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US4713362A Expired / Lapsed US ⏱️ 0.0 years remaining

Selective zeolitic adsorbent and a method for activation thereof

Assignee: Air Products and Chemicals Inc
•
Filing: 1986-05-22
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Granted: 1987-12-15
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Expires: 2006-05-22
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Abstract

Abstract A selective zeolitic adsorbent is prepared by activating a zeolitic composition having at least a portion, preferably at least 50%, of the exchangeable ion capacity occupied by a cation having a charge density of 2.0 or greater, preferably a divalent cation with a charge density of 2.0 or greater, such as calcium or magnesium by thoroughly dehydrating the exchanged zeolite. Additionally, separation ability of the zeolitic adsorbent can be further increased by reacting the thoroughly dehydrated zeolite in an oxidizing atmosphere.

Inventors

  • 👤 Peter J. Maroulis
  • 👤 Charles G. Coe
  • 👤 Steven M. Kuznicki
  • 👤 Patrick J. Clark
  • 👤 David A. Roberts

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 17:59
CPC Classifications
B; B01; B01D; B01D53/00; B01D53/02; B01D53/04; C; C01; C01B; C01B23/00; B01J; B01J20/00; B01J20/02; B01J20/10; B01J20/16; B01J20/18; C01B13/00; C01B13/02; C01B13/0229; C01B13/0248; C01B13/0259; C01B13/0262; C01B13/027; C01B3/00; C01B3/50; C01B3/56; C01B2203/00; C01B2203/04; C01B2203/042; C01B2203/0465; C01B2203/047; C01B2203/048; C01B2210/00; C01B2210/0043; C01B2210/0078; C01B2210/0082

Claims Analysis

Total Claims: 30
Claim 1
Independent Claim 88 words
A method for activation of a zeolitic composition for use as a selective chromatographic adsorbent, wherein said zeolitic composition has at least a portion of any exchangeable ion capacity exchanged with a metal cation having a charge density of about 2.0 or greater, which comprises the steps of: (a) heating said exchanged, zeolitic composition in a nonreactive atmosphere or under a vacuum for a period of time sufficient to thoroughly dehydrate said exchanged, zeolitic composition; and (b) reacting said heat treated, exchanged, zeolitic composition with an oxidizing atmosphere.
Claim 2
Independent Claim 88 words
A method for activation of a zeolitic composition for use as a selective chromatographic adsorbent, wherein said zeolitic composition has at least a portion of any exchangeable ion capacity exchanged with a metal cation having a charge density of about 2.0 or greater, which comprises the steps of: (a) heating said exchanged, zeolitic composition in a nonreactive atmosphere or under a vacuum for a period of time sufficient to thoroughly dehydrate said exchanged, zeolitic composition; and (b) reacting said heat treated, exchanged, zeolitic composition with an oxidizing atmosphere.
Claim 3
Dependent Claim 29 words
The method of claim 1 wherein at least 50% of any exchangeable ion capacity are exchanged with a metal cation having a charge density of about 2.0 or greater.
Claim 4
Dependent Claim 13 words
The method of claim 1 wherein said metal cation is a divalent metal.
Claim 5
Dependent Claim 26 words
The method according to claim 1 wherein said zeolitic composition is selected from the group consisting of chabazite, mordenite, A zeolite, X zeolite and mixtures thereof.
Claim 6
Dependent Claim 11 words
The method of claim 4 wherein said zeolitic composition is chabazite.
Claim 7
Dependent Claim 15 words
The method according to claim 3 wherein said divalent metal is an alkaline earth metal.
Claim 8
Dependent Claim 12 words
The method of claim 6 wherein said alkaline earth metal is calcium.
Claim 9
Dependent Claim 11 words
The method of claim 1 wherein said metal cation is lithium.
Claim 10
Dependent Claim 16 words
The method of claim 1 wherein said zeolite is chabazite and said metal cation is calcium.
Claim 11
Dependent Claim 43 words
The method of claim 1 wherein said heat step comprises gradually heating said zeolitic composition from ambient temperature to about 400° C. and heat soaking said zeolitic composition at temperature for a period of time sufficient to thoroughly dehydrate said exchanged, zeolitic composition.
Claim 12
Dependent Claim 22 words
The method of claim 10 wherein said gradual heating is at a temperature increase in the range of 0.5° to 25° C./min.
Claim 13
Dependent Claim 23 words
The method of claim 10 wherein said gradual heating is at a temperature increase in the range of 3° to 12 ° C./min.
Claim 14
Dependent Claim 19 words
The method of claim 10 wherein said heat soaking is for a period of not less than eight hours.
Claim 15
Dependent Claim 30 words
The method of claim 1 wherein said nonreactive atmosphere is selected from the group consisting of helium, nitrogen, argon, hydrogen, CF 4 , fluorinated hydrocarbons, zero air and mixtures thereof.
Claim 16
Dependent Claim 32 words
The method of claim 1 wherein said reacting comprises gradually heating said exchanged heat treated zeolitic composition from ambient temperature to about 250° C. and heat soaking said zeolite composition at temperature.
Claim 17
Dependent Claim 23 words
The method of claim 15 wherein said gradual heating is at a rate in the range of 2° to 10° C. per minute.
Claim 18
Dependent Claim 19 words
The method of claim 15 wherein said heat soaking is for a period of not less than 1.5 hours.
Claim 19
Dependent Claim 12 words
The method of claim 1 wherein said oxidizing atmosphere is zero air.
Claim 20
Dependent Claim 13 words
The method of claim 1 wherein said oxidizing atmosphere is N 2 O.
Claim 21
Independent Claim 90 words
A method for activation of a zeolitic composition for use as a selective chromatographic adsorbent, wherein said zeolitic composition has at least a portion of any exchangeable ion capacity exchanged with a metal cation having a charge density of about 2.0 or greater, which comprises heating said exchanged zeolitic composition in a nonreactive oxidizing atmosphere from ambient temperature to about 400° C. and heat soaking at that temperature said exchanged zeolitic composition for a period of time sufficient to throughly dehydrate and react in an oxidizing atmosphere the zeolitic composition.
Claim 22
Independent Claim 90 words
A method for activation of a zeolitic composition for use as a selective chromatographic adsorbent, wherein said zeolitic composition has at least a portion of any exchangeable ion capacity exchanged with a metal cation having a charge density of about 2.0 or greater, which comprises heating said exchanged zeolitic composition in a nonreactive oxidizing atmosphere from ambient temperature to about 400° C. and heat soaking at that temperature said exchanged zeolitic composition for a period of time sufficient to throughly dehydrate and react in an oxidizing atmosphere the zeolitic composition.
Claim 23
Dependent Claim 29 words
The method of claim 20 wherein at least 50% of any exchangeable ion capacity are exchanged with a metal cation having a charge density of about 2.0 or greater.
Claim 24
Dependent Claim 22 words
The method of claim 20 wherein said metal cation is selected from the group consisting of calcium, magnesium, lithium and mixtures thereof.
Claim 25
Dependent Claim 26 words
The method according to claim 20 wherein said zeoltic composition is selected from the group consisting of chabazite, mordenite, A zeolite, X zeolite and mixtures thereof.
Claim 26
Dependent Claim 11 words
The method of claim 23 wherein said zeolitic composition is chabazite.
Claim 27
Dependent Claim 85 words
A selective chromatographic adsorbent produced by activation of a zeolitic composition, wherein said zeolitic composition has at least a portion of any exchangeable ion capacity exchanged with a metal cation having a charge density of about 2.0 or greater, said activation comprising the steps of: (a) heating said exchanged, zeolitic composition in a nonreactive atmosphere or under a vacuum for a period of time sufficient to thoroughly dehydrate said exchanged, zeolitic composition; and (b) reacting said heat treated, exchanged, zeolitic composition with an oxidizing atmosphere.
Claim 28
Dependent Claim 85 words
A selective chromatographic adsorbent produced by activation of a zeolitic composition, wherein said zeolitic composition has at least a portion of any exchangeable ion capacity exchanged with a metal cation having a charge density of about 2.0 or greater, said activation comprising the steps of: (a) heating said exchanged, zeolitic composition in a nonreactive atmosphere or under a vacuum for a period of time sufficient to thoroughly dehydrate said exchanged, zeolitic composition; and (b) reacting said heat treated, exchanged, zeolitic composition with an oxidizing atmosphere.
Claim 29
Dependent Claim 87 words
A selective chromatographic adsorbent produced by activation of a zeolitic composition, wherein said zeolitic composition has at least a portion of any exchangeable ion capacity exchanged with a metal cation having a charge density of about 2.0 or greater, said activation comprising heating said exchanged zeolitic composition in a nonreactive oxidizing atmosphere from ambient temperature to about 400° C. and heat soaking at that temperature said exchanged zeolitic composition for a period of time sufficient to thoroughly dehydrate and react in an oxidizing atmosphere the zeolitic composition.
Claim 30
Dependent Claim 87 words
A selective chromatographic adsorbent produced by activation of a zeolitic composition, wherein said zeolitic composition has at least a portion of any exchangeable ion capacity exchanged with a metal cation having a charge density of about 2.0 or greater, said activation comprising heating said exchanged zeolitic composition in a nonreactive oxidizing atmosphere from ambient temperature to about 400° C. and heat soaking at that temperature said exchanged zeolitic composition for a period of time sufficient to thoroughly dehydrate and react in an oxidizing atmosphere the zeolitic composition.

References Cited (Backward Citations)

US3239471A Cited
US3374056A Cited
US3391075A Cited
DD104962A1 Cited
US4544378A Cited
US4536485A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1990-12-14 1991-06-15 1991-12-15 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1994-12-14 1995-06-15 1995-12-15 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1998-12-14 1999-06-15 1999-12-15 $7700.00 Window Closed / Lapsed

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