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US4416805A
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Synthesis of zeolites of small and uniform size having a high magnesium exchange capacity
Assignee: JM Huber Corp
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Filing: 1980-11-04
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Granted: 1983-11-22
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Expires: 2000-11-04
Abstract
Abstract Zeolites of small and uniform size are formed having high magnesium exchange capacities. Zeolite A is disclosed having an average particle size less than 1.7 microns, a calcium carbonate exchange capacity of more than 230 mg calcium carbonate per gram zeolite and a magnesium exchange capacity of more than 140 mg magnesium carbonate per gram zeolite. This zeolite A is produced from a reaction mixture having a water to sodium oxide molar ratio of less than 35:1, and a sodium oxide to silica molar ratio of between 1:1 and 4:1, wherein the silica to alumina molar ratio is greater than 3:1 when the sodium oxide to silica molar ratio is less than 4:3 and the sodium oxide to alumina molar ratio is greater than 4:1 when the sodium oxide to silica molar ratio is greater than 4:3. Zeolite X is disclosed having an average particle size less than 2.2 microns, a calcium carbonate exchange capacity of more than 205 mg calcium carbonate per gram zeolite, and a magnesium exchange capacity of more than 130 mg magnesium carbonate per gram zeolite. This zeolite X is produced from a reaction mixture having a silicate alumina molar ratio greater than 5:1. A combination of zerolite A and zeolite X can be produced from the same reaction mixture.
Inventors
- 👤 John A. Kostinko
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 22:02
CPC Classifications
D; D21; D21H; D21H19/00; D21H19/36; D21H19/38; D21H19/40; A; A01; A01K; A01K1/00; A01K1/015; C; C01; C01B; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2815; C01B33/2823; C09; C09D; C09D7/00; C09D7/40; C09D7/42; C11; C11D; C11D3/00; C11D3/02; C11D3/12; C11D3/124; C11D3/1246; C11D3/128; D21H17/00; D21H17/63; D21H17/67; D21H17/68; Y; Y10; Y10S; Y10S423/00; Y10S423/21; Y10S423/24
Claims Analysis
Total Claims: 9
Claim 1
Independent Claim
202 words
A method of producing a combination of zeolite A and zeolite X comprising the steps of: (a) dissolving sand in a sodium hydroxide solution at a pressure of at least 100 psig heated to a temperature of at least 130 degrees Celsius to produce a sodium silicate solution having a silica to sodium oxide molar ratio of between 2.4:1 and 2.8:1 to form a sodium silicate solution; (b) activating said sodium silicate solution by treating with from 50 to 2000 ppm alumina; (c) forming a sodium aluminate solution; (d) heating said sodium silicate and sodium aluminate solution to between 40 and 120 degrees Celsius; (e) adding together said sodium aluminate solution and said sodium silicate solution to produce a reaction mixture comprising a sodium silicate mother liquor and an amorphous sodium alumina silicate, in total having a water to sodium oxide molar ratio of between 10:1 and 60:1; a sodium oxide to silica molar ratio of between 0.5:1 and 3:1; and a silica to alumina molar ratio of between 2:1 and 15:1; (f) heating said mixture; (g) reacting said mixture until a combination of zeolite A and zeolite X is formed; and (h) recovering said combination of zeolite A and zeolite X.
Claim 2
Independent Claim
202 words
A method of producing a combination of zeolite A and zeolite X comprising the steps of: (a) dissolving sand in a sodium hydroxide solution at a pressure of at least 100 psig heated to a temperature of at least 130 degrees Celsius to produce a sodium silicate solution having a silica to sodium oxide molar ratio of between 2.4:1 and 2.8:1 to form a sodium silicate solution; (b) activating said sodium silicate solution by treating with from 50 to 2000 ppm alumina; (c) forming a sodium aluminate solution; (d) heating said sodium silicate and sodium aluminate solution to between 40 and 120 degrees Celsius; (e) adding together said sodium aluminate solution and said sodium silicate solution to produce a reaction mixture comprising a sodium silicate mother liquor and an amorphous sodium alumina silicate, in total having a water to sodium oxide molar ratio of between 10:1 and 60:1; a sodium oxide to silica molar ratio of between 0.5:1 and 3:1; and a silica to alumina molar ratio of between 2:1 and 15:1; (f) heating said mixture; (g) reacting said mixture until a combination of zeolite A and zeolite X is formed; and (h) recovering said combination of zeolite A and zeolite X.
Claim 3
Dependent Claim
40 words
A method of producing a combination of zeolite A and zeolite X according to claim 1 wherein the amount of alumina used to activate said sodium silicate is from 400 to 600 ppm and said activation occurs at room temperature.
Claim 4
Dependent Claim
56 words
A method of producing a combination of zeolite A and zeolite X according to claim 1 wherein the mixture has a water to sodium oxide molar ratio of between 10:1 and 60:1; a sodium oxide to silica molar ratio of between 0.5:1 and 2.5:1; and a silica to alumina molar ratio of between 5:1 and 15:1.
Claim 5
Dependent Claim
56 words
A method of producing a combination of zeolite A and zeolite X according to claim 1 wherein the mixture has a water to sodium oxide molar ratio of between 15:1 and 60:1; a sodium oxide to silica molar ratio of between 0.7:1 and 1.7:1; and a silica to alumina molar ratio of between 5:1 and 10:1.
Claim 6
Independent Claim
221 words
A method of producing a combination of zeolite A and zeolite X, said method comprising the steps of: (a) dissolving sand in a sodium hydroxide solution at a pressure of about 140 psig heated to a temperature of at least 130 degrees Celsius to produce sodium silicate having a silica to sodium oxide molar ratio of about 2.4:1; (b) activating said sodium silicate with about 600 ppm alumina at room temperature for at least 10 minutes; (c) heating said sodium silicate solution to a temperature of about 90 degrees Celsius; (d) forming a sodium aluminate solution; (e) heating said sodium aluminate solution to a temperature of about 90 degrees Celsius; (f) adding said sodium aluminate solution to said activated sodium silicate so that all of the sodium aluminate solution is added within a period of time less than 30 seconds to form a mixture having a water to sodium oxide molar ratio of about 15.8:1; a sodium oxide to silica molar ratio of about 0.7:1; and a silica to alumina molar ratio of about 9.8:1. (g) heating said mixture to a temperature of about 90 degrees Celsius; (h) reacting said mixture at a temperature of about 100 degrees Celsius until said combination of zeolite A and zeolite X is formed; and (i) recovering said combination of zeolite A and zeolite X.
Claim 7
Independent Claim
221 words
A method of producing a combination of zeolite A and zeolite X, said method comprising the steps of: (a) dissolving sand in a sodium hydroxide solution at a pressure of about 140 psig heated to a temperature of at least 130 degrees Celsius to produce sodium silicate having a silica to sodium oxide molar ratio of about 2.4:1; (b) activating said sodium silicate with about 600 ppm alumina at room temperature for at least 10 minutes; (c) heating said sodium silicate solution to a temperature of about 90 degrees Celsius; (d) forming a sodium aluminate solution; (e) heating said sodium aluminate solution to a temperature of about 90 degrees Celsius; (f) adding said sodium aluminate solution to said activated sodium silicate so that all of the sodium aluminate solution is added within a period of time less than 30 seconds to form a mixture having a water to sodium oxide molar ratio of about 15.8:1; a sodium oxide to silica molar ratio of about 0.7:1; and a silica to alumina molar ratio of about 9.8:1. (g) heating said mixture to a temperature of about 90 degrees Celsius; (h) reacting said mixture at a temperature of about 100 degrees Celsius until said combination of zeolite A and zeolite X is formed; and (i) recovering said combination of zeolite A and zeolite X.
Claim 8
Dependent Claim
91 words
In a method for producing a sodium aluminosilicate zeolite by the reaction of a sodium silicate and a sodium aluminate, the improvement wherein said sodium silicate solution is formed by dissolving sand in a sodium hydroxide solution at a pressure of at least 100 psig heated to a temperature of at least 130 degrees Celsius to produce a sodium silicate solution having a silica to sodium oxide molar ratio of between 2.4:1 and 2.8:1, and activating said sodium silicate solution by reaction with from about 50 to 2000 ppm of alumina.
Claim 9
Dependent Claim
91 words
In a method for producing a sodium aluminosilicate zeolite by the reaction of a sodium silicate and a sodium aluminate, the improvement wherein said sodium silicate solution is formed by dissolving sand in a sodium hydroxide solution at a pressure of at least 100 psig heated to a temperature of at least 130 degrees Celsius to produce a sodium silicate solution having a silica to sodium oxide molar ratio of between 2.4:1 and 2.8:1, and activating said sodium silicate solution by reaction with from about 50 to 2000 ppm of alumina.
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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) | 1986-11-21 | 1987-05-23 | 1987-11-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-11-21 | 1991-05-23 | 1991-11-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-11-21 | 1995-05-23 | 1995-11-22 | $7700.00 | Window Closed / Lapsed |