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US4401634A
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Two step process for the preparation of zeolite A by hydrothermal treatment of clinoptilolite
Assignee: Lyondell Chemical Technology LP
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Filing: 1982-01-28
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Granted: 1983-08-30
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Expires: 2002-01-28
Abstract
Abstract A two step hydrothermal process for the preparation of zeolite A from clinoptilolite by (1) heat treating a mixture of clinoptilolite in an aqueous solution of sodium hydroxide and filtering the mixture followed by (2) reacting the filtrate with at least 75 percent of a stoichiometric amount of sodium aluminate to form and precipitate zeolite A from solution and recovering zeolite A.
Inventors
- 👤 Hsiang-ning Sun
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 09:52
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2815; Y; Y10; Y10S; Y10S423/00; Y10S423/24
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
185 words
A hydrothermal process for the preparation of a sodium cation form of zeolite A from natural clinoptilolite of the formula Na.sub.x (AlO.sub.2).sub.x (SiO.sub.2).sub.y.ZH.sub.2 O wherein x=5 to 7, y/x=4.5 to 5.5 and z=1 to 30 which comprises the steps of: (a) heating at a temperature of from about 60° C. to 110° C. said natural clinoptilolite in a 1 to 30 weight percent aqueous solution of sodium hydroxide to dissolve clinoptilolite, the clinoptilolite having a concentration of at least one gram clinoptilolite per 100 cc of aqueous sodium hydroxide solution; (b) filtering the clinoptilolite-sodium hydroxide solution to remove undissolved clinoptilolite and elemental impurities and form a filtrate; (c) reacting the filtrate at a temperature of from about 60° C. to 110° C. in the presence of up to 15 weight percent NaCl with at least 75 percent of a stoichiometric amount of sodium aluminate in an aqueous solution to precipitate and form zeolite A having a mean particle size of about 3 to 6 microns, said sodium aluminate having a concentration of from 1 to 16.5 weight percent in water; and recovering said zeolite A.
Claim 2
Dependent Claim
185 words
A hydrothermal process for the preparation of a sodium cation form of zeolite A from natural clinoptilolite of the formula Na.sub.x (AlO.sub.2).sub.x (SiO.sub.2).sub.y.ZH.sub.2 O wherein x=5 to 7, y/x=4.5 to 5.5 and z=1 to 30 which comprises the steps of: (a) heating at a temperature of from about 60° C. to 110° C. said natural clinoptilolite in a 1 to 30 weight percent aqueous solution of sodium hydroxide to dissolve clinoptilolite, the clinoptilolite having a concentration of at least one gram clinoptilolite per 100 cc of aqueous sodium hydroxide solution; (b) filtering the clinoptilolite-sodium hydroxide solution to remove undissolved clinoptilolite and elemental impurities and form a filtrate; (c) reacting the filtrate at a temperature of from about 60° C. to 110° C. in the presence of up to 15 weight percent NaCl with at least 75 percent of a stoichiometric amount of sodium aluminate in an aqueous solution to precipitate and form zeolite A having a mean particle size of about 3 to 6 microns, said sodium aluminate having a concentration of from 1 to 16.5 weight percent in water; and recovering said zeolite A.
Claim 3
Dependent Claim
24 words
A process according to claim 1 wherein the aqueous sodium hydroxide solution is in the range of from 10 to 20 percent by weight.
Claim 4
Dependent Claim
25 words
A process according to claim 1 wherein the concentration of clinoptilolite is from 4 to 15 g. per 100 cc of aqueous sodium hydroxide solution.
Claim 5
Dependent Claim
27 words
A process according to claim 1 wherein the temperature of heating in step (a) and reacting the filtrate in step (c) is from 90° to 100° C.
Claim 6
Dependent Claim
34 words
A process according to claim 1 wherein the heating in step (a) and reacting the filtrate in step (c) are carried out at a temperature of from 110° C. to 150° C. under pressure.
Claim 7
Dependent Claim
29 words
The process according to claim 1 wherein the heating in step (a) and reacting the filtrate in step (c) are carried out for from 15 minutes to 4 hours.
Claim 8
Dependent Claim
15 words
The process of claim 6 wherein the time is from 15 minutes to 1 hour.
Claim 9
Dependent Claim
18 words
A process according to claim 1 wherein a stoichiometric amount of sodium aluminate in aqueous solution is employed.
Claim 10
Dependent Claim
21 words
A process according to claim 1 wherein said sodium aluminate concentration in water is from 4 to 15 percent by weight.
Claim 11
Dependent Claim
21 words
A process according to claim 1 wherein the NaCl based on the aqueous sodium hydroxide solution is added in step (a).
Claim 12
Dependent Claim
21 words
A process according to claim 1 wherein the NaCl based on the sodium aluminate aqueous solution is added in step (c).
Claim 13
Dependent Claim
27 words
A process according to claim 1 wherein from 0 to 30 weight percent sodium hydroxide based on the aqueous sodium aluminate solution is added in step (c).
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) | 1986-08-29 | 1987-02-28 | 1987-08-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-08-29 | 1991-02-28 | 1991-08-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-08-29 | 1995-02-28 | 1995-08-30 | $7700.00 | Window Closed / Lapsed |