US4021447A
Expired / Lapsed
US
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Synthesis of zeolite ZSM-4
Assignee: Mobil Oil AS
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Filing: 1975-04-30
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Granted: 1977-05-03
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Expires: 1995-04-30
Abstract
Abstract As synthesized by previous methods, ZSM-4 zeolites are crystallized in the presence of substantial amounts of a tetramethylammonium hydroxide or halide. When synthesized in this way, they contain the tetramethylammonium cation as well as a metal cation such as sodium. To obtain a more catalytically active form, the sodium ion must be exchanged to very low levels. Catalysts prepared in this manner have been found to be quite low in stability. By synthesizing these zeolites in the presence of pyrrolidine or choline salts, ZSM-4 having a different organic nitrogen containing cation but the same crystal structure as previously prepared ZSM-4 is obtained. Catalysts made therefrom are, surprisingly, much more stable than those prepared from ZSM-4 made by previous methods.
Inventors
- 👤 Mae K. Rubin
- 👤 Charles J. Plank
- 👤 Edward J. Rosinski
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 01:33
CPC Classifications
C; C01; C01B; C01B39/00; C01B39/02; C01B39/34; B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/70; B01J29/7011; Y; Y10; Y10S; Y10S423/00; Y10S423/26
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
72 words
A synthetic crystalline aluminosilicate zeolite having a composition as synthesized in terms of moles of oxides as follows: 1.0 ± 0.3 R.sub.2 O : Al.sub.2 O.sub.3 : 3-20 SiO.sub.2 on an anhydrous basis, wherein R is a mixture of alkali metal cations and nitrogen-containing cations derived from a member of the group consisting of choline, choline salts and pyrrolidine and having the X-ray powder diffraction pattern as set forth in Table A.
Claim 2
Dependent Claim
72 words
A synthetic crystalline aluminosilicate zeolite having a composition as synthesized in terms of moles of oxides as follows: 1.0 ± 0.3 R.sub.2 O : Al.sub.2 O.sub.3 : 3-20 SiO.sub.2 on an anhydrous basis, wherein R is a mixture of alkali metal cations and nitrogen-containing cations derived from a member of the group consisting of choline, choline salts and pyrrolidine and having the X-ray powder diffraction pattern as set forth in Table A.
Claim 3
Dependent Claim
66 words
The zeolite of claim 1 having a composition in terms of mole ratios of oxides as follows: 1.0 ± 0.3 [xM.sub.2 O + (1-x)R.sub.2 O] : Al.sub.2 O.sub.3 : 3-20 SiO.sub.2 on an anhydrous basis, wherein R is derived from a member of the group consisting of choline, choline salts and pyrrolidine, M is an alkali metal and x is from about 0.10 to about 0.80.
Claim 4
Dependent Claim
16 words
The zeolite of claim 2 wherein M is sodium and R is derived from choline chloride.
Claim 5
Dependent Claim
15 words
The zeolite of claim 2 wherein M is sodium and R is derived from pyrrolidine.
Claim 6
Dependent Claim
67 words
In a method for synthesizing a ZSM-4 crystalline aluminosilicate zeolite containing an organic nitrogen cation, wherein a reaction mixture comprising sources of silica, alumina, alkali metal, water and organonitrogen cation precursor is prepared and maintained under conditions of temperature and pressure to effect crystallization of said zeolite, the improvement wherein said precursor is derived from a member of the group consisting of choline, choline salts and pyrrolidine.
Claim 7
Dependent Claim
67 words
In a method for synthesizing a ZSM-4 crystalline aluminosilicate zeolite containing an organic nitrogen cation, wherein a reaction mixture comprising sources of silica, alumina, alkali metal, water and organonitrogen cation precursor is prepared and maintained under conditions of temperature and pressure to effect crystallization of said zeolite, the improvement wherein said precursor is derived from a member of the group consisting of choline, choline salts and pyrrolidine.
Claim 8
Dependent Claim
18 words
The method of claim 5 wherein the crystallization temperature is from about 75° C. to about 175° C.
Claim 9
Dependent Claim
11 words
The method of claim 5 wherein the precursor is choline chloride.
Claim 10
Dependent Claim
10 words
The method of claim 5 wherein the precursor is pyrrolidine.
Claim 11
Dependent Claim
21 words
The method of claim 5 wherein all ingredients used to form the ZSM-4 were mixed and vigorously stirred prior to heating.
References Cited (Backward Citations)
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GB1117568A
Cited
US3642434A
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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) | 1980-05-02 | 1980-11-01 | 1981-05-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-05-02 | 1984-11-01 | 1985-05-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-05-02 | 1988-11-01 | 1989-05-03 | $7700.00 | Window Closed / Lapsed |