US5057472A
Expired / Lapsed
US
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Process for the dealumination and ion exchange of zeolites
Assignee: Shell USA Inc
•
Filing: 1989-11-28
•
Granted: 1991-10-15
•
Expires: 2009-11-28
Abstract
Abstract The instant invention comprises a process for concurrently dealuminating and ion exchanging an acid stable sodium ion-containing zeolite by contacting the zeolite with an about 0.5M to about 3M nitric acid solution containing ammonium nitrate in an amount sufficient to fully exchange the sodium ions for ammonium and hydrogen ions at a temperature of at least about -10° C. The instant invention also relates to the zeolites thus prepared by the instant process and catalysts prepared utilizing these zeolites.
Inventors
- 👤 Elliot P. Hertzengerg
- 👤 Brendan D. Murray
- 👤 Gary M. Pasquale
- 👤 Bruce H. C. Winquist
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 23:14
CPC Classifications
C; C10; C10G; C10G35/00; C10G35/04; C10G35/06; C10G35/095; B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/18; B01J29/20; B01J29/22; B01J2229/00; B01J2229/10; B01J2229/16; B01J2229/30; B01J2229/37; B01J2229/42
Claims Analysis
Total Claims: 57
Claim 1
Independent Claim
50 words
A process for concurrently dealuminating and ion exchanging an acid stable sodium ion-containing zeolite which comprises contacting said zeolite with an about 0.5M to about 3M nitric acid solution containing ammonium nitrate in an amount sufficient to fully exchange said sodium ions in said zeolite for ammonium and hydrogen ions.
Claim 2
Dependent Claim
50 words
A process for concurrently dealuminating and ion exchanging an acid stable sodium ion-containing zeolite which comprises contacting said zeolite with an about 0.5M to about 3M nitric acid solution containing ammonium nitrate in an amount sufficient to fully exchange said sodium ions in said zeolite for ammonium and hydrogen ions.
Claim 3
Dependent Claim
23 words
The process of claim 1 wherein said nitric acid solution has a concentration in the range of from about 1M to about 2.5M.
Claim 4
Dependent Claim
27 words
The process of claims 1 or 2 wherein said ammonium nitrate which is added to said nitric acid solution has a concentration of at least about 1M.
Claim 5
Dependent Claim
32 words
The process of claims 1 or 2 wherein said ammonium nitrate which is added to said nitric acid solution has a concentration in the range of from about 2M to about 15M.
Claim 6
Dependent Claim
31 words
The process of claim 1 wherein said dealuminated and ion exchanged zeolite has a SiO 2 /Al 2 O 3 ratio in the range of from about 15.1 to about 26:1.
Claim 7
Dependent Claim
31 words
The process of claim 5 wherein said dealuminated and ion exchanged zeolite has a SiO 2 /Al 2 O 3 ratio in the range of from about 17:1 to about 23:1.
Claim 8
Dependent Claim
21 words
The process of claim 1 wherein said zeolite is contacted with said nitric acid solution containing ammonium nitrate more than once.
Claim 9
Dependent Claim
21 words
The process of claim 7 wherein the number of contacting steps is in the range of from two to about four.
Claim 10
Dependent Claim
19 words
The process of claim 1 wherein said contacting is carried out at a temperature greater than about -10° C.
Claim 11
Dependent Claim
14 words
The process of claim 9 wherein the temperature is greater than about 20° C.
Claim 12
Dependent Claim
17 words
The process of claim 10 wherein the temperature ranges between about 40° C. and about 100° C.
Claim 13
Dependent Claim
10 words
The process of claim 1 wherein said zeolite is mordenite.
Claim 14
Dependent Claim
80 words
A process for concurrently dealuminating and ion exchanging an acid stable sodium-ion containing mordenite which comprises contacting said mordenite with an about 1M to about 2.5M nitric acid solution containing at least about 1M ammonium nitrate in an amount sufficient to fully exchange said sodium ions in said mordenite for ammonium and hydrogen ions to produce a dealuminated, ion exchanged mordenite having a SiO 2 /Al 2 O 3 ratio in the range of from about 15:1 to about 26:1.
Claim 15
Dependent Claim
80 words
A process for concurrently dealuminating and ion exchanging an acid stable sodium-ion containing mordenite which comprises contacting said mordenite with an about 1M to about 2.5M nitric acid solution containing at least about 1M ammonium nitrate in an amount sufficient to fully exchange said sodium ions in said mordenite for ammonium and hydrogen ions to produce a dealuminated, ion exchanged mordenite having a SiO 2 /Al 2 O 3 ratio in the range of from about 15:1 to about 26:1.
Claim 16
Dependent Claim
46 words
A zeolite prepared by a process which comprises contacting an acid stable sodium ion-containing zeolite with an about 0.5M to about 3M nitric acid solution containing ammonium nitrate in an amount sufficient to fully exchange said sodium ions in said zeolite for ammonium and hydrogen ions.
Claim 17
Dependent Claim
46 words
A zeolite prepared by a process which comprises contacting an acid stable sodium ion-containing zeolite with an about 0.5M to about 3M nitric acid solution containing ammonium nitrate in an amount sufficient to fully exchange said sodium ions in said zeolite for ammonium and hydrogen ions.
Claim 18
Dependent Claim
23 words
The zeolite of claim 14 wherein said nitric acid solution has a concentration in the range of from about 1M to about 2.5M.
Claim 19
Dependent Claim
27 words
The zeolite of claims 14 or 15 wherein said ammonium nitrate which is added to said nitric acid solution has a concentration of at least about 1.0M.
Claim 20
Dependent Claim
32 words
The zeolite of claims 14 or 15 wherein said ammonium nitrate which is added to said nitric acid solution has a concentration in the range of from about 2M to about 15M.
Claim 21
Dependent Claim
31 words
The zeolite of claim 14 wherein said dealuminated and ion exchanged zeolite has a SiO 2 /Al 2 O 3 ratio in the range of from about 15:1 to about 26:1.
Claim 22
Dependent Claim
31 words
The zeolite of claim 18 wherein said dealuminated and ion exchanged zeolite has a SiO 2 /Al 2 O 3 ratio in the range of from about 17:1 to about 23:1.
Claim 23
Dependent Claim
21 words
The zeolite of claim 14 wherein said zeolite is contacted with said nitric acid solution containing ammonium nitrate more than once.
Claim 24
Dependent Claim
21 words
The zeolite of claim 20 wherein the number of contacting steps is in the range of from two to about four.
Claim 25
Dependent Claim
19 words
The zeolite of claim 14 wherein said contacting is carried out at a temperature greater than about -10° C.
Claim 26
Dependent Claim
13 words
The zeolite of claim 22 wherein the temperature is greater than 20° C.
Claim 27
Dependent Claim
17 words
The zeolite of claim 23 wherein the temperature ranges between about 40° C. and about 100° C.
Claim 28
Dependent Claim
10 words
The zeolite of claim 14 wherein said zeolite is mordenite.
Claim 29
Dependent Claim
33 words
The zeolite of claim 14 wherein said zeolite is additionally calcined at a temperature sufficient to at least partially convert the ammonium hydrogen form of the zeolite to a hygrogen form of zeolite.
Claim 30
Dependent Claim
25 words
The zeolite of claim 26 wherein said zeolite is calcined at a temperature in the range of from about 350° C. to about 650° C.
Claim 31
Dependent Claim
25 words
The zeolite of claim 25 wherein said zeolite is calcined at a temperature in the range of from about 475° C. to about 575° C.
Claim 32
Dependent Claim
17 words
The zeolite of claim 14 or 26 wherein said zeolite is additionally admixed with an inorganic oxide.
Claim 33
Dependent Claim
20 words
The zeolite of claim 28 wherein said inorganic oxide is selected from the group consisting of alumina, silica and silica-alumina.
Claim 34
Dependent Claim
69 words
A mordenite having a SiO 2 /Al 2 O 3 ratio in the range of from about 15:1 to about 26:1 prepared by a process which comprises contacting said mordenite with an about 1M to about 2.5M nitric acid solution containing ammonium nitrate having a concentration of at least about 1M in an amount sufficient to fully exchange said sodium ions in said mordenite for ammonium and hydrogen ions.
Claim 35
Dependent Claim
69 words
A mordenite having a SiO 2 /Al 2 O 3 ratio in the range of from about 15:1 to about 26:1 prepared by a process which comprises contacting said mordenite with an about 1M to about 2.5M nitric acid solution containing ammonium nitrate having a concentration of at least about 1M in an amount sufficient to fully exchange said sodium ions in said mordenite for ammonium and hydrogen ions.
Claim 36
Dependent Claim
85 words
A zeolite catalyst comprising at least one metal selected from Group VIII and a zeolite prepared of a process which comprises contacting an acid stable sodium ion-containing zeolite with an about 0.5M to about 3M nitric acid solution containing ammonium nitrate in an amount sufficient to fully exchange said sodium ions in said zeolite for ammonium and hydrogen ions and subsequently calcining at a temperature sufficient to at least partially convert the ammonium hydrogen form of the zeolite to a hydrogen form of the zeolite.
Claim 37
Dependent Claim
85 words
A zeolite catalyst comprising at least one metal selected from Group VIII and a zeolite prepared of a process which comprises contacting an acid stable sodium ion-containing zeolite with an about 0.5M to about 3M nitric acid solution containing ammonium nitrate in an amount sufficient to fully exchange said sodium ions in said zeolite for ammonium and hydrogen ions and subsequently calcining at a temperature sufficient to at least partially convert the ammonium hydrogen form of the zeolite to a hydrogen form of the zeolite.
Claim 38
Dependent Claim
12 words
The catalyst of claim 32 wherein said Group VIII metal is platinum.
Claim 39
Dependent Claim
20 words
The catalyst of claim 33 wherein said catalyst contains from about 0.01 to about 10 percent by weight of platinum.
Claim 40
Dependent Claim
12 words
The catalyst of claim 32 wherein said Group VIII metal is palladium.
Claim 41
Dependent Claim
20 words
The catalyst of claim 35 wherein said catalyst contains from about 0.01 to about 10 percent by weight of palladium.
Claim 42
Dependent Claim
14 words
The catalyst of claim 32 wherein said Group VIII metals are platinum and palladium.
Claim 43
Dependent Claim
32 words
The catalyst of claim 37 wherein said catalyst contains from about 0.01 to about 10 percent by weight of platinum and from about 0.01 to about 10 percent by weight of palladium.
Claim 44
Dependent Claim
23 words
The catalyst of claim 32 wherein said nitric acid solution has a concentration in the range of from about 1M to about 2.5M.
Claim 45
Dependent Claim
26 words
The catalyst of claims 32 or 39 said ammonium nitrate which is added to said nitric acid solution has a concentration of at least about 1M.
Claim 46
Dependent Claim
32 words
The catalyst of claims 32 or 39 wherein said ammonium nitrate which is added to said nitric acid solution has a concentration in the range of from about 2M to about 15M.
Claim 47
Dependent Claim
31 words
The catalyst of claim 32 wherein said dealuminated and ion exchanged zeolite has a SiO 2 /Al 2 O 3 ratio in the range of from about 15:1 to about 26:1.
Claim 48
Dependent Claim
31 words
The catalyst of claim 42 wherein said dealuminated and ion exchanged zeolite has a SiO 2 /Al 2 O 3 ratio in the range of from about 17:1 to about 23:1.
Claim 49
Dependent Claim
21 words
The catalyst of claim 32 wherein said zeolite is contacted with said nitric acid solution containing ammonium nitrate more than once.
Claim 50
Dependent Claim
21 words
The catalyst of claim 44 wherein the number of contacting steps is in the range of from two to about four.
Claim 51
Dependent Claim
10 words
The catalyst of claim 32 wherein the zeolite is mordenite.
Claim 52
Dependent Claim
26 words
The catalyst of claim 32 wherein said zeolite is additionally calcined at a temperature in the range of from about 350° C. to about 650° C.
Claim 53
Dependent Claim
25 words
The catalyst of claim 46 wherein said zeolite is calcined at a temperature in the range of from about 475° C. to about 575° C.
Claim 54
Dependent Claim
13 words
The catalyst of claim 32 wherein said catalyst additionally comprises an inorganic oxide.
Claim 55
Dependent Claim
20 words
The catalyst of claim 49 wherein said inorganic oxide is selected from the group consisting of alumina, silica and silica-alumina.
Claim 56
Dependent Claim
84 words
A zeolite catalyst comprising at least one metal selected from Group VIII and a mordenite prepared by a process which comprises contacting an acid stable sodium ion-containing mordenite with an about 1M to about 2.5M nitric acid solution containing ammonium nitrate having a concentration of at least about 1M in an amount sufficient to fully exchange said sodium ions in said mordenite for ammonium and hydrogen ions and subsequently calcining at a temperature in the range between about 350° C. and about 650° C.
Claim 57
Dependent Claim
84 words
A zeolite catalyst comprising at least one metal selected from Group VIII and a mordenite prepared by a process which comprises contacting an acid stable sodium ion-containing mordenite with an about 1M to about 2.5M nitric acid solution containing ammonium nitrate having a concentration of at least about 1M in an amount sufficient to fully exchange said sodium ions in said mordenite for ammonium and hydrogen ions and subsequently calcining at a temperature in the range between about 350° C. and about 650° C.
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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) | 1994-10-14 | 1995-04-15 | 1995-10-15 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1998-10-14 | 1999-04-15 | 1999-10-15 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2002-10-14 | 2003-04-15 | 2003-10-15 | $7700.00 | Window Closed / Lapsed |