US4271135A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Preparation of finely-divided, water-insoluble silicate cation-exchangers with a narrow particle size spectra
Assignee: Henkel AG and Co KGaA
•
Filing: 1979-10-04
•
Granted: 1981-06-02
•
Expires: 1999-10-04
Abstract
Abstract A method for the preparation of finely-divided, water-insoluble, aluminosilicate cation-exchangers with a narrow particle size spectra suitable for detergent formulations comprising: (1) agitating a water-dissolved alkali metal silicate at a temperature of from 55° C. to 95° C. (2) mixing therewith at a temperature of from 55° C. to 95° C. over a period of from three seconds to five minutes with vigorous agitation, a water-dissolved alkali metal aluminate, in the presence of an excess of alkali to give a suspension of a silicate compound containing bound water and having a calcium binding power, when measured at 22° C. by the Calcium Binding Power Test Method, of at least 50 mg CaO/gm of anhydrous active substance, and having the formula, bound water not shown, (M.sub.2 O).sub.0.8-1.3.Al.sub.2 O.sub.3.(SiO.sub.2).sub.1.75-2.0 wherein M represents an alkali metal, wherein said reactant solutions when mixed have a composition corresponding to the desired Al 2 O 3 and SiO 2 amounts of the above formula, with a ratio of from 3.2 to 4.4 mols M 2 O/mol Al 2 O 3 and a ratio of from 70 to 85 mols of water/mol Al 2 O 3 , (3) maintaining said silicate compound suspension after said mixing step is completed, for a period of from two to twenty minutes under the agitation and temperature conditions of said mixing step, (4) rapidly heating said silicate compound suspension at least 5° C. above the temperature of said mixing step to a temperature of from 60° C. to 100° C., (5) allowing said silicate compound suspension to crystallize at said elevated temperature of from 60° C. to 100° C. while agitating sufficiently to keep said suspension flowable, (6) adjusting said crystalline silicate compound suspension to a pH of below 12.5, and (7) recovering said crystalline silicate compound.
Inventors
- 👤 Willi Wuest
- 👤 Guenther Just
- 👤 Bernd W. Peters
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 12:17
CPC Classifications
C; C01; C01B; C01B39/00; C01B39/02; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2815; C01B33/2823; C11; C11D; C11D3/00; C11D3/02; C11D3/12; C11D3/124; C11D3/1246; C11D3/128; Y; Y10; Y10S; Y10S423/00; Y10S423/24
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
326 words
A method for the preparation of finely-divided, water-insoluble, aluminosilicate cation-exchangers with a narrow particle size spectra suitable for detergent formulations having a grain size distribution with 96% less than 10μ and a mazimum size range of from 3 to 5μ comprising: (1) agitating a water-dissolved alkali metal silicate at a temperature of from 60° C. to 85° C., (2) mixing therewith at a temperature of from 60° C. to 85° C. over a period of from three seconds to five minutes with vigorous agitation, a water-dissolved alkali metal aluminate, in the presence of an excess of alkali to give a suspension of a silicate compound containing bound water, and having the formula, bound water not shown, (M.sub.2 O).sub.0.8-1.3.Al.sub.2 O.sub.2.(SiO.sub.2).sub.1.75-2.0 wherein M represents an alkali metal, wherein said reactant solutions when mixed have a composition corresponding to the desired AL 2 O 3 and SiO 2 amounts of the above formula, with a ratio of from 3.5 to 4 mols M 2 O/mol Al 2 O 3 and a ratio of from 75 to 80 mols of water/mol Al 2 O 3 , (3) maintaining said silicate compound suspension after said mixing step is completed, for a period of from two to twenty minutes under the agitation and temperature conditions of said mixing step, (4) rapidly heating said silicate compound suspension at least 5° C. above the temperature of said mixing step to a temperature of from 65° C. to 100° C., (5) allowing said silicate compound suspension to crystallize at said elevated temperature of from 65° C. to 100° C. while agitating sufficiently to keep said suspension flowable for a time sufficient to obtain the desired calcium binding power of from 100 to 200 mg CaO/gm of active substance when measured at 22° C. by the Calcium Binding Power Test Method, but less than two hours, (6) adjusting said crystalline silicate compound suspension to a pH of below 12.5 and (7) recovering said crystalline silicate compound.
Claim 2
Independent Claim
326 words
A method for the preparation of finely-divided, water-insoluble, aluminosilicate cation-exchangers with a narrow particle size spectra suitable for detergent formulations having a grain size distribution with 96% less than 10μ and a mazimum size range of from 3 to 5μ comprising: (1) agitating a water-dissolved alkali metal silicate at a temperature of from 60° C. to 85° C., (2) mixing therewith at a temperature of from 60° C. to 85° C. over a period of from three seconds to five minutes with vigorous agitation, a water-dissolved alkali metal aluminate, in the presence of an excess of alkali to give a suspension of a silicate compound containing bound water, and having the formula, bound water not shown, (M.sub.2 O).sub.0.8-1.3.Al.sub.2 O.sub.2.(SiO.sub.2).sub.1.75-2.0 wherein M represents an alkali metal, wherein said reactant solutions when mixed have a composition corresponding to the desired AL 2 O 3 and SiO 2 amounts of the above formula, with a ratio of from 3.5 to 4 mols M 2 O/mol Al 2 O 3 and a ratio of from 75 to 80 mols of water/mol Al 2 O 3 , (3) maintaining said silicate compound suspension after said mixing step is completed, for a period of from two to twenty minutes under the agitation and temperature conditions of said mixing step, (4) rapidly heating said silicate compound suspension at least 5° C. above the temperature of said mixing step to a temperature of from 65° C. to 100° C., (5) allowing said silicate compound suspension to crystallize at said elevated temperature of from 65° C. to 100° C. while agitating sufficiently to keep said suspension flowable for a time sufficient to obtain the desired calcium binding power of from 100 to 200 mg CaO/gm of active substance when measured at 22° C. by the Calcium Binding Power Test Method, but less than two hours, (6) adjusting said crystalline silicate compound suspension to a pH of below 12.5 and (7) recovering said crystalline silicate compound.
Claim 3
Dependent Claim
22 words
The process of claim 1 wherein said agitating and mixing steps are conducted at a temperature between 60° C. and 70° C.
Claim 4
Dependent Claim
9 words
The process of claim 1 wherein M is sodium:
Claim 5
Dependent Claim
20 words
The process of claim 1 wherein said maintaining step (3) is for a period of from 5 to 10 minutes.
Claim 6
Dependent Claim
17 words
The process of claim 1 wherein said rapidly heating step is for a period of 5 minutes.
Claim 7
Dependent Claim
22 words
The process of claim 1 wherein said crystallization step (5) is conducted at a temperature of from 90° C. to 95° C.
Claim 8
Dependent Claim
29 words
The process of claim 1 wherein said crystallization step (5) is conducted at a temperature initially at from 90° C. where during crystallization the temperature is allowed to drop.
Claim 9
Dependent Claim
16 words
The process of claim 1 wherein said crystalline silicate compound is recovered as an aqueous suspension.
Claim 10
Dependent Claim
17 words
The process of claim 1 wherein said crystalline silicate compound is recovered as a finely-divided pulverulent material.
Claim 11
Dependent Claim
36 words
The process of claim 1 wherein said step (6) of adjusting the pH to below 12.5 is conducted by separating at least some of the mother liquor from said crystalline silicate suspension and replacing by water.
Claim 12
Dependent Claim
26 words
The process of claim 10 wherein said mother liquor is utilized in the preparation of said water-dissolved alkali metal silicate and/or said water-dissolved alkali metal aluminate.
Claim 13
Dependent Claim
58 words
The process of claim 1 wherein said step (6) of adjusting the pH to below 12.5 is conducted by replacing the mother liquor from said crystalline silicate suspension with water until the pH is between 11.5 and 13.5 and thereafter adjusting the pH of the crystalline silicate suspension to from 7 to 11.4 by adding an acid thereto.
Claim 14
Dependent Claim
19 words
The process of claim 12 wherein sufficient acid is added to bring the pH to from 8 to 11.
Claim 15
Dependent Claim
13 words
The process of claim 13 wherein said acid is a strong mineral acid.
Claim 16
Dependent Claim
23 words
The process of claim 13 wherein said acid is an anionic surface-active compound of the sulfate or sulfonate type in the acid form.
Claim 17
Dependent Claim
22 words
The process of claim 1 wherein the total weight of the reactants of said mixing step (3) is at least 1173 kg.
Claim 18
Dependent Claim
24 words
The process of claim 1 wherein the total time required for steps (2), (3), (4) and (5) is from 301/2 minutes to 701/2 minutes.
Claim 19
Dependent Claim
20 words
The process of claim 1, step (5), wherein said suspension is allowed to crystallize for from 5 to 65 minutes.
References Cited (Backward Citations)
US2882243A
Cited
US3058805A
Cited
US4071377A
Cited
US3985669A
Cited
US4041135A
Cited
US4102977A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-06-01 | 1984-12-01 | 1985-06-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-06-01 | 1988-12-01 | 1989-06-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-06-01 | 1992-12-01 | 1993-06-02 | $7700.00 | Window Closed / Lapsed |