US4950631A
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US
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Modified silica based catalyst
Assignee: Equistar Chemicals LP
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Filing: 1989-03-21
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Granted: 1990-08-21
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Expires: 2009-03-21
Abstract
Abstract A catalyst comprising the product formed by (a) treating silica to remove surface hydroxyl groups; (b) contacting said treated silica with (1) a modifying compound selected from the group consisting of silicon halides, boron halides, aluminum halides, alkyl silicon halides and mixtures thereof; and (2) at least one hydrocarbon soluble magnesium-containing compound selected from the group consisting of hydrocarbyloxy magnesium, hydrocarbyloxymagnesium halides and mixtures thereof; said contacting steps (1) and (2) occurring in random order; (c) contacting the product of step (b) with at least one titanium-containing compound having the structural formula Ti(OR) n X m , where R is aryl, alkyl or mixtures thereof; X is halogen; n is an integer of 1 to 4; m is 0 or an integer of 1 to 3; and the sum of m and n is 4; and (d) treating the product of step (c) with a titanium-containing compound having the structural formula TiX 1 p OR 1 ) q , where X 1 is halogen; R 1 is aryl or alkyl; p is an integer of 1 to 4; q is 0 or an integer of 1 to 3; and the sum of p and q is 4, with the proviso that the titanium-containing compound of this step is not the same as the titanium-containing compound of step (c). The catalyst is useful in polymerizing propylene. In this application propylene is polymerized under propylene polymerization conditions in the presence of a first co-catalyst, an aluminum-containing compound, and a second co-catalyst, a slane.
Inventors
- 👤 Charles K. Buehler
- 👤 Richard W. Fries
- 👤 Thomas J. Pullukat
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 06:08
CPC Classifications
C; C08; C08F; C08F10/00
Claims Analysis
Total Claims: 24
Claim 1
Independent Claim
219 words
A catalyst comprising the product obtained by: (a) treating silica to remove surface hydroxyl groups ##STR3## (b) contacting said treated silica with (1) a modifying compound selected from the group consisting of silicon halides, boron halides, aluminum halides, alkyl silicon halides and mixtures thereof; and (2) at least one hydrocarbon soluble magnesium-containing compound selected from the group consisting of hydrocarbyloxy magnesiums, hydrocarbyloxymagnesium halides and mixtures thereof; said contacting steps (1) and (2) occurring in random order; (c) contacting said product of step (b) with at least one titanium-containing compound having the structural formula Ti(OR) n X m , where R is aryl, alkyl or mixtures thereof; X is halogen; n is an integer of 1 to 4; m is 0 or an integer of 1 to 3; and the sum of m and n is 4; and (d) treating the product of step (c) with a titanium-containing compound having the structural formula TiX 1 p (OR 1 ) q , where X 1 is halogen; R 1 is aryl or alkyl; p is an integer of 1 to 4; q is 0 or an integer of 1 to 3; and the sum of p and q is 4, with the proviso that the titanium-containing compound of this step is not the same as the titanium-containing compound of step (c).
Claim 2
Dependent Claim
219 words
A catalyst comprising the product obtained by: (a) treating silica to remove surface hydroxyl groups ##STR3## (b) contacting said treated silica with (1) a modifying compound selected from the group consisting of silicon halides, boron halides, aluminum halides, alkyl silicon halides and mixtures thereof; and (2) at least one hydrocarbon soluble magnesium-containing compound selected from the group consisting of hydrocarbyloxy magnesiums, hydrocarbyloxymagnesium halides and mixtures thereof; said contacting steps (1) and (2) occurring in random order; (c) contacting said product of step (b) with at least one titanium-containing compound having the structural formula Ti(OR) n X m , where R is aryl, alkyl or mixtures thereof; X is halogen; n is an integer of 1 to 4; m is 0 or an integer of 1 to 3; and the sum of m and n is 4; and (d) treating the product of step (c) with a titanium-containing compound having the structural formula TiX 1 p (OR 1 ) q , where X 1 is halogen; R 1 is aryl or alkyl; p is an integer of 1 to 4; q is 0 or an integer of 1 to 3; and the sum of p and q is 4, with the proviso that the titanium-containing compound of this step is not the same as the titanium-containing compound of step (c).
Claim 3
Dependent Claim
19 words
A catalyst in accordance with claim 1 wherein said step (a) comprises calcining said silica in an inert atmosphere.
Claim 4
Dependent Claim
19 words
A catalyst in accordance with claim 1 wherein said step (a) comprises treating said silica with a hexaalkyl disilazane.
Claim 5
Dependent Claim
50 words
A catalyst in accordance with claim 1 wherein said silica has a surface area in the range of between about 80 and about 300 m 2 /g, a median particle size of about 20 to about 200 microns and a pore volume of between about 0.6 to about 3.0 cc/g.
Claim 6
Dependent Claim
36 words
A catalyst in accordance with claim 4 wherein said silica support is selected from the group consisting of pure silica, silica containing minor amounts of one or more of alumina, titania, zirconia, magnesia and mixtures thereof.
Claim 7
Dependent Claim
33 words
A catalyst in accordance with claim 1 wherein said compound having the structural formula Ti(OR) n X m is selected from the group consisting of tetrahydrocarbyloxytitaniums, trihydrocarbyloxytitanium halides, dihydrocarbyloxytitanium dihalides and mixtures thereof.
Claim 8
Dependent Claim
15 words
A catalyst in accordance with claim 6 wherein n is 4 and m is 0.
Claim 9
Dependent Claim
23 words
A catalyst in accordance with claim 1 wherein p is an integer of 2 to 4 and q is 0, 1 or 2.
Claim 10
Dependent Claim
15 words
A catalyst in accordance with claim 8 wherein p is 4 and q is 0.
Claim 11
Dependent Claim
32 words
A catalyst in accordance with claim 1 wherein each of steps (a), (b) and (c) are conducted at a temperature in the range of between about 0° C. and about 100° C.
Claim 12
Dependent Claim
165 words
A catalyst comprising the product of the steps of: (a) treating silica having a surface area of about 80 to about 300 m 2 /g, a median particle size of about 20 to about 200 microns and a pore volume of about 0.6 to about 3.0 cc/g whereby hydroxyl groups on the surface of said silica are removed ##STR4## (b) contacting said treated silica with (1) a modifying compound selected from the group consisting of silicon halides, boron halides, aluminum halides and mixtures thereof; and (2) a hydrocarbon soluble magnesium-containing compound selected from the group consisting of hydrocarbyloxy magnesiums, hydrocarbyloxymagnesium halides and mixtures thereof; said sequence of contacting steps (1) and (2) being random; (c) contacting said product of step (b) with a titanium ester having the structural formula Ti(OR) 4 , where R is aryl, alkyl or mixtures thereof; and (d) treating said product of step (c) with a titanium halide having the structural formula TiX 1 4 , where X 1 is halogen.
Claim 13
Dependent Claim
165 words
A catalyst comprising the product of the steps of: (a) treating silica having a surface area of about 80 to about 300 m 2 /g, a median particle size of about 20 to about 200 microns and a pore volume of about 0.6 to about 3.0 cc/g whereby hydroxyl groups on the surface of said silica are removed ##STR4## (b) contacting said treated silica with (1) a modifying compound selected from the group consisting of silicon halides, boron halides, aluminum halides and mixtures thereof; and (2) a hydrocarbon soluble magnesium-containing compound selected from the group consisting of hydrocarbyloxy magnesiums, hydrocarbyloxymagnesium halides and mixtures thereof; said sequence of contacting steps (1) and (2) being random; (c) contacting said product of step (b) with a titanium ester having the structural formula Ti(OR) 4 , where R is aryl, alkyl or mixtures thereof; and (d) treating said product of step (c) with a titanium halide having the structural formula TiX 1 4 , where X 1 is halogen.
Claim 14
Dependent Claim
33 words
A catalyst in accordance with claim 11 wherein said step (a) comprises calcining silica at a temperature in the range of between about 550° C. and about 650° C. in a nitrogen atmosphere.
Claim 15
Dependent Claim
17 words
A catalyst in accordance with claim 11 wherein said step (a) comprises treating silica with hexamethyl disilazane.
Claim 16
Dependent Claim
25 words
A catalyst in accordance with claim 11 wherein said modifying compound is selected from the group consisting of silicon tetrachloride, boron trichloride and aluminum trichloride.
Claim 17
Dependent Claim
25 words
A catalyst in accordance with claim 11 wherein said magnesium compound is selected from the group consisting of magnesium alkoxides, alkoxymagnesium halides and mixtures thereof.
Claim 18
Dependent Claim
26 words
A catalyst in accordance with claim 15 wherein said magnesium compound is selected from the group consisting of 2-methylpenyloxymagnesium chloride, di-2-ethylhexyloxymagnesium, pentoxymagnesium chloride and mixtures thereof.
Claim 19
Dependent Claim
34 words
A catalyst in accordance with claim 11 wherein said titanium ester is selected from the group consisting of tetracresyl titanate, titanium tetrabutoxide, titanium tetranonolate and tetra-2-ethylhexyltitanate, tetraisobutyltitanate, tetra n-propyltitanate, tetraisopropyl titanate and mixtures thereof.
Claim 20
Dependent Claim
14 words
A catalyst in accordance with claim 17 wherein said titanium halide is titanium tetrachloride.
Claim 21
Dependent Claim
110 words
A catalyst comprising the product obtained by: (a) treating silica having a surface area of about 80 to about 300 m 2 /g, a median particle size of about 20 to about 200 microns and a pore volume of about 0.6 to about 3.0 cc/g to remove hydroxyl groups from the surface of said silica; (b) contacting said treated silica with (1) a compound selected from the group consisting of silicon tetrachloride, boron trichloride and aluminum trichloride; and (2) 2-methylpentyloxymagnesium chloride; said contacting steps (1) and (2) being random; (c) contacting said product of step (b) with tetracresyl titanate; and (d) treating the product of step (c) with titanium tetrachloride.
Claim 22
Dependent Claim
110 words
A catalyst comprising the product obtained by: (a) treating silica having a surface area of about 80 to about 300 m 2 /g, a median particle size of about 20 to about 200 microns and a pore volume of about 0.6 to about 3.0 cc/g to remove hydroxyl groups from the surface of said silica; (b) contacting said treated silica with (1) a compound selected from the group consisting of silicon tetrachloride, boron trichloride and aluminum trichloride; and (2) 2-methylpentyloxymagnesium chloride; said contacting steps (1) and (2) being random; (c) contacting said product of step (b) with tetracresyl titanate; and (d) treating the product of step (c) with titanium tetrachloride.
Claim 23
Dependent Claim
22 words
A catalyst in accordance with claim 19 wherein said step (a) comprises calcining said silica at a temperature of about 600° C.
Claim 24
Dependent Claim
18 words
A catalyst in accordance with claim 19 wherein said step (a) comprises treating said silica with hexamethyl disilazane.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1993-08-20 | 1994-02-19 | 1994-08-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1997-08-20 | 1998-02-19 | 1998-08-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2001-08-20 | 2002-02-19 | 2002-08-21 | $7700.00 | Window Closed / Lapsed |