US4007124A
Expired / Lapsed
US
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Process for preparing a silicate-pyrophosphate detergent composition
Assignee: Procter and Gamble Co
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Filing: 1975-06-30
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Granted: 1977-02-08
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Expires: 1995-06-30
Abstract
Abstract An acidified detergent composition is prepared by acidifying aqueous alkali metal silicate to form a premix; mixing that premix with an aqueous slurry containing surfactant and at least one structurant, i.e. structure-forming compound; drying; and optionally adding admixed adjuvant. Alkali metal pyrophosphate must be included in the composition, either as structurant or admixed adjuvant or both.
Inventors
- 👤 Everett Joshua Collier
- 👤 John Edward Morrow
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 18:18
CPC Classifications
C; C11; C11D; C11D3/00; C11D3/02; C11D3/04; C11D3/06; C11D11/00; C11D11/0082; C11D3/08
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
362 words
A process for preparing a detergent composition comprising: a. acidifying an aqueous alkali metal silicate with acid, during agitation, thereby forming a silicate premix; wherein the alkali metal silicate has the formula ρ M 2 O.SiO 2 , where M is alkali metal and ρ, the ratio of (mols M 2 O) to (mols SiO 2 ), is from about 0.25 to about 0.50; and wherein the amount of acid, expressed as a ratio of (equivalents of acid) to (mols SiO 2 in the silicate), is between about 0.0005 and about 0.4; b. mixing said silicate premix with an aqueous slurry comprised of surfactant, water, and at least one structurant, i.e. structure-forming compound, thereby forming a crutcher mix; wherein the surfactant is anionic, nonionic, semi-polar, zwitterionic, ampholytic, or mixtures thereof; and wherein the structurant is selected from the group consisting of calcium carbonate; natural and synthetic clays; nitrilotriacetates; aluminosilicates; and alkali metal pyrophosphates, triphosphates, glassy phosphates, carbonates, bicarbonates, sesquicarbonates, chlorides, borates, perborates, sulfates, bisulfates, aluminates, and mixtures thereof; c. drying said crutcher mix to a moisture of from about 0.5% to about 15% by weight of the dried crutcher mix; and d. adding admixed adjuvant to said dried crutcher mix, thereby forming said detergent composition; wherein the admixed adjuvant is selected from the group consisting of calcium carbonate; sodium aluminosilicates; alkali metal pyrophosphates, carbonates, borates, bicarbonates and sulfates; water-soluble aminopolycarboxylates; water-soluble salts of phytic acid; water-soluble polyphosphonates; and water-soluble salts of mellitic acid, citric acid, pyromellitic acid, benzene pentacarboxylic acid, oxydiacetic acid, carboxymethyloxysuccinic acid, and oxydisuccinic acid; wherein percentages of the components by weight, expressed in relation to the final detergent composition, are: SiO 2 in the silicate from about 1.5% to about 16%; surfactant from about 4% to about 50%; structurant from about 4% to about 90%; and admixed adjuvant from 0 to about 80%; and wherein alkali metal pyrophosphate, M x H y P 2 O 7 , where M is alkali metal and x and y are integers having the sum of 4, is present in the composition in an amount from about 5% to about 60%, said pyrophosphate being present as either structurant or admixed adjuvant or both.
Claim 2
Dependent Claim
362 words
A process for preparing a detergent composition comprising: a. acidifying an aqueous alkali metal silicate with acid, during agitation, thereby forming a silicate premix; wherein the alkali metal silicate has the formula ρ M 2 O.SiO 2 , where M is alkali metal and ρ, the ratio of (mols M 2 O) to (mols SiO 2 ), is from about 0.25 to about 0.50; and wherein the amount of acid, expressed as a ratio of (equivalents of acid) to (mols SiO 2 in the silicate), is between about 0.0005 and about 0.4; b. mixing said silicate premix with an aqueous slurry comprised of surfactant, water, and at least one structurant, i.e. structure-forming compound, thereby forming a crutcher mix; wherein the surfactant is anionic, nonionic, semi-polar, zwitterionic, ampholytic, or mixtures thereof; and wherein the structurant is selected from the group consisting of calcium carbonate; natural and synthetic clays; nitrilotriacetates; aluminosilicates; and alkali metal pyrophosphates, triphosphates, glassy phosphates, carbonates, bicarbonates, sesquicarbonates, chlorides, borates, perborates, sulfates, bisulfates, aluminates, and mixtures thereof; c. drying said crutcher mix to a moisture of from about 0.5% to about 15% by weight of the dried crutcher mix; and d. adding admixed adjuvant to said dried crutcher mix, thereby forming said detergent composition; wherein the admixed adjuvant is selected from the group consisting of calcium carbonate; sodium aluminosilicates; alkali metal pyrophosphates, carbonates, borates, bicarbonates and sulfates; water-soluble aminopolycarboxylates; water-soluble salts of phytic acid; water-soluble polyphosphonates; and water-soluble salts of mellitic acid, citric acid, pyromellitic acid, benzene pentacarboxylic acid, oxydiacetic acid, carboxymethyloxysuccinic acid, and oxydisuccinic acid; wherein percentages of the components by weight, expressed in relation to the final detergent composition, are: SiO 2 in the silicate from about 1.5% to about 16%; surfactant from about 4% to about 50%; structurant from about 4% to about 90%; and admixed adjuvant from 0 to about 80%; and wherein alkali metal pyrophosphate, M x H y P 2 O 7 , where M is alkali metal and x and y are integers having the sum of 4, is present in the composition in an amount from about 5% to about 60%, said pyrophosphate being present as either structurant or admixed adjuvant or both.
Claim 3
Dependent Claim
36 words
The process of claim 1 wherein the silicate premix is subjected to an agitation period of from about 1 minute to about 120 minutes after acid addition is complete, prior to mixing with the aqueous slurry.
Claim 4
Dependent Claim
27 words
The process of claim 2 wherein the crutcher mix is dried to a moisture from about 1% to about 10% by weight of the dried crutcher mix.
Claim 5
Dependent Claim
11 words
The process of claim 2 wherein the drying process is spray-drying.
Claim 6
Dependent Claim
16 words
The process of claim 4 wherein the spray-drying is carried out in a multilevel tower process.
Claim 7
Dependent Claim
30 words
The process of claim 2 wherein the crutcher mix is dried to a moisture from 2% to 5% by weight of the dried crutcher mix by the process of spray-drying.
Claim 8
Dependent Claim
34 words
The process of claim 1 wherein the surfactant is selected from the group consisting of alkali metal and ammonium salts of fatty acid, alkyl benzene sulfonate, alkyl sulfate, alkyl ether sulfate, and mixtures thereof.
Claim 9
Dependent Claim
21 words
The process of claim 1 wherein the alkali metal silicate is sodium silicate and the alkali metal pyrophosphate is sodium pyrophosphate.
Claim 10
Dependent Claim
17 words
The process of claim 1 wherein the acid is a surfactant-acid, acid pyrophosphate, or a mineral acid.
Claim 11
Dependent Claim
84 words
The process of claim 2 wherein the crutcher mix is dried to a moisture from about 1% to about 10% by weight of the dried crutcher mix; and wherein percentages of the components by weight, expressed in relation to the final detergent composition, are: SiO 2 in the silicate from about 2% to about 13%; surfactant from about 8% to about 40%; structurant from about 40 to about 85%; pyrophosphate from about 10% to about 50%; and admixed adjuvant from 0 to about 50%.
Claim 12
Dependent Claim
49 words
The process of claim 2 wherein ρ, the ratio of (mols M 2 O) to (mols SiO 2 ), is between about 0.26 and about 0.42; and wherein the ratio of (equivalents of acid) to (mols SiO 2 ) in the silicate is between about 0.001 and about 0.1.
Claim 13
Dependent Claim
172 words
The process of claim 10 wherein the surfactant is selected from the group consisting of sodium salts of fatty acid, alkyl benzene sulfonate, alkyl sulfate, alkyl ether sulfate, and mixtures thereof; wherein the alkali metal silicate is sodium silicate and the alkali metal pyrophosphate is sodium pyrophosphate; wherein ρ, the ratio of (mols Na 2 O) to (mols SiO 2 ), is between 0.27 and 0.33, the ratio of (equivalents if acid) to (mols SiO 2 ) in the silicate is between 0.002 and 0.02, and the agitation period of the silicate premix is from 5 to 30 minutes; wherein the crutcher mix is dried to a moisture from 2% to 5% by weight of the dried crutcher mix by the process of spray-drying; and wherein percentages of the components by weight, expressed in relation to the final detergent composition, are SiO 2 in the silicate from 2.5% to 10%; surfactant from 12% to 30%; structurant from 60% to 80%; pyrophosphate from 15% to 40%; and admixed adjuvant from 0 to 20%.
Claim 14
Dependent Claim
87 words
The process of claim 1 containing as structurant or admixed adjuvant from about 1% to about 40% on a detergent composition basis of an amorphous water-insoluble hydrated compound of the formula Na x (xAlO 2 .ySiO 2 ), wherein x is a number from 1 to 1.2 and y is 1, said amorphous compound being further characterized by a Mg + + exchange capacity of from about 50 milligrams equivalent of CaCO 3 hardness/gram to about 150 milligrams equivalent of CaCO 3 hardness/gram on an anhydrous basis.
Claim 15
Dependent Claim
130 words
The process of claim 1 containing as structurant or admixed adjuvant from about 1% to about 40% on a detergent composition basis of a water-insoluble crystalline synthetic aluminosilicate ion exchange material of the formula Na z xH 2 O, wherein z and y are integers of at least 6; the molar ratio of z to y is in the range from 1.0 to about 0.5, and x is an integer from about 15 to about 264; said aluminosilicate ion exchange material having a particle size diameter from about 0.1 micron to about 100 microns; a calcium ion exchange capacity on an anhydrous basis of at least about 200 milligrams equivalent of CaCO 3 hardness/gram; and a calcium ion exchange rate on an anhydrous basis of at least about 2 grains/gallon/minute/gram.
Claim 16
Dependent Claim
53 words
The process of claim 1 additionally containing from about 0.1% to about 4% by weight of a glassy phosphate of the formula (M.sub.2 O).sub.x (P.sub.2 O.sub.5).sub.y wherein y is from about 5 to about 50 and the ratio of y:x is from about 1:1 to about 1:15 and M is an alkali metal.
Claim 17
Dependent Claim
53 words
The process of claim 12 additionally containing from about 0.1% to about 4% by weight of a glassy phosphate of the formula (M.sub.2 O).sub.x (P.sub.2 O.sub.5).sub.y wherein y is from about 5 to about 50 and the ratio of y:x is from about 1:1 to about 1:15 and M is an alkali metal.
Claim 18
Dependent Claim
15 words
The process of claim 16 wherein the glassy phosphate has 14 or 21 phosphorus atoms.
Claim 19
Dependent Claim
53 words
The process of claim 13 additionally containing from about 0.1% to about 4% by weight of a glassy phosphate of the formula (M.sub.2 O).sub.x (P.sub.2 O.sub.5).sub.y wherein y is from about 5 to about 50 and the ratio of y:x is from about 1:1 to about 1:15 and M is an alkali metal.
Claim 20
Dependent Claim
53 words
The process of claim 14 additionally containing from about 0.1% to about 4% by weight of a glassy phosphate of the formula (M.sub.2 O).sub.x (P.sub.2 O.sub.5).sub.y wherein y is from about 5 to about 50 and the ratio of y:x is from about 1:1 to about 1:15 and M is an alkali metal.
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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) | 1980-02-08 | 1980-08-09 | 1981-02-08 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-02-08 | 1984-08-09 | 1985-02-08 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-02-08 | 1988-08-09 | 1989-02-08 | $7700.00 | Window Closed / Lapsed |