US5371053A
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Process for deactivating Ziegler-Natta and metallocene catalysts
Assignee: ExxonMobil Chemical Patents Inc
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Filing: 1993-05-18
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Granted: 1994-12-06
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Expires: 2013-05-18
Abstract
Abstract A process for deactivating Ziegler-Natta and metallocene catalysts or catalyst systems "such systems are typically used for olefin polymerization". The process includes heating the active catalyst or catalyst system to a temperature sufficient to drive off volatile constituents, and to form complexes and compounds that are non-reactive or less reactive with ambient air than the active catalyst or catalyst system. The process includes steps for safe deactivation including scrubbing to substantially eliminate corrosive compounds, and burning volatile chemicals in a flare. This process essentially eliminates the production of hazardous classification waste from conventional water catalyst deactivation techniques.
Inventors
- 👤 Agapios K. Agapiou
- 👤 Steve K. Ackerman
- 👤 David M. LaBorde
- 👤 Marc L. DeChellis
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 03:02
CPC Classifications
C; C08; C08F; C08F6/00; C08F6/02
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
177 words
A transition metal catalyst deactivation process comprising: (a) heating a transition metal catalyst to about 100° C. from ambient temperature, at the rate of about 10° C. per hour; (b) holding the catalyst of step (a) at a temperature in the range of from about 90° to about 110° C. for a time period sufficient to volatilize substantially all hydrocarbons; (c) heating the catalyst of step (b) to a temperature of about 200° C. said heating taking place at the rate of about 10° C. per hour; (d) holding the catalyst of step (c) at a temperature of from about 180° C. to about 300° C. for a period in the range of from about 4 hours to about 30 hours. (e) cooling the catalyst of step (d); and (f) exposing the catalyst of step (e) to air; wherein said catalyst is selected from the group consisting of a Ziegler-Natta catalyst, a Ziegler-Natta catalyst component, a metallocene catalyst, and a metallocene-alumoxane catalyst component; said heating taking place in an environment substantially free from air, oxygen and water.
Claim 2
Dependent Claim
177 words
A transition metal catalyst deactivation process comprising: (a) heating a transition metal catalyst to about 100° C. from ambient temperature, at the rate of about 10° C. per hour; (b) holding the catalyst of step (a) at a temperature in the range of from about 90° to about 110° C. for a time period sufficient to volatilize substantially all hydrocarbons; (c) heating the catalyst of step (b) to a temperature of about 200° C. said heating taking place at the rate of about 10° C. per hour; (d) holding the catalyst of step (c) at a temperature of from about 180° C. to about 300° C. for a period in the range of from about 4 hours to about 30 hours. (e) cooling the catalyst of step (d); and (f) exposing the catalyst of step (e) to air; wherein said catalyst is selected from the group consisting of a Ziegler-Natta catalyst, a Ziegler-Natta catalyst component, a metallocene catalyst, and a metallocene-alumoxane catalyst component; said heating taking place in an environment substantially free from air, oxygen and water.
Claim 3
Dependent Claim
127 words
A deactivated transition metal catalyst prepared by a process comprising: (a) heating an active transition metal catalyst to a temperature sufficient to volatilize substantially all hydrocarbons, and sufficient to effect decomposition of substantially all active compounds, said temperature being in the range of from about 100° C. to about 1000° C., at a rate of about 10° C. per hour; (b) holding the product of step (a) at about a maximum temperature reached in step (a) for a time period in the range of from about 4 to about 30 hours; wherein said transition metal catalyst is selected from the group consisting of a Ziegler-Natta catalyst, a Ziegler-Natta catalyst system, a Ziegler-Natta catalyst component, a metallocene catalyst, a metallocene-alumoxane catalyst system, and a metallocene-alumoxane catalyst system component.
Claim 4
Dependent Claim
127 words
A deactivated transition metal catalyst prepared by a process comprising: (a) heating an active transition metal catalyst to a temperature sufficient to volatilize substantially all hydrocarbons, and sufficient to effect decomposition of substantially all active compounds, said temperature being in the range of from about 100° C. to about 1000° C., at a rate of about 10° C. per hour; (b) holding the product of step (a) at about a maximum temperature reached in step (a) for a time period in the range of from about 4 to about 30 hours; wherein said transition metal catalyst is selected from the group consisting of a Ziegler-Natta catalyst, a Ziegler-Natta catalyst system, a Ziegler-Natta catalyst component, a metallocene catalyst, a metallocene-alumoxane catalyst system, and a metallocene-alumoxane catalyst system component.
Claim 5
Independent Claim
81 words
A method for producing a deactivated transition metal catalyst, comprising: (a) heating a transition metal catalyst, above about 100° C. in an environment, said environment having insufficient amounts of elements or compounds or combinations thereof to cause combustion of the transition metal polyolefin catalyst; and (b) exposing said catalyst of step (a) to air; wherein said catalyst of step (a) is selected from the group consisting of a Ziegler-Natta catalyst, a Ziegler-Natta catalyst component, a metallocene catalyst, and a metallocene-alumoxane catalyst.
Claim 6
Independent Claim
81 words
A method for producing a deactivated transition metal catalyst, comprising: (a) heating a transition metal catalyst, above about 100° C. in an environment, said environment having insufficient amounts of elements or compounds or combinations thereof to cause combustion of the transition metal polyolefin catalyst; and (b) exposing said catalyst of step (a) to air; wherein said catalyst of step (a) is selected from the group consisting of a Ziegler-Natta catalyst, a Ziegler-Natta catalyst component, a metallocene catalyst, and a metallocene-alumoxane catalyst.
Claim 7
Independent Claim
91 words
A method of producing a substantially environmentally neutral waste from a transition metal catalyst, comprising; (a) placing a transition metal catalyst in an environment substantially free from components that spontaneously react with said catalyst; (b) heating said catalyst of step (a) to a temperature in the range from about 30° C. to about 300° C.; and (c) exposing said catalyst of step (b) to air; wherein said catalyst selected from the group consisting of a metallocene catalyst, components of a metallocene catalyst, a Ziegler-Natta catalyst, and components of a Ziegler-Natta catalyst.
Claim 8
Independent Claim
91 words
A method of producing a substantially environmentally neutral waste from a transition metal catalyst, comprising; (a) placing a transition metal catalyst in an environment substantially free from components that spontaneously react with said catalyst; (b) heating said catalyst of step (a) to a temperature in the range from about 30° C. to about 300° C.; and (c) exposing said catalyst of step (b) to air; wherein said catalyst selected from the group consisting of a metallocene catalyst, components of a metallocene catalyst, a Ziegler-Natta catalyst, and components of a Ziegler-Natta catalyst.
Claim 9
Dependent Claim
74 words
A method of producing a substantially environmentally neutral waste as recited in claim 4 wherein said heating comprises a heat rise of about 10° C. per hour, until a maximum temperature sufficient to volatilize the volatile compounds, and sufficient to cause complex formation, disproportionation or other decomposition of the active, non-volatile catalyst system components is reached, after which the maximum temperature is maintained in the range of from about 10 to about 48 hours.
Claim 10
Dependent Claim
78 words
A deactivation process for a transition metal catalyst, comprising heating a transition metal catalyst system to a temperature sufficient to decompose active compounds in said catalyst system, said temperature being sufficient to drive off volatile compounds, said heating being carried out in a manner to substantially eliminate combustion or violent reaction upon exposure of the catalyst to air, wherein said transition metal catalyst is selected from the group consisting of a Ziegler-Natta catalyst system and a metallocene catalyst.
Claim 11
Dependent Claim
78 words
A deactivation process for a transition metal catalyst, comprising heating a transition metal catalyst system to a temperature sufficient to decompose active compounds in said catalyst system, said temperature being sufficient to drive off volatile compounds, said heating being carried out in a manner to substantially eliminate combustion or violent reaction upon exposure of the catalyst to air, wherein said transition metal catalyst is selected from the group consisting of a Ziegler-Natta catalyst system and a metallocene catalyst.
Claim 12
Independent Claim
93 words
A method for deactivating a transition metal catalyst, said method comprising: (a) placing a transition metal catalyst in a vessel; (b) heating said catalyst to achieve at least a partial decomposition of said catalyst and to volatilize substantially all volatile materials in said vessel; and (c) transferring substantially all non-solid materials from step (b) to a means for safety disposing of said non-solid materials, wherein said transition metal catalyst is selected from the group consisting of a metallocene catalyst, components of a metallocene catalyst, a Ziegler-Natta catalyst, and components of a Ziegler-Natta catalyst.
Claim 13
Independent Claim
93 words
A method for deactivating a transition metal catalyst, said method comprising: (a) placing a transition metal catalyst in a vessel; (b) heating said catalyst to achieve at least a partial decomposition of said catalyst and to volatilize substantially all volatile materials in said vessel; and (c) transferring substantially all non-solid materials from step (b) to a means for safety disposing of said non-solid materials, wherein said transition metal catalyst is selected from the group consisting of a metallocene catalyst, components of a metallocene catalyst, a Ziegler-Natta catalyst, and components of a Ziegler-Natta catalyst.
Claim 14
Dependent Claim
18 words
A method as recited in claim 7, comprising the further step of exposing the solid materials to air.
Claim 15
Dependent Claim
22 words
A method as recited in claim 7 wherein said heating takes place in a controlled amount of one of water or oxygen.
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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) | 1997-12-05 | 1998-06-06 | 1998-12-06 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2001-12-05 | 2002-06-06 | 2002-12-06 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2005-12-05 | 2006-06-06 | 2006-12-06 | $7700.00 | Window Closed / Lapsed |