Patent US4397765A successfully refreshed from Google Patents.
US4397765A
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US
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Phosphated alumina or aluminum phosphate chromium catalyst
Assignee: Phillips Petroleum Co
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Filing: 1982-05-05
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Granted: 1983-08-09
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Expires: 2002-05-05
Abstract
Abstract A catalyst system suitable for olefin polymerization comprising a catalyst component made up of chromium on a phosphated alumina or low phosphorus aluminum phosphate base and optionally an organometal cocatalyst. The resulting catalyst is particularly sensitive to the effects of hydrogen as a molecular weight control agent, thus allowing the production of polymers of having a melt flow varying over a wide spectrum utilizing the same catalyst.
Inventors
- 👤 Max P. McDaniel
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 03:40
CPC Classifications
C; C08; C08F; C08F10/00
Claims Analysis
Total Claims: 38
Claim 1
Independent Claim
69 words
A method of making a catalyst system comprising (a) treating a separately prepared alumina gel with a phosphating agent to give a surface treatment and activating the thus treated gel in an oxidizing atmosphere at an elevated temperature, said gel either having a chromium compound coprecipitated therewith or having a chromium compound added thereto prior to said activating; and (b) combining an organometal cocatalyst with the thus activated catalyst.
Claim 2
Independent Claim
69 words
A method of making a catalyst system comprising (a) treating a separately prepared alumina gel with a phosphating agent to give a surface treatment and activating the thus treated gel in an oxidizing atmosphere at an elevated temperature, said gel either having a chromium compound coprecipitated therewith or having a chromium compound added thereto prior to said activating; and (b) combining an organometal cocatalyst with the thus activated catalyst.
Claim 3
Dependent Claim
36 words
A method according to claim 1 wherein said phosphating agent is phosphoric acid and is incorporated in an amount within the range of 1 to 10 mole percent based on the total moles of said alumina.
Claim 4
Dependent Claim
11 words
A method according to claim 1 wherein said cocatalyst is tri-n-butylborane.
Claim 5
Dependent Claim
34 words
A method according to claim 1 wherein said chromium compound is present in an amount within the range of 0.1 to 5 weight percent chromium based on the weight of said gel after activation.
Claim 6
Dependent Claim
23 words
A method according to claim 1 wherein said activating is carried out in air for 1 minute to 48 hours at 150°-800° C.
Claim 7
Dependent Claim
14 words
A method according to claim 1 wherein said alumina gel consists essentially of alumina.
Claim 8
Dependent Claim
11 words
A method according to claim 1 wherein said cocatalyst is triethylborane.
Claim 9
Dependent Claim
60 words
A method according to claim 1 wherein said phosphating agent is orthophosphoric acid and said phosphoric acid is used in an amount to give 0.01 to 0.5 milligrams phosphorus per square meter of surface area of the alumina after said alumina has been converted from a hydrogel to a zerogel and said cocatalyst is one of triethylborane, tripropylborane and tri-n-butylborane.
Claim 10
Dependent Claim
52 words
A method according to claim 1 wherein said alumina gel is treated with said phosphating agent while in the xerogel state, thereafter said chromium compound is added and the chromium-containing xerogel activated in air for a time within the range of 1 minute to 48 hours at a temperature of 150°-800° C.
Claim 11
Dependent Claim
80 words
A method according to claim 1 wherein said alumina gel is treated with said phosphating agent while in a hydrogel state, said chromium compound is added to the resulting treated hydrogel and the hydrogel converted to a xerogel by azeotrope drying or washing with a water miscible organic liquid prior to said activating, and wherein said activating is carried out in air for a time within the range of 1 minute to 48 hours at a temperature of 150°-800° C.
Claim 12
Dependent Claim
13 words
A method according to claim 10 wherein said phosphating agent is orthophosphoric acid.
Claim 13
Dependent Claim
60 words
A method according to claim 11 wherein said treating is carried out using said phosphoric acid in an amount to give 0.01 to 0.5 milligrams phosphorus per square meter of surface area of said alumina xerogel and said chromium is present in an amount within the range of 0.1 to 5 weight percent based on the weight of said xerogel.
Claim 14
Dependent Claim
16 words
A method according to claim 12 wherein said cocatalyst is one of triethylborane, tripropylborane, or tri-n-butylborane.
Claim 15
Dependent Claim
9 words
A catalyst produced by the method of claim 13.
Claim 16
Dependent Claim
9 words
A catalyst produced by the method of claim 1.
Claim 17
Dependent Claim
23 words
A catalyst system comprising (a) a catalyst comprising a chromium oxide on a surface phosphated alumina gel base; and (b) an organometal cocatalyst.
Claim 18
Dependent Claim
23 words
A catalyst system comprising (a) a catalyst comprising a chromium oxide on a surface phosphated alumina gel base; and (b) an organometal cocatalyst.
Claim 19
Independent Claim
59 words
A method of preparing a catalyst comprising treating a separately prepared low phosphorus aluminum phosphate gel with a phosphating agent to give a surface treatment and activating the thus treated gel in an oxidizing atmosphere at an elevated temperature, said gel either having a chromium compound coprecipitated therewith or having a chromium compound added thereto prior to said activating.
Claim 20
Independent Claim
59 words
A method of preparing a catalyst comprising treating a separately prepared low phosphorus aluminum phosphate gel with a phosphating agent to give a surface treatment and activating the thus treated gel in an oxidizing atmosphere at an elevated temperature, said gel either having a chromium compound coprecipitated therewith or having a chromium compound added thereto prior to said activating.
Claim 21
Dependent Claim
19 words
A method according to claim 17 wherein in addition an organometal cocatalyst is combined with said thus activated catalyst.
Claim 22
Dependent Claim
26 words
A method according to claim 17 wherein said low phosphorus aluminum phosphate has a phosphorus to aluminum atom ratio within the range of 0.02:1 to 0.6:1.
Claim 23
Dependent Claim
67 words
A method according to claim 19 wherein said phosphating agent is one of orthophosphoric acid or monoammonium dihydrogen phosphate, and said phosphating agent is added to said low phosphorus aluminum phosphate in the hydrogel state after which the hydrogel is converted to a xerogel by means of azeotropic distillation or washing with a water miscible organic compound, dried of organic compound and then subjected to said activating.
Claim 24
Dependent Claim
34 words
A method according to claim 20 wherein said activating is carried out in air at a temperature within the range of 150°-800° C. for a time within the range of 0.5 to 10 hours.
Claim 25
Dependent Claim
24 words
A method according to claim 20 wherein said chromium is introduced at the hydrogel state by means of adding a water soluble chromium compound.
Claim 26
Dependent Claim
23 words
A method according to claim 22 wherein said water soluble chromium compound is one of CrO 3 , chromium acetate, or chromium nitrate.
Claim 27
Dependent Claim
9 words
A catalyst produced by the method of claim 23.
Claim 28
Dependent Claim
9 words
A catalyst produced by the method of claim 17.
Claim 29
Independent Claim
136 words
A method of making a catalyst comprising (a) treating an alumina hydrogel with orthophosphoric acid, adding a chromium compound to the resulting treated hydrogel, converting the hydrogel to a xerogel by azeotrope drying or washing with a water miscible organic liquid, and activating the thus treated xerogel in air for a time within the range of 1 minute to 48 hours at a temperature of 150°-800° C., wherein said phosphoric acid is used in an amount to give 0.01 to 0.5 milligrams phosphorus per square meter of surface area of said alumina zerogel and said chromium compound is added in an amount sufficient to provide chromium in an amount within the range of 0.1 to 5 weight percent based on the weight of said xerogel; and (b) combining an organometal cocatalyst with the thus activated catalyst.
Claim 30
Independent Claim
136 words
A method of making a catalyst comprising (a) treating an alumina hydrogel with orthophosphoric acid, adding a chromium compound to the resulting treated hydrogel, converting the hydrogel to a xerogel by azeotrope drying or washing with a water miscible organic liquid, and activating the thus treated xerogel in air for a time within the range of 1 minute to 48 hours at a temperature of 150°-800° C., wherein said phosphoric acid is used in an amount to give 0.01 to 0.5 milligrams phosphorus per square meter of surface area of said alumina zerogel and said chromium compound is added in an amount sufficient to provide chromium in an amount within the range of 0.1 to 5 weight percent based on the weight of said xerogel; and (b) combining an organometal cocatalyst with the thus activated catalyst.
Claim 31
Dependent Claim
16 words
A method according to claim 26 wherein said cocatalyst is one of triethylborane, tripropylborane or tri-n-butylborane.
Claim 32
Dependent Claim
9 words
A catalyst produced by the method of claim 27.
Claim 33
Dependent Claim
9 words
A catalyst produced by the method of claim 26.
Claim 34
Independent Claim
106 words
A method of making a catalyst system comprising (a) treating an alumina xerogel with phosphoric acid in an amount sufficient to give 0.01 to 0.5 milligrams phosphorus per square meter of surface area of said alumina xerogel, adding a chromium compound in an amount sufficient to give chromium in an amount within the range of 0.1 to 5 weight percent based on the weight of said xerogel, activating said xerogel containing said chromium by heating in air for a time within the range of 1 minute to 48 hours at a temperature of 150°-800° C.; and (b) combining an organometal cocatalyst with the thus activated catalyst.
Claim 35
Independent Claim
106 words
A method of making a catalyst system comprising (a) treating an alumina xerogel with phosphoric acid in an amount sufficient to give 0.01 to 0.5 milligrams phosphorus per square meter of surface area of said alumina xerogel, adding a chromium compound in an amount sufficient to give chromium in an amount within the range of 0.1 to 5 weight percent based on the weight of said xerogel, activating said xerogel containing said chromium by heating in air for a time within the range of 1 minute to 48 hours at a temperature of 150°-800° C.; and (b) combining an organometal cocatalyst with the thus activated catalyst.
Claim 36
Dependent Claim
16 words
A method according to claim 26 wherein said cocatalyst is one of triethylborane, tripropylborane, or tri-n-butylborane.
Claim 37
Dependent Claim
9 words
A catalyst produced by the method of claim 31.
Claim 38
Dependent Claim
9 words
A catalyst produced by the method of claim 30.
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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) | 1986-08-08 | 1987-02-07 | 1987-08-09 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-08-08 | 1991-02-07 | 1991-08-09 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-08-08 | 1995-02-07 | 1995-08-09 | $7700.00 | Window Closed / Lapsed |