US5728640A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Preparation of supported metallocene/aluminoxane solid catalyst
Assignee: Sinopec Research Institute of Petroleum Processing
•
Filing: 1996-07-10
•
Granted: 1998-03-17
•
Expires: 2016-07-10
Abstract
Abstract A process for preparing a supported metallocene/aluminoxane solid catalyst comprises preparing a water-in-oil emulsion of water and an inert solvent by using an emulsifier, adding dropwise the emulsion to a solution of an organoaluminium compound in an inert solvent to carry out the reaction to obtain a suspension of the particulate aluminoxane, followed by adding a solution of a metallocene to the above suspension to support the metallocene on the aluminoxane. The solid catalyst thus obtained can be used in the polymerization and copolymerization of olefins. Polymerization can be carried out by slurry polymerization, bulk polymerization, gas phase polymerization, etc.
Inventors
- 👤 Bing Lu
- 👤 Jinmei Wang
- 👤 Xiaoyu Hong
- 👤 Zhenhua Jing
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 13:11
CPC Classifications
C; C08; C08F; C08F10/00; C07; C07F; C07F17/00; C08F4/00; C08F4/42; C08F4/44; C08F4/60; C08F4/619; C08F4/61912; C08F4/61916; C08F4/6192; C08F4/61922; Y; Y10; Y10S; Y10S526/00; Y10S526/943
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
235 words
A process for preparing a supported metallocene/aluminoxane solid catalyst which comprises the steps of: a) preparing a water-in-oil emulsion by combining a first inert solvent, water, and emulsifier, wherein the volume ratio of said first inert solvent, water, and emulsifier is about 100:0.5 to 10:0.1 to 1; b) dissolving an organoaluminum compound in a second inert solvent to make a solution having about 5 to about 30% by weight of the organoaluminum compound; c) adding dropwise said emulsion to said solution of the organoaluminum compound in a molar ratio of the organoaluminum compound to water in emulsion of about 0.8 to 2:1 in an inert atmosphere at a temperature of about -10° to about 40° C. and a rate of about 0.2 to about 20 ml/min, followed by heating the resulting solution to a temperature of about 40° to about 80° C. and allowing the reaction to proceed for about 1 to about 4 hours to obtain a suspension of a particulate aluminoxane; and d) adding a solution of a transition metal metallocene to said suspension of the particulate aluminoxane in a molar ratio of transition metal atom to aluminum atom of about 1:100 to 10,000 at about 0° to about 60° C. for about 1 to about 4 hours and removing the solvent to form said catalyst, wherein said transition metal is selected from a metal in Group IV B of the Periodic Table.
Claim 2
Dependent Claim
235 words
A process for preparing a supported metallocene/aluminoxane solid catalyst which comprises the steps of: a) preparing a water-in-oil emulsion by combining a first inert solvent, water, and emulsifier, wherein the volume ratio of said first inert solvent, water, and emulsifier is about 100:0.5 to 10:0.1 to 1; b) dissolving an organoaluminum compound in a second inert solvent to make a solution having about 5 to about 30% by weight of the organoaluminum compound; c) adding dropwise said emulsion to said solution of the organoaluminum compound in a molar ratio of the organoaluminum compound to water in emulsion of about 0.8 to 2:1 in an inert atmosphere at a temperature of about -10° to about 40° C. and a rate of about 0.2 to about 20 ml/min, followed by heating the resulting solution to a temperature of about 40° to about 80° C. and allowing the reaction to proceed for about 1 to about 4 hours to obtain a suspension of a particulate aluminoxane; and d) adding a solution of a transition metal metallocene to said suspension of the particulate aluminoxane in a molar ratio of transition metal atom to aluminum atom of about 1:100 to 10,000 at about 0° to about 60° C. for about 1 to about 4 hours and removing the solvent to form said catalyst, wherein said transition metal is selected from a metal in Group IV B of the Periodic Table.
Claim 3
Dependent Claim
23 words
The process according to claim 1, wherein said volume ratio of inert solvent, water, and emulsifier is about 100:1 to 5:0.2 to 0.5.
Claim 4
Dependent Claim
25 words
The process according to claim 1, wherein said solution made in step b) has about 10 to about 20% by weight of the organoaluminum compound.
Claim 5
Dependent Claim
23 words
The process according to claim 1, wherein said molar ratio of the organoaluminum compound to water in emulsion is about 1 to 1.5:1.
Claim 6
Dependent Claim
35 words
The process according to claim 1, wherein said addition of step c) is carried out at a temperature of about 0° to about 20° C. and a rate of about 0.5 to about 5 ml/min.
Claim 7
Dependent Claim
28 words
The process according to claim 1, wherein said reaction after said addition in step c) is carried out at a temperature of about 40° to about 60° C.
Claim 8
Dependent Claim
26 words
The process according to claim 1, wherein said molar ratio of the transition metal atom in the metallocene to aluminum atom is about 1:300 to 8,000.
Claim 9
Dependent Claim
25 words
The process according to claim 1, wherein said emulsifier is a polyol nonionic surfactant having a hydrophilic-lypophilic balance value of about 2 to about 6.
Claim 10
Dependent Claim
28 words
The process according to claim 1, wherein said first inert solvent and said second inert solvent comprise those solvents in which said aluminoxane is insoluble or slightly soluble.
Claim 11
Dependent Claim
27 words
The process according to claim 1, wherein said organoaluminum compound is selected from the group consisting of alkyl aluminum, alkoxy aluminum, aryl aluminum and alkyl aluminum halide.
Claim 12
Dependent Claim
26 words
The process according to claim 7, wherein said molar ration of the transition metal atom in the metallocene to aluminum atom is about 1:500 to 5,000.
Claim 13
Dependent Claim
25 words
The process according to claim 8, wherein said emulsifier is a polyol nonionic surfactant having a hydrophilic-lypophilic balance value of about 3 to about 5.
Claim 14
Dependent Claim
17 words
The process according to claim 9, wherein said first and second inert solvents are saturated hydrocarbon compounds.
Claim 15
Dependent Claim
13 words
The process according to claim 13, wherein said saturated hydrocarbon compounds are hexane.
Claim 16
Dependent Claim
14 words
The process according to claim 10, wherein said organoaluminum compound is a trialkyl aluminum.
Claim 17
Dependent Claim
13 words
The process according to claim 15, wherein said trialkykl aluminum is trimethyl aluminum.
References Cited (Backward Citations)
GB783605A
Cited
US3792070A
Cited
US4203867A
Cited
US4474704A
Cited
EP0206794A1
Cited
US5280000A
Cited
EP0226463A1
Cited
WO1987003889A1
Cited
EP0269987A2
Cited
WO1988005057A1
Cited
WO1988005058A1
Cited
EP0279586B1
Cited
EP0285443B1
Cited
EP0294942A1
Cited
EP0293815A1
Cited
US4925821A
Cited
US5276117A
Cited
US5008228A
Cited
US5006500A
Cited
US5278263A
Cited
US5405816A
Cited
US5663394A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 2001-03-16 | 2001-09-15 | 2002-03-17 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2005-03-16 | 2005-09-15 | 2006-03-17 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2009-03-16 | 2009-09-15 | 2010-03-17 | $7700.00 | Window Closed / Lapsed |