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US4581216A
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Process for preparing crystalline aluminosilicate zeolites using a carboxylic acid
Assignee: Toray Industries Inc
•
Filing: 1985-01-22
•
Granted: 1986-04-08
•
Expires: 2005-01-22
Abstract
Abstract A crystalline aluminosilicate zeolite is obtained by stirring under heating an aqueous reaction mixture containing a silica source, an alumina source, an alkali source and an organic carboxylic acid.
Inventors
- 👤 Kazuyoshi Iwayama
- 👤 Takao Kamano
- 👤 Kuniyuki Tada
- 👤 Takehisa Inoue
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 09:17
CPC Classifications
C; C01; C01B; C01B39/00; C01B39/02; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2861; Y; Y10; Y10S; Y10S423/00; Y10S423/34
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
198 words
A process for preparing a crystalline aluminosilicate zeolite, which process comprises reacting an aqueous reaction mixture containing a silica source, an alumina source, an alkali source and a single organic template selected from the group consisting of benzoic acid, phthalic acid, terephthalic acid, salicyclic acid, para-hydroxybenzoic acid, toluic acid, and alkali metal salts thereof, and the composition, in terms of mole ratios, of said reaction mixture being as follows: ______________________________________
SiO.sub.2 Al.sub.2 O.sub.3
above 20
H.sub.2 O/SiO.sub.2 5 to 100
OH.sup.- /SiO.sub.2 0.05 to 0.40
A/Al.sub.2 O.sub.3 0.10 to 200
______________________________________ wherein A represents said organic compound, said process being conducted at a crystallization temperature of 140°-180° C. to form a crystalline aluminosilicate zeolite having the following X-ray diffraction pattern: ______________________________________
d(Å)
100 I/I.sub.o
______________________________________
11.2 ± 002
S
10.1 ± 0.2
S
9.8 ± 0.2
M
6.37 ± 0.1
W
6.00 ± 0.1
W
5.71 ± 0.1
W
5.58 ± 0.1
W
4.37 ± 0.08
W
4.27 ± 0.08
W
3.86 ± 0.08
VS
3.82 ± 0.02
VS
3.75 ± 0.08
S
3.72 ± 0.08
S
3.66 ± 0.05
M
3.00 ± 0.05
M
2.00 ± 0.05
W
______________________________________ wherein VS=very strong, S=strong, M=medium strength and W=weak.
Claim 2
Dependent Claim
198 words
A process for preparing a crystalline aluminosilicate zeolite, which process comprises reacting an aqueous reaction mixture containing a silica source, an alumina source, an alkali source and a single organic template selected from the group consisting of benzoic acid, phthalic acid, terephthalic acid, salicyclic acid, para-hydroxybenzoic acid, toluic acid, and alkali metal salts thereof, and the composition, in terms of mole ratios, of said reaction mixture being as follows: ______________________________________
SiO.sub.2 Al.sub.2 O.sub.3
above 20
H.sub.2 O/SiO.sub.2 5 to 100
OH.sup.- /SiO.sub.2 0.05 to 0.40
A/Al.sub.2 O.sub.3 0.10 to 200
______________________________________ wherein A represents said organic compound, said process being conducted at a crystallization temperature of 140°-180° C. to form a crystalline aluminosilicate zeolite having the following X-ray diffraction pattern: ______________________________________
d(Å)
100 I/I.sub.o
______________________________________
11.2 ± 002
S
10.1 ± 0.2
S
9.8 ± 0.2
M
6.37 ± 0.1
W
6.00 ± 0.1
W
5.71 ± 0.1
W
5.58 ± 0.1
W
4.37 ± 0.08
W
4.27 ± 0.08
W
3.86 ± 0.08
VS
3.82 ± 0.02
VS
3.75 ± 0.08
S
3.72 ± 0.08
S
3.66 ± 0.05
M
3.00 ± 0.05
M
2.00 ± 0.05
W
______________________________________ wherein VS=very strong, S=strong, M=medium strength and W=weak.
Claim 3
Dependent Claim
24 words
A process according to claim 1, in which said organic template is a compound that is water soluble in its alkali metal salt form.
Claim 4
Dependent Claim
14 words
A process according to claim 1, in which said organic template is salicylic acid.
Claim 5
Dependent Claim
19 words
A process according to claim 1, in which said process requires from 5 hours to 30 days for completion.
Claim 6
Dependent Claim
211 words
A process for preparing a crystalline aluminosilicate zeolite, which process comprises reacting an aqueous reaction mixture containing a silica source, an alumina source, an alkali source and a single organic template, selected from the group consisting of benzoic acid, phthalic acid, terephthalic acid, salicyclic acid, para-hydroxybenzoic acid, toluic acid, and alkali metal salts thereof, and the composition, in terms of mole ratios, of said reaction mixture being as follows: ______________________________________
SiO.sub.2 Al.sub.2 O.sub.3
15 to 75
H.sub.2 O/SiO.sub.2 10 to 50
OH.sup.- /SiO.sub.2 0.14 to 0.40
A/Al.sub.2 O.sub.3 0.10 to 50
______________________________________ wherein A represents said organic compound, said process being conducted at a crystallization temperature of 140°-180° C. to form a crystalline aluminosilicate zeolite having the following X-ray diffraction pattern: ______________________________________
d(Å)
100 I/I.sub.o
______________________________________
13.6 ± 0.2
M
10.2 ± 0.2
W
9.0 ± 0.2
S
6.56 ± 0.1
S
6.40 ± 0.1
S
6.05 ± 0.1
W
5.80 ± 0.1
M
4.52 ± 0.08
M
3.99 ± 0.08
S
3.83 ± 0.08
W
3.76 ± 0.08
W
3.53 ± 0.05
W
3.46 ± 0.05
VS
3.38 ± 0.05
S
3.28 ± 0.05
W
3.20 ± 0.05
S
3.15 ± 0.05
W
2.89 ± 0.05
M
2.51 ± 0.05
W
______________________________________ wherein VS=very strong, S=strong, M=medium strength and W=weak.
Claim 7
Dependent Claim
211 words
A process for preparing a crystalline aluminosilicate zeolite, which process comprises reacting an aqueous reaction mixture containing a silica source, an alumina source, an alkali source and a single organic template, selected from the group consisting of benzoic acid, phthalic acid, terephthalic acid, salicyclic acid, para-hydroxybenzoic acid, toluic acid, and alkali metal salts thereof, and the composition, in terms of mole ratios, of said reaction mixture being as follows: ______________________________________
SiO.sub.2 Al.sub.2 O.sub.3
15 to 75
H.sub.2 O/SiO.sub.2 10 to 50
OH.sup.- /SiO.sub.2 0.14 to 0.40
A/Al.sub.2 O.sub.3 0.10 to 50
______________________________________ wherein A represents said organic compound, said process being conducted at a crystallization temperature of 140°-180° C. to form a crystalline aluminosilicate zeolite having the following X-ray diffraction pattern: ______________________________________
d(Å)
100 I/I.sub.o
______________________________________
13.6 ± 0.2
M
10.2 ± 0.2
W
9.0 ± 0.2
S
6.56 ± 0.1
S
6.40 ± 0.1
S
6.05 ± 0.1
W
5.80 ± 0.1
M
4.52 ± 0.08
M
3.99 ± 0.08
S
3.83 ± 0.08
W
3.76 ± 0.08
W
3.53 ± 0.05
W
3.46 ± 0.05
VS
3.38 ± 0.05
S
3.28 ± 0.05
W
3.20 ± 0.05
S
3.15 ± 0.05
W
2.89 ± 0.05
M
2.51 ± 0.05
W
______________________________________ wherein VS=very strong, S=strong, M=medium strength and W=weak.
Claim 8
Dependent Claim
24 words
A process according to claim 5, in which said organic template is a compound that is water soluble in its alkali metal salt form.
Claim 9
Dependent Claim
14 words
A process according to claim 5, in which said organic template is salicylic acid.
Claim 10
Dependent Claim
19 words
A process according to claim 5, in which said process requires from 5 hours to 30 days for completion.
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) | 1989-04-07 | 1989-10-07 | 1990-04-08 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-04-07 | 1993-10-07 | 1994-04-08 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-04-07 | 1997-10-07 | 1998-04-08 | $7700.00 | Window Closed / Lapsed |