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US4606900A
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Method of preparing crystalline zeolitic aluminosilicates
Assignee: Sued Chemie AG
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Filing: 1985-01-24
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Granted: 1986-08-19
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Expires: 2005-01-24
Abstract
Abstract There is disclosed an improvement in the preparation of a crystalline zeolitic aluminosilicate with an atomic Si-to-Al ratio ≧10 by hydrothermal crystallization from a reaction batch that contains SiO 2 and Al 2 O 3 or their hydrated derivatives or alkali silicates and aluminates along with crystallization accelerators and optionally in the copresence of a quaternary ammonium compound amino or mixture of alcohol and ammonia, in an aqueous and alkaline medium, the improvement wherein an aged but still X-ray amorphous aluminosilicate nucleating gel with an atomic Si-to-Al ratio ≧10 is added to the reaction batch as a crystallization accelerator.
Inventors
- 👤 Harmut Kacirek
- 👤 Andreas Meyer
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 21:22
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2876; C01B33/113; C01B33/12; C01B33/18; C01B33/181; C01B33/185; C01B39/00; C01B39/02; C01B39/36; C01B39/38; C01P; C01P2002/00; C01P2002/02; Y; Y10; Y10S; Y10S423/00; Y10S423/22
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
92 words
In a method of preparing crystalline ZSM-5 or ZSM 11 zeolites with an atomic Si-to-Al ratio≧10 by hydrothermal crystallization from a reaction batch that contains SiO 2 and Al 2 O 3 or their hydrated derivatives or alkali silicates and aluminates along with crystallization accelerators, in an aqueous and alkaline medium, the improvement wherein an aged but still X-ray amorphous aluminosilicate nucleating gel with an atomic Si-to-Al ratio≧20 which has been aged at 15° to 100° C. from 2 to 100 days is added to the reaction batch as a crystallization accelerator.
Claim 2
Dependent Claim
92 words
In a method of preparing crystalline ZSM-5 or ZSM 11 zeolites with an atomic Si-to-Al ratio≧10 by hydrothermal crystallization from a reaction batch that contains SiO 2 and Al 2 O 3 or their hydrated derivatives or alkali silicates and aluminates along with crystallization accelerators, in an aqueous and alkaline medium, the improvement wherein an aged but still X-ray amorphous aluminosilicate nucleating gel with an atomic Si-to-Al ratio≧20 which has been aged at 15° to 100° C. from 2 to 100 days is added to the reaction batch as a crystallization accelerator.
Claim 3
Dependent Claim
46 words
A method according to claim 1, wherein an aged nucleating gel with the composition (in molar terms) SiO 2 :AlO 2 - ≧20, HO - :SiO 2 =0.05 to 1.0, quaternary ammonium compound:SiO 2 =0.0 to 2.0, H 2 O:SiO 2 =10 to 1000 is employed
Claim 4
Dependent Claim
24 words
A method according to claim 1 wherein the aluminosilicate is prepared from a composition containing a quaternary ammonium compound which is a tetrapropylammonium salt.
Claim 5
Dependent Claim
27 words
A method according to claim 1 wherein the aluminosilicate is prepared in the copresence of a quaternary ammonium compound, amine or a mixture of alcohol and ammonia.
Claim 6
Dependent Claim
22 words
A method according to claim 4 wherein an amine, or a mixture of alcohol and ammonia is present in the reaction mixture.
Claim 7
Dependent Claim
19 words
A method according to claim 1 wherein the nucleating gel is one that has been aged under atmospheric pressure.
Claim 8
Dependent Claim
25 words
A method according to claim 6 wherein the nucleating gel is one that has been aged under atmospheric pressure at 20°-60° C. by 10-50 days.
Claim 9
Dependent Claim
66 words
A method according to claim 1 wherein the aged nucleating gel is added to reaction batches with the composition (in molar terms) SiO 2 :Al 2 O 3 =5, HO - :SiO 2 =10 -10 -1.0, quaternary ammonium compound:SiO 2 =0.01-2.0, H 2 O:SiO 2 =0.7-3000, and Me:SiO 2 =0.3-3.0, where Me is an alkali or alkaline earth metal cation is added to said reaction batch.
Claim 10
Dependent Claim
34 words
A method according to claim 1 wherein 4 to 40% by weight of the aged nucleating gel in terms of the SiO 2 content of the prepared reaction batch is added to the batch.
Claim 11
Dependent Claim
24 words
A method according to claim 9 wherein 15 to 25 percent by weight of the aged nucleating gel is added to said reaction batch.
Claim 12
Dependent Claim
25 words
A method according to claim 1 wherein the aged nucleating gel is employed in a reaction batch at a temperature of 40° to 200° C.
Claim 13
Dependent Claim
36 words
A method according to claim 1 wherein an alkali metal fluoride, or ammonium fluoride, is added to the reaction batch along with the aged nucleating gel at a molar ratio of F - :SiO 2 =0.4-1.5.
Claim 14
Dependent Claim
25 words
A method according to claim 12 wherein an alkali metal fluoride is added to said reaction batch and said alkali metal fluoride is sodium fluoride.
Claim 15
Dependent Claim
46 words
A method according to claim 2 wherein an aged nucleating gel with the composition (in molar terms) SiO 2 :AlO 2 - ≧20, HO - :SiO 2 =0.05 to 1.0 quaternary ammonium compound:SiO 2 =0.01 to 2.0 H 2 O:SiO 2 =10 to 1000 is employed.
Claim 16
Dependent Claim
28 words
A method according to claim 3 wherein the aluminosilicate is prepared from a composition containing a quaternary ammonium compound which is tetrapropylammonium bromide (TPABr) or tetrapropylammonium hydroxide (TPAOH).
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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) | 1989-08-18 | 1990-02-17 | 1990-08-19 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-08-18 | 1994-02-17 | 1994-08-19 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-08-18 | 1998-02-17 | 1998-08-19 | $7700.00 | Window Closed / Lapsed |