom or a hydrogen atom; and n is a number satisfying the relation, 1.5</=n</=3; in the presence of an ether compound of the formula (II): R2OR3 (II) wherein R2 and R3, which may be the same or different, each is an alkyl group, an aralkyl group or an alkenyl group, each having up to 10 carbon atoms, to reduce the titanium tetrachloride; maintaining the mixed solution at a temperature of 10 DEG C. to 50 DEG C. thereby performing the reduction; at the time when the reduction reaction proceeds at least 90%, adding iodine to the resulting liquid titanium trichloride product; maintaining the resulting mixture at a temperature of about 30 DEG C. to about 150 DEG C. after the addition thereby precipitating solid titanium trichloride; and then separating the solid titanium trichloride.
Inventors
- 👤 Akinobu Shiga
- 👤 Yoshiharu Fukui
- 👤 Kazuhiro Matsumura
- 👤 Toshio Sasaki
- 👤 Masahisa Okawa
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 01:01
CPC Classifications
C; C08; C08F; C08F10/00
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
249 words
A solid titanium trichloride catalyst produced by the steps of (a) at a temperature of -40° C. to 40° C., over a period of 5 minutes to 6 hours, mixing titanium tetrachloride with from 0.2 to 1.1 moles per mole of said titanium tetrachloride of an organo-aluminum compound of the formula (I): AlR.sub.n X.sub.3-n (I) wherein R has up to 10 carbon atoms and is an aliphatic hydrocarbon group which may be straight chain, branched chain or cyclic, or an aromatic hydrocarbon group; X is a halogen atom or a hydrogen atom; and n is a number satisfying the relation, 1.5≦n≦3; in the presence of from 0.1 to about 3 moles per mole of said titanium tetrachloride of an ether compound of the formula (II); R.sup.2 OR.sup.3 (II) wherein R 2 and R 3 , which may be the same or different, each is an alkyl group, an aralkyl group or an alkenyl group, each having up to 10 carbon atoms, to reduce the titanium tetrachloride; (b) maintaining the mixed solution at a temperature of 10° C. to 50° C. for 1.5 to 6 hours thereby performing the reduction; (c) at the time when the reduction proceeds at least 90%, adding iodine in an amount of 0.01 to about 1 mole of said titanium tetrachloride to the resulting liquid titanium trichloride product; (d) maintaining the resulting mixture at about 30° C. to about 150° C. thereby precipitating solid titanium trichloride; and (e) then separating the solid titanium trichloride catalyst.
Claim 2
Dependent Claim
249 words
A solid titanium trichloride catalyst produced by the steps of (a) at a temperature of -40° C. to 40° C., over a period of 5 minutes to 6 hours, mixing titanium tetrachloride with from 0.2 to 1.1 moles per mole of said titanium tetrachloride of an organo-aluminum compound of the formula (I): AlR.sub.n X.sub.3-n (I) wherein R has up to 10 carbon atoms and is an aliphatic hydrocarbon group which may be straight chain, branched chain or cyclic, or an aromatic hydrocarbon group; X is a halogen atom or a hydrogen atom; and n is a number satisfying the relation, 1.5≦n≦3; in the presence of from 0.1 to about 3 moles per mole of said titanium tetrachloride of an ether compound of the formula (II); R.sup.2 OR.sup.3 (II) wherein R 2 and R 3 , which may be the same or different, each is an alkyl group, an aralkyl group or an alkenyl group, each having up to 10 carbon atoms, to reduce the titanium tetrachloride; (b) maintaining the mixed solution at a temperature of 10° C. to 50° C. for 1.5 to 6 hours thereby performing the reduction; (c) at the time when the reduction proceeds at least 90%, adding iodine in an amount of 0.01 to about 1 mole of said titanium tetrachloride to the resulting liquid titanium trichloride product; (d) maintaining the resulting mixture at about 30° C. to about 150° C. thereby precipitating solid titanium trichloride; and (e) then separating the solid titanium trichloride catalyst.
Claim 3
Dependent Claim
30 words
The catalyst of claim 1, wherein R 2 and R 3 of said ether compound of the formula (II), each is an alkyl group having 2 to 5 carbon atoms.
Claim 4
Dependent Claim
16 words
The catalyst of claim 2, wherein said ether compound of the formula (II) is di-n-butyl ether.
Claim 5
Dependent Claim
34 words
The catalyst of claim 1 or 2, wherein said organoaluminum compound of the formula (I) is selected from the group consisting of an alkylaluminum sesquihalide, a dialkylaluminum halide, a trialkylaluminum and a dialkylaluminum hydride.
Claim 6
Dependent Claim
16 words
The catalyst of claim 4, wherein said organo-aluminum compound of the formula (I) is diethylaluminum chloride.
Claim 7
Dependent Claim
25 words
The catalyst according to claim 1, wherein the chemical equivalent of the organo-aluminum compound is about 1 to 1.2 times of that of titanium tetrachloride.
Claim 8
Dependent Claim
28 words
The catalyst of claim 1 or 2, wherein said amount of said ether compound of the formula (II) is 0.5 to 1.5 moles per mole of titanium tetrachloride.
Claim 9
Dependent Claim
23 words
The catalyst of claim 1 or 2, wherein mixing is carried out at a temperature of about -20° C. to about 40° C.
Claim 10
Dependent Claim
22 words
The catalyst of claim 1 or 2, wherein the mixed solution is maintained at a temperature of 20° C. to 50° C.
Claim 11
Dependent Claim
18 words
The catalyst of claim 1, wherein the iodine is added after the reduction has proceeded at least 95%.
Claim 12
Dependent Claim
18 words
The catalyst of claim 2, wherein the iodine is added at the time when the reduction is completed.
Claim 13
Dependent Claim
22 words
The catalyst of claim 1 or 2, wherein the amount of iodine is 0.03 to 0.5 mole per mole of titanium tetrachloride.
Claim 14
Dependent Claim
29 words
The catalyst of claim 1, wherein said treatment with the mixture of iodine and the ether compound is at a temperature of about 50° C. to about 150° C.
Claim 15
Dependent Claim
15 words
The catalyst of claim 13, wherein said treatment is at 80° C. to 130° C.
Claim 16
Dependent Claim
292 words
A solid titanium trichloride catalyst represented by the formula: TiCl.sub.3 (AlCl.sub.3).sub.p (E).sub.q (I).sub.r wherein E is an ether compound represented by the formula R 2 OR 3 wherein R 2 and R 3 , which may be the same or different, each is an alkyl group, an aralkyl group or an alkenyl group, each having up to 10 carbon atoms and p, q and r are numbers satisfying the relations, 0<p<0.02, 0<q<0.15 and 0.001<r<0.05, produced by the steps of (a) at a temperature of -40° C. to 40° C., over a period of 5 minutes to 6 hours, mixing titanium tetrachloride with from 0.2 to 1.1 moles per mole of said titanium tetrachloride of an organo-aluminum compound of the formula (I): AlR.sub.n X.sub.3-n wherein R has up to 10 carbon atoms and is an aliphatic hydrocarbon group which may be straight chain, branched chain or cyclic, or an aromatic hydrocarbon group; X is a halogen atom or a hydrogen atom; and n is a number satisfying the relation, 1.5≦n≦3; in the presence of from 0.1 to about 3 moles per mole of said titanium tetrachloride of an ether compound of the formula (II): R.sup.2 OR.sup.3 wherein R 2 and R 3 are as set forth above, to reduce the titanium tetrachloride; (b) maintaining the mixed solution at a temperature of 10° C. to 50° C. thereby performing the reduction; (c) at the time when the reduction proceeds to at least 90%, adding iodine in an amount of 0.01 to about 1 mole per mole of said titanium tetrachloride to the resulting liquid titanium trichloride product; (d) maintaining the resulting mixture at about 30° C. to about 150° C. thereby pr-cipitating solid titanium trichloride; and (e) then separating the solid titanium trichloride catalyst.
Claim 17
Dependent Claim
292 words
A solid titanium trichloride catalyst represented by the formula: TiCl.sub.3 (AlCl.sub.3).sub.p (E).sub.q (I).sub.r wherein E is an ether compound represented by the formula R 2 OR 3 wherein R 2 and R 3 , which may be the same or different, each is an alkyl group, an aralkyl group or an alkenyl group, each having up to 10 carbon atoms and p, q and r are numbers satisfying the relations, 0<p<0.02, 0<q<0.15 and 0.001<r<0.05, produced by the steps of (a) at a temperature of -40° C. to 40° C., over a period of 5 minutes to 6 hours, mixing titanium tetrachloride with from 0.2 to 1.1 moles per mole of said titanium tetrachloride of an organo-aluminum compound of the formula (I): AlR.sub.n X.sub.3-n wherein R has up to 10 carbon atoms and is an aliphatic hydrocarbon group which may be straight chain, branched chain or cyclic, or an aromatic hydrocarbon group; X is a halogen atom or a hydrogen atom; and n is a number satisfying the relation, 1.5≦n≦3; in the presence of from 0.1 to about 3 moles per mole of said titanium tetrachloride of an ether compound of the formula (II): R.sup.2 OR.sup.3 wherein R 2 and R 3 are as set forth above, to reduce the titanium tetrachloride; (b) maintaining the mixed solution at a temperature of 10° C. to 50° C. thereby performing the reduction; (c) at the time when the reduction proceeds to at least 90%, adding iodine in an amount of 0.01 to about 1 mole per mole of said titanium tetrachloride to the resulting liquid titanium trichloride product; (d) maintaining the resulting mixture at about 30° C. to about 150° C. thereby pr-cipitating solid titanium trichloride; and (e) then separating the solid titanium trichloride catalyst.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-01-20 | 1984-07-21 | 1985-01-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-01-20 | 1988-07-21 | 1989-01-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-01-20 | 1992-07-21 | 1993-01-20 | $7700.00 | Window Closed / Lapsed |