Patent US4311607A successfully refreshed from Google Patents.
US4311607A
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Method for manufacture of non-gelling, stable zeolite - inorganic salt crutcher slurries
Assignee: Colgate Palmolive Co
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Filing: 1980-10-21
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Granted: 1982-01-19
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Expires: 2000-10-21
Abstract
Abstract Gelation and setting of desirably miscible and pumpable aqueous crutcher slurries comprising zeolite (hydrated sodium aluminosilicate), sodium bicarbonate, sodium silicate and sodium carbonate are retarded and often are prevented by the addition of sodium sesquicarbonate (which also serves as a source of sodium carbonate and sodium bicarbonate) after admixing of the zeolite, sodium bicarbonate, sodium carbonate (if added earlier) and sodium silicate. Desirably, citric acid (and preferbly also, magnesium sulfate) is(are) dissolved in the crutcher medium before addition of the sodium sesquicarbonate but the presence(s) thereof is(are) not necessary. The method of the invention appreciably increases workable crutcher time, stabilizing the mix against gelation, compared to prior methods for the manufacture of similar crutcher mixes of similar contents of water, zeolite, bicarbonate, carbonate and silicate (considering the sesquicarbonate of the present method as a source of carbonate and bicarbonate), whether all the carbonate and bicarbonate are separately added to the crutcher before the silicate or are added partially before and partially after silicate addition. The improved workability and stability of the crutcher mix permit the making of higher solids content crutcher slurries, thereby resulting in significant energy savings and increases in production rates when such slurries are subsequently spray dried to produce free flowing zeolite - inorganic salt base beads, from which beads built or heavy duty detergent compositions may be made by post-spraying onto them a nonionic synthetic organic detergent in liquid state.
Inventors
- 👤 James A. Kaeser
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 13:59
CPC Classifications
C; C11; C11D; C11D3/00; C11D3/02; C11D3/12; C11D3/124; C11D3/1246; C11D3/128; C11D3/1286; C11D3/04; C11D3/10; C11D3/16; C11D3/20; C11D3/2075; C11D3/2086
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
182 words
A method of retarding or preventing the gelation of a crutcher slurry containing from about 40 to 70% of solids and 60 to 30% of water, of which solids content, on a 100% solids basis, about 20 to 60% is zeolite, about 11 to 45% is sodium bicarbonate, about 4 to 20% is sodium carbonate and about 5 to 20% is sodium silicate of Na 2 O:SiO 2 ratio within the range of 1:1.4 to 1:3, with the ratio of sodium bicarbonate:sodium carbonate being within the range of about 1.2:1 to 8:1, the ratio of sodium carbonate:sodium silicate being within the range of about 1:3 to 3:1, the ratio of sodium bicarbonate:sodium silicate being within the range of about 1.5:1 to 5:1 and the ratio of zeolite to the sum of sodium bicarbonate, sodium carbonate and sodium silicate being within the range of about 1:4 to 4:1, which comprises preparing a crutcher slurry of the described composition by admixing with other components of such slurry an amount of sodium sesquicarbonate which will supply from about 20 to 100% of the sodium carbonate.
Claim 2
Independent Claim
182 words
A method of retarding or preventing the gelation of a crutcher slurry containing from about 40 to 70% of solids and 60 to 30% of water, of which solids content, on a 100% solids basis, about 20 to 60% is zeolite, about 11 to 45% is sodium bicarbonate, about 4 to 20% is sodium carbonate and about 5 to 20% is sodium silicate of Na 2 O:SiO 2 ratio within the range of 1:1.4 to 1:3, with the ratio of sodium bicarbonate:sodium carbonate being within the range of about 1.2:1 to 8:1, the ratio of sodium carbonate:sodium silicate being within the range of about 1:3 to 3:1, the ratio of sodium bicarbonate:sodium silicate being within the range of about 1.5:1 to 5:1 and the ratio of zeolite to the sum of sodium bicarbonate, sodium carbonate and sodium silicate being within the range of about 1:4 to 4:1, which comprises preparing a crutcher slurry of the described composition by admixing with other components of such slurry an amount of sodium sesquicarbonate which will supply from about 20 to 100% of the sodium carbonate.
Claim 3
Dependent Claim
130 words
A method according to claim 1 wherein the crutcher slurry contains from 50 to 65% of solids and 50 to 35% of water, of which solids content 30 to 50% is zeolite, 25 to 40% is sodium bicarbonate, 8 to 17% is sodium carbonate and 8 to 18% is sodium silicate of Na 2 O:SiO 2 ratio within the range of 1:1.6 to 1:2.6, the ratio of sodium bicarbonate:sodium carbonate is within the range of 1.5:1 to 3:1, the ratio of sodium carbonate:sodium silicate is within the range of 1:2 to 2:1, the ratio of sodium bicarbonate:sodium silicate is within the range of 1.5:1 to 3:1 and the ratio of zeolite to the sum of sodium bicarbonate, sodium carbonate and sodium silicate is within the range of 1:3 to 2:1.
Claim 4
Dependent Claim
48 words
A method according to claim 1 wherein the crutcher slurry contains from 0.05 to 1% of a gelation inhibiting citric material selected from the group consisting of citric acid, water soluble citrate and mixtures thereof, which is incorporated in the slurry before addition of the sodium sesquicarbonate thereto.
Claim 5
Dependent Claim
51 words
A method according to claim 2 wherein the crutcher slurry contains from 0.1 to 0.5% of a gelation inhibiting citric material selected from the group consisting of citric acid, water soluble citrate and mixtures thereof, which is incorporated in the slurry before addition thereto of the sodium silicate and sodium sesquicarbonate.
Claim 6
Dependent Claim
18 words
A method according to claim 3 wherein the crutcher slurry contains from 0.1 to 2% of magnesium sulfate.
Claim 7
Dependent Claim
14 words
A method according to claim 4 wherein the zeolite is a Type A zeolite.
Claim 8
Dependent Claim
58 words
A method according to claim 6 wherein the order of addition to the crutcher of the components to form the crutcher slurry is water, citric material, zeolite, sodium bicarbonate, sodium carbonate, sodium silicate, as an aqueous solution, and sodium sesquicarbonate, and wherein the proportion of sodium carbonate supplied by the sodium sesquicarbonate is from 40 to 100% thereof.
Claim 9
Dependent Claim
27 words
A method according to claim 7 wherein the crutcher slurry is at a temperature in the range of 35° to 70° C. and is at atmospheric pressure.
Claim 10
Dependent Claim
167 words
A method according to claim 8 wherein the crutcher slurry contains from 53 to 65% of solids and 47 to 35% of water, of which solids content 35 to 45% is zeolite, 25 to 35% is sodium bicarbonate, 10 to 15% is sodium carbonate and 10 to 15% is sodium silicate of Na 2 O:SiO 2 ratio within the range of 1:2 to 1:2.4, the ratio of sodium bicarbonate:sodium carbonate is within the range of 1.7:1 to 2.2:1, the ratio of sodium carbonate:sodium silicate is within the range of 0.7:1 to 1.3:1, the ratio of sodium bicarbonate:sodium silicate is within the range of 1.7:1 to 2.4:1, the ratio of zeolite to the sum of sodium bicarbonate, sodium carbonate and sodium silicate is within the range of 1:2 to 1:1, the citric material is added as citric acid, the percentage of citric acid is 0.4 to 0.8%, on a solids basis and the percentage of sodium sesquicarbonate added is from 5 to 32%, on such solids content basis.
Claim 11
Dependent Claim
42 words
A method according to claim 1 wherein the mixing is at an elevated temperature, in the range of 35° to 70° C. and such mixing or holding is continued for at least one hour after completion of the making of crutcher slurry.
Claim 12
Dependent Claim
70 words
A method according to claim 9 wherein the crutcher slurry temperature is from 40° to 60° C., mixing or holding of the slurry is effected for at least two hours after completion of the making of the slurry, and at least a part of the slurry, after such two-hour period, is pumped out of the crutcher to a spray drying tower and is spray dried therein to dry particulate form.
Claim 13
Dependent Claim
15 words
A method according to claim 4 wherein the gelation preventing citric material is citric acid.
Claim 14
Dependent Claim
20 words
A method according to claim 12 wherein from 0.1 to 10% of the crutcher slurry is of adjuvant(s) and/or diluent(s).
Claim 15
Dependent Claim
18 words
A method according to claim 4 wherein the crutcher slurry contains from 0.2 to 1.5% of magnesium sulfate.
Claim 16
Dependent Claim
51 words
A method according to claim 12 wherein the percentage of citric acid is from 0.2 to 0.4, the crutcher slurry contains from 0.8 to 1.2% of magnesium sulfate and the citric acid and magnesium sulfate are incorporated in the slurry before addition thereto of at least some of the sodium silicate.
Claim 17
Dependent Claim
92 words
A method of making a particulate base material in bead form, suitable for absorbing nonionic detergent to make a built heavy duty synthetic organic detergent composition, which comprises making a miscible and pumpable slurry in a crutcher by the method of claim 1, pumping the slurry out of the crutcher in ungelled and readily pumpable state and spray drying the slurry to particulate bead form, during which spray drying a portion of the sodium sesquicarbonate is converted to sodium carbonate and a portion of the sodium bicarbonate is converted to sodium carbonate.
Claim 18
Dependent Claim
30 words
A method according to claim 16 wherein the sodium sesquicarbonate added to the crutcher slurry is of particle sizes in the range of No's. 160 to 230, U.S. Sieve Series.
Claim 19
Dependent Claim
30 words
A method according to claim 1 wherein the sodium sesquicarbonate added to the crutcher slurry is of particle sizes in the range of No's. 60 to 325, U.S. Sieve Series.
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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) | 1985-01-18 | 1985-07-20 | 1986-01-19 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-01-18 | 1989-07-20 | 1990-01-19 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-01-18 | 1993-07-20 | 1994-01-19 | $7700.00 | Window Closed / Lapsed |