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US4248847A
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Process for preparing a substantially crystalline sodium aluminosilicate
Assignee: Kali Chemie AG
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Filing: 1978-02-08
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Granted: 1981-02-03
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Expires: 1998-02-08
Abstract
Abstract A process for preparing a synthetic substantially crystalline sodium aluminosilicate of the zeolite A type is disclosed. The process comprises rapidly and simultaneously introducing a sodium silicate and a sodium aluminate solution under thorough agitation at a constant by volume ratio which provides for a reaction mixture the content of which is equivalent to a molar ratio of x' Na 2 O/ 1 Al 2 O 3 / y SiO 2 /z' H 2 O wherein x' is from about 6.5 to about 9.0, y is from about 1.7 to about 2.2 and z' is from about 180 to about 250, maintaining the reaction mixture at a temperature of from about 70° to about 100° C. under stirring for a sufficient period of time, usually 1-3 hours, in order to allow the initially amorphous reaction product to crystallize and recovering the substantially crystalline product from the resulting suspension. The essential feature of the process is a continuously maintained constant molar ratio Na 2 O/ Al 2 O/ SiO 2 /H 2 O throughout the reaction mixture during the entire course of the process. The resulting product exhibits a small particle size, an excellent wettability and a high calcium binding power, and is especially suited as a detergent additive.
Inventors
- 👤 Helmut Derleth
- 👤 Ludwig Walter
- 👤 Karl-Heinrich Bretz
- 👤 Artur Kurs
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 17:37
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2815; C01B33/2823; Y; Y10; Y10S; Y10S423/00; Y10S423/24
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
302 words
A process for preparing a synthetic substantially crystalline sodium aluminosilicate of the molar composition xNa 2 O.Al 2 O 3 .ySiO 2 .zH 2 O, wherein x is a value of from about 0.8 to about 1.2, y is a value from about 1.7 to about 2.2, and z is a value from about 3.0 to about 10.0 which comprises the steps of: (a) thoroughly and rapidly mixing an aqueous sodium silicate solution and an aqueous sodium aluminate solution in such amounts that the content of the mixtue is equivalent to a molar ratio of x'Na 2 O:1Al 2 O 3 :ySiO 2 :z'H 2 O wherein x' is a value of from about 6.5 to about 9.0, y is a value of from about 1.7 to about 2.2, and z' is a value of from about 180 to about 250 within the minimum period of time which is sufficient to obtain a uniform mixture by simultaneously introducing said sodium silicate solution and said sodium aluminate solution at a constant ratio into a reaction zone under sufficiently intensive agitation to maintain a constant molar ratio of Na 2 O/AL 2 O 3 /SiO 2 /H 2 O throughout the reaction mixture whereby a reacton mixture containing an intermediate amorphous sodium aluminosilicate is formed; (b) maintaining the reaction mixture at a temperature of from about 70° to about 100° C. under sufficient agitation in order to continuously ensure the constant molar ratio Na 2 O/Al 2 O 3 /SiO 2 /H 2 O throughout the reaction mixture for a period of time of from about 1 to about 3 hours which is sufficient to transform the reaction mixture into a suspension of a substantially crystalline sodium aluminosilicate precipitate in a mother liquor; and (c) separating said substantially crystalline sodium aluminosilicate from the suspension.
Claim 2
Dependent Claim
302 words
A process for preparing a synthetic substantially crystalline sodium aluminosilicate of the molar composition xNa 2 O.Al 2 O 3 .ySiO 2 .zH 2 O, wherein x is a value of from about 0.8 to about 1.2, y is a value from about 1.7 to about 2.2, and z is a value from about 3.0 to about 10.0 which comprises the steps of: (a) thoroughly and rapidly mixing an aqueous sodium silicate solution and an aqueous sodium aluminate solution in such amounts that the content of the mixtue is equivalent to a molar ratio of x'Na 2 O:1Al 2 O 3 :ySiO 2 :z'H 2 O wherein x' is a value of from about 6.5 to about 9.0, y is a value of from about 1.7 to about 2.2, and z' is a value of from about 180 to about 250 within the minimum period of time which is sufficient to obtain a uniform mixture by simultaneously introducing said sodium silicate solution and said sodium aluminate solution at a constant ratio into a reaction zone under sufficiently intensive agitation to maintain a constant molar ratio of Na 2 O/AL 2 O 3 /SiO 2 /H 2 O throughout the reaction mixture whereby a reacton mixture containing an intermediate amorphous sodium aluminosilicate is formed; (b) maintaining the reaction mixture at a temperature of from about 70° to about 100° C. under sufficient agitation in order to continuously ensure the constant molar ratio Na 2 O/Al 2 O 3 /SiO 2 /H 2 O throughout the reaction mixture for a period of time of from about 1 to about 3 hours which is sufficient to transform the reaction mixture into a suspension of a substantially crystalline sodium aluminosilicate precipitate in a mother liquor; and (c) separating said substantially crystalline sodium aluminosilicate from the suspension.
Claim 3
Dependent Claim
20 words
The process as defined in claim 1 wherein the period of time is from about 1 to about 2 hours.
Claim 4
Dependent Claim
54 words
The process as defined in claim 1 wherein the minimum period of time during which the mixing step (a) is carried out is from about 5 to about 20% of the period of time during which the suspension is maintained at a temperature of from about 70° to about 100° C. in step (b).
Claim 5
Dependent Claim
20 words
The process as defined in claim 3 wherein the minimum period of time is from about 5 to about 10%.
Claim 6
Dependent Claim
35 words
The process as defined in claim 1 which further comprises the steps of heating the sodium silicate solution and the sodium aluminate solution to a temperature of at least 60° C. prior to the mixing.
Claim 7
Dependent Claim
53 words
The process as defined in claim 1 wherein the sodium aluminate solution has a sodium aluminate content which is equivalent to a molar ratio Na 2 O/Al 2 O 3 of from about 5.5 to about 7.0 and a molar ratio H 2 O/Na 2 O of from about 23 to about 35.
Claim 8
Dependent Claim
51 words
The process as defined in claim 1 wherein the sodium silicate solution has a sodium silicate content which is equivalent to a molar ratio Na 2 O/SiO 2 of from about 0.6 to about 0.9 and a molar ratio H 2 O/Na 2 O of from about 10 to about 16.
Claim 9
Dependent Claim
36 words
The process as defined in claim 1 wherein said separating step c further comprises the step of recovering a mother liquor from said suspension and recycling the mother liquor as a solvent for the starting solutions.
Claim 10
Dependent Claim
38 words
The process as defined in claim 1, wherein the reaction mixture after termination of the crystallization is cooled under agitation so rapidly that cooling of the mixture to 50° C. does not exceed 30% of the crystallization period.
Claim 11
Dependent Claim
18 words
The process as defined in claim 1, wherein the temperature is from about 80° to about 95° C.
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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) | 1984-02-03 | 1984-08-04 | 1985-02-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-02-03 | 1988-08-04 | 1989-02-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-02-03 | 1992-08-04 | 1993-02-03 | $7700.00 | Window Closed / Lapsed |