US3878128A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method for manufacturing an adsorbent useful for olefin separation
Assignee: Universal Oil Products Co
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Filing: 1973-09-28
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Granted: 1975-04-15
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Expires: 1993-09-28
Abstract
Abstract A method for the production of a solid adsorbent useful in the separation of olefins from a hydrocarbon feed mixture comprising olefins and paraffins. The method basically comprises the steps of: contacting a base material comprising type X or type Y structured zeolite with a fluoride-containing solution of sodium hydroxide to effect the addition of alkali metal cations to and the extraction of alumina from the base material; washing the material at washing conditions until substantially free of sodium hydroxide; and drying the treated base material at conditions to reduce the LOI at 900*C. to less than about 10 wt. %. The combination fluoride-caustic treatment produces a superior adsorbent for separating olefins from a hydrocarbon feed mixture comprising olefins and paraffins. The adsorbent produced has increased capacity for olefins, decreased catalytic activity and reduced dustiness.
Inventors
- 👤 Donald H Rosback
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 20:15
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/02; B01J20/10; B01J20/16; B01J20/18; B01J20/186; Y; Y10; Y10S; Y10S423/00; Y10S423/21
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
85 words
A METHOD OF MANUFACTURING A SOLID ADSORBENT COMPRISING THE STEPS OF: A. CONTACTING A BASE MATERIAL COMPRISING X OR Y ZEOLITE WITH A FLUORIDE-CONTAINING AQUEOUS SOLUTION OF SODIUM HYDROXIDE AT ION EXCHANGE CONDITIONS TO EFFECT THE ADDITION OF SODIUM CATIONS TO AND THE EXTRACTION OF ALUMINA FROM SAID BASE MATERIAL; B. WASHING THE ION EXCHANGED MATERIAL AT WASHING CONDITIONS UNTIL SUBSTANTIALLY FREE OF SODIUM HYDROXIDE; C. DRYING THE ADSORBENT AT DRYING CONDITIONS TO REDUCE THE LOI AT 900*C. TO LESS THAN ABOUT 10 WT. %.
Claim 2
Independent Claim
85 words
A METHOD OF MANUFACTURING A SOLID ADSORBENT COMPRISING THE STEPS OF: A. CONTACTING A BASE MATERIAL COMPRISING X OR Y ZEOLITE WITH A FLUORIDE-CONTAINING AQUEOUS SOLUTION OF SODIUM HYDROXIDE AT ION EXCHANGE CONDITIONS TO EFFECT THE ADDITION OF SODIUM CATIONS TO AND THE EXTRACTION OF ALUMINA FROM SAID BASE MATERIAL; B. WASHING THE ION EXCHANGED MATERIAL AT WASHING CONDITIONS UNTIL SUBSTANTIALLY FREE OF SODIUM HYDROXIDE; C. DRYING THE ADSORBENT AT DRYING CONDITIONS TO REDUCE THE LOI AT 900*C. TO LESS THAN ABOUT 10 WT. %.
Claim 3
Dependent Claim
21 words
The method of claim 1 further characterized in that said base material has a Na2O/Al2O3 ratio of about 0.7 or less.
Claim 4
Dependent Claim
38 words
The method of claim 1 further characterized in that said solution contains sodium fluoride in a concentration of less than its solubility limit and sodium hydroxide in a concentration of from about 0.5 to about 10 wt. %.
Claim 5
Dependent Claim
28 words
The method of claim 1 further characterized in that said ion exchange conditions include a temperature within the range of from about 50* F. to about 250* F.
Claim 6
Dependent Claim
22 words
The method of claim 1 further characterized in that said sodium exchanged base material has a Na2O/Al2O3 ratio greater than about 0.7.
Claim 7
Dependent Claim
41 words
The method of claim 1 further characterized in that said washing conditions include a pH sufficient to preclude formation of the hydrogen form of the zeolite, and a temperature within the range of from about 50* F. to about 250* F.
Claim 8
Dependent Claim
27 words
The method of claim 1 further characterized in that said drying conditions include a temperature within the range of from about 100* F. to about 1,000* F.
Claim 9
Independent Claim
106 words
A method of manufacturing a solid adsorbent which method comprises the steps of: a. contacting a base material comprising X or Y structured zeolite having a Na2O/Al2O3 ratio of about 0.7 or less with a fluoride-containing aqueous sodium hydroxide solution at ion exchange conditions to increase the sodium cation content of said mass to a Na2O/Al2O3 ratio of greater than about 0.7 and extract alumina from said base material; b. washing the sodium-exchanged base material at washing conditions until substantially free of sodium hydroxide; and, c. drying the adsorbent at conditions sufficient to reduce the LOI at 900* C. to less than about 10 wt. %.
Claim 10
Independent Claim
106 words
A method of manufacturing a solid adsorbent which method comprises the steps of: a. contacting a base material comprising X or Y structured zeolite having a Na2O/Al2O3 ratio of about 0.7 or less with a fluoride-containing aqueous sodium hydroxide solution at ion exchange conditions to increase the sodium cation content of said mass to a Na2O/Al2O3 ratio of greater than about 0.7 and extract alumina from said base material; b. washing the sodium-exchanged base material at washing conditions until substantially free of sodium hydroxide; and, c. drying the adsorbent at conditions sufficient to reduce the LOI at 900* C. to less than about 10 wt. %.
Claim 11
Dependent Claim
37 words
The method of claim 8 further characterized in that said solution contains fluoride in a concentration of less than its solubility limit and sodium hydroxide in a concentration of from about 0.5 to about 10 wt. %.
Claim 12
Dependent Claim
28 words
The method of claim 8 further characterized in that said ion exchange conditions include a temperature within the range of from about 50* F. to about 250* F.
Claim 13
Dependent Claim
41 words
The method of claim 8 further characterized in that said washing conditions include a pH sufficient to preclude formation of the hydrogen form of the zeolite, and a temperature within the range of from about 50* F. to about 250* F.
Claim 14
Dependent Claim
27 words
The method of claim 8 further characTerized in that said drying conditions include a temperature within the range of from about 100* F. to about 1,000* F.
Claim 15
Dependent Claim
77 words
A solid adsorbent prepared by contacting a base material comprising X or Y structured zeolite with a fluoride-containing aqueous sodium hydroxide solution at ion exchange conditions to effect the addition of sodium cations to and the extraction of alumina from said base material, washing the sodium-exchange base material at washing conditions until essentially free of sodium hydroxide and drying the adsorbent at conditions to reduce the LOI at 900* C. to less than about 10 wt. %.
Claim 16
Dependent Claim
77 words
A solid adsorbent prepared by contacting a base material comprising X or Y structured zeolite with a fluoride-containing aqueous sodium hydroxide solution at ion exchange conditions to effect the addition of sodium cations to and the extraction of alumina from said base material, washing the sodium-exchange base material at washing conditions until essentially free of sodium hydroxide and drying the adsorbent at conditions to reduce the LOI at 900* C. to less than about 10 wt. %.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-04-14 | 1978-10-14 | 1979-04-15 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-04-14 | 1982-10-14 | 1983-04-15 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-04-14 | 1986-10-14 | 1987-04-15 | $7700.00 | Window Closed / Lapsed |