US5213786A
Expired / Lapsed
US
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Synthesis of crystalline silicate ZSM-11
Assignee: Mobil Oil AS
•
Filing: 1991-12-20
•
Granted: 1993-05-25
•
Expires: 2011-12-20
Abstract
Abstract This invention relates to a new form of crystalline material identified as zeolite ZSM-11, to a new and useful improvement in synthesizing said crystalline material and to use of said crystalline material prepared in accordance herewith as a catalyst for organic compound, e.g. hydrocarbon compound, conversion.
Inventors
- 👤 Jeffrey S. Beck
- 👤 John D. Schlenker
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 23:56
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/40; C; C01; C01B; C01B37/00; C01B37/02
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
182 words
A method for synthesizing crystalline material exhibiting a characteristic X-ray diffraction pattern including d-spacing maxima values, in Angstroms, as follows: ______________________________________
11.2 ± 0.2
10.1 ± 0.2
6.73 ± 0.2
5.61 ± 0.1
5.03 ± 0.1
4.62 ± 0.1
4.39 ± 0.08
3.86 ± 0.07
3.73 ± 0.07
3.49 ± 0.07
(3.07, 3.00 ± 0.05)
2.01 ± 0.02
______________________________________ which comprises (i) preparing a mixture capable of forming said material, said mixture comprising sources of alkali or alkaline earth metal (M), an oxide of trivalent element (X), an oxide of tetravalent element (Y), water and C n N + (CH 3 ) 3 , wherein n=9, 10, 11 or 12, directing agent (R), and having a composition in terms of mole ratios within the following ranges: ______________________________________
X.sub.2 O.sub.3 /YO.sub.2
0 to .05
H.sub.2 O/YO.sub.2
10 to 200
OH.sup.- /YO.sub.2
10.sup.-6 to 1
M/YO.sub.2 .01 to 2
R/YO.sub.2 .1 to 5;
______________________________________ (ii) maintaining said mixture under sufficient conditions until crystals of said material are formed; and (iii) recovering said crystalline material from step (ii), said recovered crystalline material containing said R.
Claim 2
Independent Claim
182 words
A method for synthesizing crystalline material exhibiting a characteristic X-ray diffraction pattern including d-spacing maxima values, in Angstroms, as follows: ______________________________________
11.2 ± 0.2
10.1 ± 0.2
6.73 ± 0.2
5.61 ± 0.1
5.03 ± 0.1
4.62 ± 0.1
4.39 ± 0.08
3.86 ± 0.07
3.73 ± 0.07
3.49 ± 0.07
(3.07, 3.00 ± 0.05)
2.01 ± 0.02
______________________________________ which comprises (i) preparing a mixture capable of forming said material, said mixture comprising sources of alkali or alkaline earth metal (M), an oxide of trivalent element (X), an oxide of tetravalent element (Y), water and C n N + (CH 3 ) 3 , wherein n=9, 10, 11 or 12, directing agent (R), and having a composition in terms of mole ratios within the following ranges: ______________________________________
X.sub.2 O.sub.3 /YO.sub.2
0 to .05
H.sub.2 O/YO.sub.2
10 to 200
OH.sup.- /YO.sub.2
10.sup.-6 to 1
M/YO.sub.2 .01 to 2
R/YO.sub.2 .1 to 5;
______________________________________ (ii) maintaining said mixture under sufficient conditions until crystals of said material are formed; and (iii) recovering said crystalline material from step (ii), said recovered crystalline material containing said R.
Claim 3
Dependent Claim
39 words
The method of claim 1 wherein said mixture has the following composition ranges: ______________________________________
X.sub.2 O.sub.3 /YO.sub.2
0 to .02
H.sub.2 O/YO.sub.2
10 to 100
OH.sup.- /YO.sub.2
10.sup.-6 to 0.5
M/YO.sub.2 .01 to 1
R/YO.sub.2 .1 to 3.
______________________________________
Claim 4
Dependent Claim
22 words
The method of claim 1 wherein said mixture further comprises seed crystals in sufficient amount to enhance synthesis of said crystalline material.
Claim 5
Dependent Claim
15 words
The method of claim 3 wherein said seed crystals have the structure of ZSM- 11.
Claim 6
Dependent Claim
29 words
The method of claim 1 wherein said X is aluminum, boron, iron, gallium, indium or a mixture thereof, and said Y is silicon, germanium, tin or a mixture thereof.
Claim 7
Dependent Claim
13 words
The method of claim 1 wherein X comprises aluminum and Y comprises silicon.
Claim 8
Dependent Claim
15 words
The method of claim 1 wherein R comprises C 9 N(CH 3 ) 3 Br.
Claim 9
Dependent Claim
15 words
The method of claim 1 wherein R comprises C 12 N(CH 3 ) 3 Br.
Claim 10
Dependent Claim
120 words
A mixture capable of forming crystals of ZSM-11 structure upon crystallization, said mixture comprising sources of alkali or alkaline earth metal (M), trivalent element (X) oxide selected from the group consisting of oxide of aluminum, boron, iron, gallium, indium and mixtures thereof; tetravalent element (Y) oxide selected from the group consisting of oxide of silicon, germanium, tin and mixtures thereof; water and a C n N + (CH 3 ) 3 , wherein n=9, 10, 11, 12, directing agent (R); and having a composition, in terms of mole ratios, within the following ranges: ______________________________________
X.sub.2 O.sub.3 /YO.sub.2
0 to .05
H.sub.2 O/YO.sub.2
10 to 200
OH.sup.- /YO.sub.2
10.sup.-6 to 1 .sup.
M/YO.sub.2 .01 to 2
R/YO.sub.2 .1 to 5.
______________________________________
Claim 11
Dependent Claim
120 words
A mixture capable of forming crystals of ZSM-11 structure upon crystallization, said mixture comprising sources of alkali or alkaline earth metal (M), trivalent element (X) oxide selected from the group consisting of oxide of aluminum, boron, iron, gallium, indium and mixtures thereof; tetravalent element (Y) oxide selected from the group consisting of oxide of silicon, germanium, tin and mixtures thereof; water and a C n N + (CH 3 ) 3 , wherein n=9, 10, 11, 12, directing agent (R); and having a composition, in terms of mole ratios, within the following ranges: ______________________________________
X.sub.2 O.sub.3 /YO.sub.2
0 to .05
H.sub.2 O/YO.sub.2
10 to 200
OH.sup.- /YO.sub.2
10.sup.-6 to 1 .sup.
M/YO.sub.2 .01 to 2
R/YO.sub.2 .1 to 5.
______________________________________
Claim 12
Dependent Claim
64 words
The method of claim 1 comprising replacing ions of the crystalline material recovered in step (iii), at least in part, by ion exchange with an ion or a mixture of ions selected from the group consisting of hydrogen and hydrogen precursors, rare earth metals and metals from Groups IIA, IIIA, IVA, IB, IIB, IIIB, IVB, VIB and VIII of the Periodic Table of Elements.
Claim 13
Dependent Claim
64 words
The method of claim 2 comprising replacing ions of the crystalline material recovered in step (iii), at least in part, by ion exchange with an ion or a mixture of ions selected from the group consisting of hydrogen and hydrogen precursors, rare earth metals and metals from Groups IIA, IIIA, IVA, IB, IIB, IIIB, IVB, VIB and VIII of the Periodic Table of Elements.
Claim 14
Dependent Claim
15 words
The method of claim 10 wherein said replacing ion is hydrogen or a hydrogen precursor.
Claim 15
Dependent Claim
15 words
The method of claim 11 wherein said replacing ion is hydrogen or a hydrogen precursor.
Claim 16
Dependent Claim
7 words
The recovered crystalline material of claim 1.
Claim 17
Dependent Claim
7 words
The recovered crystalline material of claim 2.
Claim 18
Dependent Claim
8 words
The R-containing product crystalline material of claim 10.
Claim 19
Dependent Claim
8 words
The R-containing product crystalline material of claim 11.
Claim 20
Dependent Claim
8 words
The R-containing product crystalline material of claim 12.
Claim 21
Dependent Claim
8 words
The R-containing product crystalline material of claim 13.
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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) | 1996-05-24 | 1996-11-23 | 1997-05-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2000-05-24 | 2000-11-23 | 2001-05-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2004-05-24 | 2004-11-23 | 2005-05-25 | $7700.00 | Window Closed / Lapsed |