US4400366A
Expired / Lapsed
US
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Method of making zeolites
Assignee: Albemarle Corp
•
Filing: 1981-09-08
•
Granted: 1983-08-23
•
Expires: 2001-09-08
Abstract
Abstract The present invention relates to a process for producing a crystalline synthetic faujasite wherein an activated sodium silicate system is provided by mixing a sodium silicate solution with a seed amount of the faujasite to be produced and the activated sodium silicate system is reacted with a sodium aluminate solution under controlled conditions to thereby form the desired crystalline synthetic faujasite.
Inventors
- 👤 Robert N. Sanders
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 19:38
CPC Classifications
C; C01; C01B; C01B39/00; C01B39/02; C01B39/20; Y; Y10; Y10S; Y10S423/00; Y10S423/21
Claims Analysis
Total Claims: 27
Claim 1
Independent Claim
158 words
A method of producing a crystalline synthetic faujasite, comprising the steps of separately preparing a sodium silicate solution and a sodium aluminate solution, providing an activated system comprising a sodium silicate solution mixed with agitation for a period of at least about one-half hour with a seed amount of bulk synthetic faujasite of the type product desired ground to a fine powder at a temperature up to about 0° C. mixing the sodium aluminate solution with the activated system over a period of up to about five hours to provide a mixture having a silica to alumina molar ratio of between 2.5:1 and 15:1, allowing the mixture to stand for up to about sixteen hours at a temperature from about 0° C. to ambient, heating the mixture to a temperature of about 90° C.-105° C., reacting the mixture at a temperature of about 90° C.-105° C. until the desired crystalline synthetic faujasite is formed, and recovering said faujasite.
Claim 2
Independent Claim
158 words
A method of producing a crystalline synthetic faujasite, comprising the steps of separately preparing a sodium silicate solution and a sodium aluminate solution, providing an activated system comprising a sodium silicate solution mixed with agitation for a period of at least about one-half hour with a seed amount of bulk synthetic faujasite of the type product desired ground to a fine powder at a temperature up to about 0° C. mixing the sodium aluminate solution with the activated system over a period of up to about five hours to provide a mixture having a silica to alumina molar ratio of between 2.5:1 and 15:1, allowing the mixture to stand for up to about sixteen hours at a temperature from about 0° C. to ambient, heating the mixture to a temperature of about 90° C.-105° C., reacting the mixture at a temperature of about 90° C.-105° C. until the desired crystalline synthetic faujasite is formed, and recovering said faujasite.
Claim 3
Dependent Claim
13 words
The method of claim 1, wherein said crystalline synthetic faujasite is zeolite Y.
Claim 4
Dependent Claim
13 words
The method of claim 1, wherein said crystalline synthetic faujasite is zeolite X.
Claim 5
Dependent Claim
24 words
The method of claim 1, wherein the activating faujasite is added in an amount of about 1% to 10% by weight of the mixture.
Claim 6
Dependent Claim
24 words
The method of claim 1, wherein the mixing period for the sodium aluminate solution with the activated system is about three to four hours.
Claim 7
Dependent Claim
16 words
The method of claim 1, wherein the reaction mixture is allowed to stand at ambient temperature.
Claim 8
Dependent Claim
23 words
The method of claim 1, wherein the reaction mixture is allowed to stand for a period of time of at least six hours.
Claim 9
Dependent Claim
18 words
The method of claim 1, wherein the total mixture has the following molar ratio: (4.2-4.4)Na.sub.2 O.Al.sub.2 O.sub.3.(2.8-3.0)SiO.sub.2.(150-180)H.sub.2 O.
Claim 10
Dependent Claim
21 words
The method of claim 1, wherein the reactants are mixed at a temperature at least as low as about 0° C.
Claim 11
Dependent Claim
10 words
The method of claim 1, wherein agitation is by stirring.
Claim 12
Independent Claim
229 words
A method of preparing a crystalline zeolite Y, comprising the steps of: (a) dissolving sand in a sodium hydroxide solution at a pressure of at least 100 psig and a temperature of at least 130° C. to produce a sodium silicate solution having a silica to sodium oxide molar ratio of between 2.0:1 and 2.6:1; (b) providing an activated system comprising a sodium silicate solution mixed with agitation for a period of at least about one-half hour with a seed amount of bulk zeolite Y ground to a fine powder at a temperature up to about 0° C.; (c) forming a sodium aluminate solution; (d) adding the sodium aluminate to the activated system over a period of from about five minutes to five hours with stirring to produce a reaction mixture comprising a sodium silicate mother liquor and an amorphous sodium alumino silicate pigment, said mixture having a sodium oxide to silica molar ratio of between 0.5:1 and 1:1, a silica to alumina molar ratio of between 10:1 and 15:1, and a water to sodium oxide molar ratio of between 40:1 and 60:1; (e) allowing the mixture to stand up to about 16 hours at a temperature of about 0° C. to ambient; (f) heating and reacting the mixture at a temperature of about 90° C.-105° C. until crystalline zeolite Y is formed; and (g) recovering the zeolite Y.
Claim 13
Independent Claim
229 words
A method of preparing a crystalline zeolite Y, comprising the steps of: (a) dissolving sand in a sodium hydroxide solution at a pressure of at least 100 psig and a temperature of at least 130° C. to produce a sodium silicate solution having a silica to sodium oxide molar ratio of between 2.0:1 and 2.6:1; (b) providing an activated system comprising a sodium silicate solution mixed with agitation for a period of at least about one-half hour with a seed amount of bulk zeolite Y ground to a fine powder at a temperature up to about 0° C.; (c) forming a sodium aluminate solution; (d) adding the sodium aluminate to the activated system over a period of from about five minutes to five hours with stirring to produce a reaction mixture comprising a sodium silicate mother liquor and an amorphous sodium alumino silicate pigment, said mixture having a sodium oxide to silica molar ratio of between 0.5:1 and 1:1, a silica to alumina molar ratio of between 10:1 and 15:1, and a water to sodium oxide molar ratio of between 40:1 and 60:1; (e) allowing the mixture to stand up to about 16 hours at a temperature of about 0° C. to ambient; (f) heating and reacting the mixture at a temperature of about 90° C.-105° C. until crystalline zeolite Y is formed; and (g) recovering the zeolite Y.
Claim 14
Dependent Claim
26 words
The method of claim 11, wherein the seed amount of bulk zeolite Y is about one percent to about ten percent by weight of the mixture.
Claim 15
Dependent Claim
20 words
The method of claim 11, wherein the temperature of step (b) is from about -5° C. to about 0° C.
Claim 16
Dependent Claim
32 words
The method of claim 11, wherein step (d), the mixture has the following molar ratios: sodium oxide to silica--0.6:1 to 0.8:1 silica to alumina--11:1 to 15:1 water to sodium oxide--45:1 to 50:1
Claim 17
Dependent Claim
26 words
The method of claim 11, wherein step (d), the mixture has the following molar ratios; sodium oxide to silica--0.7:1 silica to alumina--12.5:1 water to sodium oxide--47:1
Claim 18
Dependent Claim
21 words
The method of claim 11, wherein in step (e), the period of standing or warming is about six to sixteen hours.
Claim 19
Dependent Claim
14 words
The method of claim 11, wherein in step (e), the temperature is ambient temperature.
Claim 20
Independent Claim
231 words
A method of preparing a crystalline zeolite X, comprising the steps of: (a) dissolving sand in a sodium hydroxide solution at a pressure of at least 100 psig and a temperature of at least 130° C. to produce a sodium silicate solution having a silica to sodium oxide molar ratio of between 2.0:1 and 2.8:1; (b) providing an activated system comprising a sodium silicate solution mixed with agitation for a period of at least about one-half hour with a seed amount of bulk zeolite X ground to a fine powder at a temperature up to about 0° C.; (c) forming a sodium aluminate solution; (d) adding the sodium aluminate to the activated system over a period of time from about seven minutes to about 30 minutes with stirring to produce a reaction mixture comprising a sodium silicate mother liquor and an amorphous sodium alumino silicate pigment, said mixture having a sodium oxide to silica molarratio of between 0.4:1 and 1:1, a silica to alumina molar ratio of between 2.5:1 and 3.5:1, and water to sodium oxide molar ratio of between 20:1 and 50:1; (e) allowing the mixture to stand for up to about 16 hours at a temperature of about 0° C. to ambient; (f) heating and reacting the mixture at a temperature of from about 90° C.-105° C. until crystalline zeolite X is formed; and, (g) recovering the zeolite X.
Claim 21
Independent Claim
231 words
A method of preparing a crystalline zeolite X, comprising the steps of: (a) dissolving sand in a sodium hydroxide solution at a pressure of at least 100 psig and a temperature of at least 130° C. to produce a sodium silicate solution having a silica to sodium oxide molar ratio of between 2.0:1 and 2.8:1; (b) providing an activated system comprising a sodium silicate solution mixed with agitation for a period of at least about one-half hour with a seed amount of bulk zeolite X ground to a fine powder at a temperature up to about 0° C.; (c) forming a sodium aluminate solution; (d) adding the sodium aluminate to the activated system over a period of time from about seven minutes to about 30 minutes with stirring to produce a reaction mixture comprising a sodium silicate mother liquor and an amorphous sodium alumino silicate pigment, said mixture having a sodium oxide to silica molarratio of between 0.4:1 and 1:1, a silica to alumina molar ratio of between 2.5:1 and 3.5:1, and water to sodium oxide molar ratio of between 20:1 and 50:1; (e) allowing the mixture to stand for up to about 16 hours at a temperature of about 0° C. to ambient; (f) heating and reacting the mixture at a temperature of from about 90° C.-105° C. until crystalline zeolite X is formed; and, (g) recovering the zeolite X.
Claim 22
Dependent Claim
26 words
The method of claim 18, wherein the seed amount of bulk zeolite X is about one percent to about ten percent by weight of the mixture.
Claim 23
Dependent Claim
21 words
The method of claim 18 wherein the temperature of step (b) is from about -5° C. up to about 0° C.
Claim 24
Dependent Claim
33 words
The method of claim 18, wherein in step (d), the mixture has the following molar ratios: sodium oxide to silica--0.4:1 to 0.8:1 silica to alumina--2.6:1 to 3.0:1 water to sodium oxide--25:1 to 40:1.
Claim 25
Dependent Claim
27 words
The method of claim 18, wherein in step (d), the mixture has the following molar ratios: sodium oxide to silica--0.6:1 silica to alumina--2.8:1 water to sodium oxide--34:1.
Claim 26
Dependent Claim
21 words
The method of claim 18, wherein in step (e), the period of standing or warming is about six to sixteen hours.
Claim 27
Dependent Claim
14 words
The method of claim 18, wherein in step (e), the temperature is ambient temperature.
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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) | 1986-08-22 | 1987-02-21 | 1987-08-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-08-22 | 1991-02-21 | 1991-08-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-08-22 | 1995-02-21 | 1995-08-23 | $7700.00 | Window Closed / Lapsed |