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US4310496A
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Process for converting silicon dioxide containing waste flue dust to crystalline zeolitic molecular sieves of type A
Assignee: Evonik Operations GmbH
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Filing: 1977-11-08
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Granted: 1982-01-12
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Expires: 1997-11-08
Abstract
Abstract Silicon dioxide containing waste flue dust from the production of silicon metal and silicon alloys is converted to crystalline zeolite molecular sieves of type A by (1) dissolving the flue dust in alkali metal hydroxide solution with the formation of alkali metal silicate solution having a module (SiO 2 :Me 2 I O) in the range of 2.0:1 to 3.5:1 at a temperature of 60°-100° C.; (2) purifying the thus obtained alkali metal silicate solution from organic constituents by treatment with activated carbon and/or an oxidizing agent and separating the non-decomposable residue from the solution; and, (3) reacting alkali metal aluminate solution present at room temperature with the diluted, purified alkali metal silicate solution with a module (SiO 2 :Na 2 O) of 2.0:1 to 3.5:1 obtained by steps (1) and (2) and subsequently crystallizing the reaction mixture ((2.0-4.4)Na 2 O:Al 2 O 3 ; (1.3-1.8)SiO 2 :(90-120)H 2 O) at a temperature of 90°-95° C. for a period of 6-12 hours, subsequently filtering, washing to pH of about 10-11 and drying to recover a crystalline, zeolitic molecular sieve of type A having a degree of whiteness according to Berger (A. Berger, Die Farbe 8 Nr. 4/6 (1959) pages 187-202) at 460μ in the range of 90-95%.
Inventors
- 👤 Karl Achenbach
- 👤 Gunter Turk
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 10:09
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/20; C01B33/32; C01B33/325; C01B33/26; C01B33/28; C01B33/2807; C01B33/2815; Y; Y10; Y10S; Y10S423/00; Y10S423/24
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
241 words
A process for the preparation of crystalline zeolite molecular sieves of type A from waste flue dust containing silicon dioxide obtained from the production of silicon metal or ferrosilicon or is a mixture of flue dusts from the production of silicon metal and ferrosilicon comprising (1) dissolving the flue dust in alkali metal hydroxide solution with the formation of alkali metal silicate solution having the mole ratio (SiO 2 :Me 2 I O) in the range of 2.0:1 to 3.5:1 at a temperature of 60°-110° C.; (2) purifying the thus obtained alkali metal silicate solution from organic constituents by treatment with both activated carbon and sodium peroxide and separating the non-decomposable residue from the solution; and (3) reacting alkali metal aluminate solution present at room temperature with the purified alkali metal silicate solution with the mole ratio (SiO 2 :Me 2 I O) of 2.0:1 to 3.5:1 obtained by steps (1) and (2) and subsequently crystallizing the reaction mixture ((2.0-4.4)Me 2 O:Al 2 O 3 :(1.3-1.8)SiO 2 :(90-120)H 2 O) at a temperature of 90°-96° C. for a period of 6- 12 hours, subsequently filtering to remove the product from the mother liquor, washing the product to pH of about 10-11 and drying to recover a crystalline, zeolite molecular sieve of type A having a degree of whiteners according to BERGER at 460μ in the range of 90-95%, the alkali metal of the hyroxide, silicate, and aluminate being sodium or potassium.
Claim 2
Dependent Claim
241 words
A process for the preparation of crystalline zeolite molecular sieves of type A from waste flue dust containing silicon dioxide obtained from the production of silicon metal or ferrosilicon or is a mixture of flue dusts from the production of silicon metal and ferrosilicon comprising (1) dissolving the flue dust in alkali metal hydroxide solution with the formation of alkali metal silicate solution having the mole ratio (SiO 2 :Me 2 I O) in the range of 2.0:1 to 3.5:1 at a temperature of 60°-110° C.; (2) purifying the thus obtained alkali metal silicate solution from organic constituents by treatment with both activated carbon and sodium peroxide and separating the non-decomposable residue from the solution; and (3) reacting alkali metal aluminate solution present at room temperature with the purified alkali metal silicate solution with the mole ratio (SiO 2 :Me 2 I O) of 2.0:1 to 3.5:1 obtained by steps (1) and (2) and subsequently crystallizing the reaction mixture ((2.0-4.4)Me 2 O:Al 2 O 3 :(1.3-1.8)SiO 2 :(90-120)H 2 O) at a temperature of 90°-96° C. for a period of 6- 12 hours, subsequently filtering to remove the product from the mother liquor, washing the product to pH of about 10-11 and drying to recover a crystalline, zeolite molecular sieve of type A having a degree of whiteners according to BERGER at 460μ in the range of 90-95%, the alkali metal of the hyroxide, silicate, and aluminate being sodium or potassium.
Claim 3
Dependent Claim
17 words
The process of claim 1 wherein the alkali metal of the hydroxide, silicate and aluminate is sodium.
Claim 4
Dependent Claim
16 words
The process of claim 2 comprising carrying out the crystallization at a temperature of 90°-95° C.
Claim 5
Dependent Claim
70 words
The process of claim 1 comprising mixing the mother liquor, said mother liquor containing alkali metal silicate and alkali metal hydroxide, of step (3) with more concentrated alkali metal hydroxide solution and returning the thus produced alkali metal hydroxide and alkali metal silicate solution to step (1) in order to produce an alkali metal silicate solution having the mole ratio SiO 2 :Me 2 I O of 2:1 to 3.5:1.
Claim 6
Dependent Claim
11 words
The process of claim 4 wherein the alkali metal is sodium.
Claim 7
Dependent Claim
17 words
The process of claim 5 wherein the more concentrated alkali metal hydroxide is 45-50% aqueous sodium hydroxide.
Claim 8
Dependent Claim
49 words
The process of claim 1 comprising dissolving solid alkali metal silicate with the mole ratio SiO 2 :Me 2 I O=3.3:1 in the mother liquor containing alkali metal hydroxide until the solution has a mole ratio of 2:1 and then returning the resulting thus formed solution to step (1).
Claim 9
Dependent Claim
11 words
The process of claim 7 wherein the alkali metal is sodium.
Claim 10
Dependent Claim
49 words
The process of claim 1 wherein the activated carbon is one prepared from pure wood charcoal and has a water content of 10%, a BET surface area in the range of 600-800 m 2 /g, a pH of 9-10 and a degree of fineness of 80% below 40 microns.
Claim 11
Dependent Claim
35 words
The process of claim 1 wherein the treatment with activated carbon and sodium peroxide is conducted at a point in time from shortly before the separation to a point in time shortly after said separation.
Claim 12
Dependent Claim
30 words
The process of claim 1 wherein the treatment with activated carbon and sodium peroxide is conducted shortly before the separation of the non-decomposable residue from the alkali metal silicate solution.
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) | 1985-01-11 | 1985-07-13 | 1986-01-12 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-01-11 | 1989-07-13 | 1990-01-12 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-01-11 | 1993-07-13 | 1994-01-12 | $7700.00 | Window Closed / Lapsed |