Patent US3909284A successfully refreshed from Google Patents.
US3909284A
Expired / Lapsed
US
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Lake process
Assignee: Colorcon Inc
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Filing: 1973-12-26
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Granted: 1975-09-30
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Expires: 1993-12-26
Abstract
Abstract A method of making dry edible non-toxic color lakes approved for food and drug use and of submicron particle size, comprising the steps of dissolving sodium bicarbonate in water at a temperature not higher than 13*C., stirring aluminum chloride slowly into the cold sodium bicarbonate solution for about 2 hours, precipitating alumina hydrate, stirring the precipitated alumina hydrate for an additional half hour to insure the completion of the reaction, dissolving a dye in water, stirring the dye solution into the alumina hydrate slurry, adding a thin stream of aluminum chloride to the alumina hydrate slurry with stirring until the pH of the slurry reaches between about 4.1 to 4.3 to effect laking, continuing the slow stirring until the water-soluble dye has been completely absorbed onto the alumina hydrate, filtering the slurry in a filter press to form a filter cake, washing the filter cake with water to reduce the sodium chloride content thereof, drying the filter cake at 50*C. to produce a dry cake of agglomerated lake particles, and grinding the cake of agglomerated lake particles into lake particles of average size of 1 micron, with the majority of particles being submicron in size.
Inventors
- 👤 Edward J Woznicki
- 👤 Charles A Signorino
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 10:38
CPC Classifications
C; C09; C09B; C09B63/00; A; A23; A23L; A23L5/00; A23L5/40; A23L5/42; A23L5/47
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
152 words
A METHOD OF MAKING DRY EDIBLE NON-TOXIE COLOR LAKES APPROVED FOR FOOD AND DRUG USE AND OF SUBMICRON PARTICLE SIZE, COMPRISING THE STEPS OF DISSOLVING SODIUM BICARBONATE IN WATER AT A TEMPERATURE NOT HIGHER THAN 20*C, STIRRING ALUMINUM CHLORIDE INTO THE SODIUM BICARBONATE SOLUTION, THE PROPORTION OF SODIUM BICARBONATE TO ALUMINUM CHLORIDE BEING ABOUT 555 TO 1,000 IN PARTS BY WEIGHT, THE FINAL PH BEING ABOUT 5,5, PRECIPATING ALUMINA HYDRATE, STIRRING A DYE SOLUTION APPROVED BY FOA FOR INGESTION AND CONTAINING AN ACID GROUP FOR FORMING AN ALUMINUM SALT INTO THE ALUMINA HYDRATE SLURRY, STIRRING ALUMINUM CHLORIDE INTO THE SLURRY TO EFFECT LAKING, FORMING A FILTER CAKE, WASHING THE FILTER CAKE WITH WATER TO REDUCE THE SODIUM CHLORIDE CONTENT THEREOF, AND DRYING THE FILTER CAKE TO PRODUCE A DRY CAKE OF AGGLOMERATED LAKE PARTICLES, WHEREBY PRODCING A LAKE WHICH IS BRIGHTER, MORE BLEED FREE, MORE LIGHT STABLE, AND OF SUPERIOR TINTING STRENGTH.
Claim 2
Independent Claim
152 words
A METHOD OF MAKING DRY EDIBLE NON-TOXIE COLOR LAKES APPROVED FOR FOOD AND DRUG USE AND OF SUBMICRON PARTICLE SIZE, COMPRISING THE STEPS OF DISSOLVING SODIUM BICARBONATE IN WATER AT A TEMPERATURE NOT HIGHER THAN 20*C, STIRRING ALUMINUM CHLORIDE INTO THE SODIUM BICARBONATE SOLUTION, THE PROPORTION OF SODIUM BICARBONATE TO ALUMINUM CHLORIDE BEING ABOUT 555 TO 1,000 IN PARTS BY WEIGHT, THE FINAL PH BEING ABOUT 5,5, PRECIPATING ALUMINA HYDRATE, STIRRING A DYE SOLUTION APPROVED BY FOA FOR INGESTION AND CONTAINING AN ACID GROUP FOR FORMING AN ALUMINUM SALT INTO THE ALUMINA HYDRATE SLURRY, STIRRING ALUMINUM CHLORIDE INTO THE SLURRY TO EFFECT LAKING, FORMING A FILTER CAKE, WASHING THE FILTER CAKE WITH WATER TO REDUCE THE SODIUM CHLORIDE CONTENT THEREOF, AND DRYING THE FILTER CAKE TO PRODUCE A DRY CAKE OF AGGLOMERATED LAKE PARTICLES, WHEREBY PRODCING A LAKE WHICH IS BRIGHTER, MORE BLEED FREE, MORE LIGHT STABLE, AND OF SUPERIOR TINTING STRENGTH.
Claim 3
Dependent Claim
25 words
The method of claim 1, including grinding said dry cake of agglomerated lake particles into lake particles of an average size of about 1 micron.
Claim 4
Dependent Claim
45 words
The method of making lakes according to claim 1, including stirring the aluminum chloride slowly into the cold sodium bicarbonate solution for about two hours to a pH of 5.5, and stirring the precipitated alumina hydrate for an additional half hour to insure complete reaction.
Claim 5
Dependent Claim
37 words
The method of making lakes according to claim 1 including dissolving a dye in water at temperatures of about 20* to 60*C. to form said dye solution, before stirring the dye solution into the alumina hydrate slurry.
Claim 6
Dependent Claim
24 words
The method of making lakes according to claim 1 including adding the aluminum chloride to the hydratE-dye slurry in a thin stream with stirring.
Claim 7
Dependent Claim
29 words
The method of making lakes according to claim 1 including the step of drying the filter cake at about 50*C. to produce the dry cake of agglomerated lake particles.
Claim 8
Dependent Claim
187 words
The method of making lakes according to claim 1 including, in parts by weight, dissolving 555 parts of sodium bicarbonate in 7, 500 parts of water at a temperature not higher than about 13*C., stirring 1,000 parts of aluminum chloride solution, iron free, 32* Be into the bicarbonate solution with stirring at a rate which permits an orderly escape of the carbon dioxide gas generated in the reaction to a pH of 5.5, stirring the precipitated alumina hydrate for about a half hour, dissolving 185 parts of FD&C Yellow No. 5 water-soluble dye in 3,000 parts of water at about 20* to 25*C., stirring the dye solution into the precipitated hydrate, adding 250 parts of 32* Be aluminum chloride solution in a thin stream to the hydrate mixture with continuous stirring to a pH range of about 4.1 to 4.3, continuing the slow stirring until the water-soluble dye has been completely absorbed by the hydrate base, filtering the resulting lake to form a filter cake and washing it with water to reduce the chloride content of the finished lake to below 2%, and drying the filter cake.
Claim 9
Dependent Claim
15 words
A dry edible non-toxic color lake made in accordance with the method of claim 1.
Claim 10
Dependent Claim
20 words
The method of claim 1, wherein the sodium bicarbonate is dissolved in the water at a temperature of about 13*C.
Claim 11
Dependent Claim
19 words
The method of claim 1 including reslurrying the filter cake by adding water thereto, and spray drying said slurry.
Claim 12
Dependent Claim
25 words
The method of claim 1, including stirring the aluminum chloride into the alumina hydrate slurry to effect laking without washing or isolating the alumina hydrate.
Claim 13
Independent Claim
210 words
The method of making lakes, in parts by weight, by dissolving 555 parts of sodium bicarbonate in 7,500 parts of water at a temperature not higher than about 13*C., stirring 1, 000 parts of aluminum chloride solution, iron free, 32* Be into the bicarbonate solution with stirring at a rate which permits an orderly escape of the carbon dioxide gas generated in the reaction to a pH of 5.5, stirring the precipitated alumina hydrate for about a half hour, dissolving 185 parts of FD&C Yellow No. 5 watersoluble dye in 3,000 parts of water at about 20* to 25*C., stirring the dye solution into the precipitated hydrate, adding 250 parts of 32 Be aluminum chloride solution in a thin stream to the hydrate mixture with continuous stirring to a pH range of about 4.1 to 4.3, continuing the slow stirring until the water-soluble dye has been completely absorbed by the hydrate base, filtering the resulting lake to form a filter cake and washing it with water to reduce the chloride content of the finished lake to below 2%, and drying the filter cake to produce a dry cake of agglomerated lake particles, thereby producing a lake which is brighter, more bleed free, more light stable and of superior tinting strength.
Claim 14
Independent Claim
210 words
The method of making lakes, in parts by weight, by dissolving 555 parts of sodium bicarbonate in 7,500 parts of water at a temperature not higher than about 13*C., stirring 1, 000 parts of aluminum chloride solution, iron free, 32* Be into the bicarbonate solution with stirring at a rate which permits an orderly escape of the carbon dioxide gas generated in the reaction to a pH of 5.5, stirring the precipitated alumina hydrate for about a half hour, dissolving 185 parts of FD&C Yellow No. 5 watersoluble dye in 3,000 parts of water at about 20* to 25*C., stirring the dye solution into the precipitated hydrate, adding 250 parts of 32 Be aluminum chloride solution in a thin stream to the hydrate mixture with continuous stirring to a pH range of about 4.1 to 4.3, continuing the slow stirring until the water-soluble dye has been completely absorbed by the hydrate base, filtering the resulting lake to form a filter cake and washing it with water to reduce the chloride content of the finished lake to below 2%, and drying the filter cake to produce a dry cake of agglomerated lake particles, thereby producing a lake which is brighter, more bleed free, more light stable and of superior tinting strength.
Claim 15
Dependent Claim
25 words
The method of claim 12, including grinding said dry cake of agglomerated lake particles into lake particles of an average size of about 1 micron.
Claim 16
Dependent Claim
45 words
The method of making lakes accordingly to claim 12, including stirring the aluminum chloride slowly into the cold sodium bicarbonate solution for about two hours to a pH of 5.5, and stirring the precipitated alumina hydrate for an additional half hour to insure complete reaction.
Claim 17
Dependent Claim
37 words
The method of making lakes according to claim 12 including dissolving a dye in water at temperatures of about 20 to 60*C. to form said dye solution, before stirring the dye solution into the alumina hydrate slurry.
Claim 18
Dependent Claim
29 words
The method of making lakes according to claim 12 including tHe step of drying the filter cake at about 50*C. to produce the dry cake of agglomerated lake particles.
Claim 19
Dependent Claim
21 words
The method of claim 12 including reslurrying the filter cake after washing by adding water thereto, and spray drying said slurry.
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) | 1978-09-29 | 1979-03-31 | 1979-09-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-09-29 | 1983-03-31 | 1983-09-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-09-29 | 1987-03-31 | 1987-09-30 | $7700.00 | Window Closed / Lapsed |