Patent US3201484A successfully refreshed from Google Patents.
US3962384A
Expired / Lapsed
US
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Spray-drying technique for preparing agglomerated powders
Assignee: Hoffmann La Roche Inc
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Filing: 1974-06-26
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Granted: 1976-06-08
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Expires: 1994-06-26
Abstract
Abstract A novel spray-drying technique process, and the resulting composition, for preparing a high density, agglomerated vitamin-containing composition having improved tableting characteristics.
Inventors
- 👤 Marco Alfred Cannalonga
- 👤 Louis Vincent Czarecki
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 19:01
CPC Classifications
B; B01; B01D; B01D1/00; B01D1/16; B01D1/18; A; A61; A61K; A61K9/00; A61K9/14; A61K9/141; A61K9/143; A61K9/148; A61K9/48; A61K9/50; A61K9/5005; A61K9/5021; A61K9/5052; A61K9/5057
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
187 words
In a process for preparing coated agglomerated powders suitable for direct compression tablets comprising: A. spraying into a spray dryer chamber droplets of a spray-dryable formulation selected from the group consisting of an aqueous vitamin slurry and an aqueous vitamin emulsion, to produce a spray-dried powder thereby, the improvement comprising: B. metering into said chamber, in a concentration of about 1-5% by weight, based on the weight of said spray-dried powder, a dry particulate absorbent having: a. a particle size of from about 2 microns to about 16 microns; b. an oil absorption capacity of from about 150 to about 400 pounds of oil per 100 pounds of absorbent; c. a surface area of from about 175 to about 360 square meters per gram; d. insolubility in cold water; e. resistance to wetting by water; f. a free-flowing property and g. ability to not develop static electricity said absorbent contacting said spray droplets in a semi-dry condition to coat said droplets and form a dry agglomerated powder thereof, wherein said absorbent minimizes the development of static electricity during step A and on the resulting dried agglomerated powder.
Claim 2
Dependent Claim
187 words
In a process for preparing coated agglomerated powders suitable for direct compression tablets comprising: A. spraying into a spray dryer chamber droplets of a spray-dryable formulation selected from the group consisting of an aqueous vitamin slurry and an aqueous vitamin emulsion, to produce a spray-dried powder thereby, the improvement comprising: B. metering into said chamber, in a concentration of about 1-5% by weight, based on the weight of said spray-dried powder, a dry particulate absorbent having: a. a particle size of from about 2 microns to about 16 microns; b. an oil absorption capacity of from about 150 to about 400 pounds of oil per 100 pounds of absorbent; c. a surface area of from about 175 to about 360 square meters per gram; d. insolubility in cold water; e. resistance to wetting by water; f. a free-flowing property and g. ability to not develop static electricity said absorbent contacting said spray droplets in a semi-dry condition to coat said droplets and form a dry agglomerated powder thereof, wherein said absorbent minimizes the development of static electricity during step A and on the resulting dried agglomerated powder.
Claim 3
Dependent Claim
30 words
The process of claim 1 wherein the absorbent is selected from the group consisting of silicic acid, silica gel, an alkali metal silicate, magnesium carbonate, kaolin clay and dicalcium phosphate.
Claim 4
Dependent Claim
87 words
The process of claim 1 wherein the formulation is an aqueous emulsion containing, in percents by weight on a dry weight basis, from about 45% to about 60% of dl-α-tocopheryl acetate, from about 38% to about 53% of a hydrolyzed gelatin having a O Bloom and a molecular weight of about 9,000 to 11,000, about 0.1% of sodium benzoate and about 0.2% of sorbic acid and the absorbent comprises from about 1% to about 3% by weight silicic acid, base on the weight of the agglomerated powder.
Claim 5
Dependent Claim
84 words
The process of claim 1 wherein the formulation is an aqueous emulsion containing, in percents by weight on a dry weight basis, from about 15% to about 30% vitamin A palmitate, from about 50% to about 65% of a hydrolyzed gelatin of low Bloom, from about 10% to about 20% of sucrose and from about 2% to about 6% of 1,2-dihydroxy-6-ethoxy-2,2,4-trimethyl-quinoline and said absorbent comprises from about 1% to about 3% by weight of silicic acid, based on the weight of the agglomerated powder.
Claim 6
Dependent Claim
76 words
The process of claim 1 wherein the formulation is an aqueous slurry containing, in percents by weight on a dry weight basis, from about 45% to about 65% of riboflavin, from about 15% to about 25% of a non-absorbent inorganic filler and from about 15% to about 35% of a hydrolyzed cereal flour and the absorbent comprises from about 1% to about 5% by weight, of silicic acid, based on the weight of the agglomerated powder.
Claim 7
Dependent Claim
65 words
The process of claim 1 wherein the formulation is an aqueous emulsion containing, in percents by weight on a dry weight basis, from about 20% to about 30% of a flavor oil, and from about 70% to about 80% of low bloom hydrolyzed gelatin and the absorbent comprises from about 1% to about 3% of silicic acid, based on the weight of the agglomerated powder.
Claim 8
Dependent Claim
51 words
The process of claim 1 wherein said absorbent is a mixture comprising, in percents by weight based on the weight of said absorbent, from about 1% to about 15% of the absorbent as defined in claim 20 and from about 99% to about 85% of the spray dried formulation without absorbent.
Claim 9
Dependent Claim
30 words
The process of claim 7 wherein the absorbent is selected from the group consisting of silicic acid, silica gel, an alkali metal silicate, magnesium carbonate, kaolin clay and dicalcium phosphate.
Claim 10
Dependent Claim
28 words
The process of claim 7 wherein the absorbent comprises from about 1% to about 2% by weight based on the dry weight of the formulation being spray dried.
Claim 11
Dependent Claim
243 words
In a process for preparing agglomerated Vitamin E powders for direct compression tabletting comprising A. spraying into a dryer chamber droplets of a spray-dryable Vitamin E aqueous emulsion formulation to produce a spraydried Vitamin E powder thereby, the improvement comprising B. metering into said chamber in a concentration of from about 1% to about 2% by weight, based on the weight of the spraydried powder, of a dry particulate absorbent consisting of a mixture of a. from about 4% to about 12% of a calcium silicate having: i. an average particle size of 3.4 microns, ii. an oil absorption capacity of 100-300 pounds of oil per 100 pounds of calcium silicate, and iii. a surface area of 175 square meters per gram and b. from about 96% to about 88% of a spray-dried Vitamin E composition, prepared without absorbent in the dryer chamber, having: i. a particle size range of from about 20 to about 30 microns, ii. from about 15% to about 20% of dl-α-tocopheryl acetate, iii. from about 80% to about 85% of hydrolyzed gelatin of O Bloom and a molecular weight of about 7,000 to about 11,000, iv. about 1% of sodium benzoate and v. about 0.7% of sorbic acid said absorbent contacting said spray droplets in a semi-dry condition to coat said droplets and form a dry agglomerated powder thereof, wherein said absorbent minimizes the development of static electricity during step A and on the resulting dried agglomerated powder.
Claim 12
Dependent Claim
243 words
In a process for preparing agglomerated Vitamin E powders for direct compression tabletting comprising A. spraying into a dryer chamber droplets of a spray-dryable Vitamin E aqueous emulsion formulation to produce a spraydried Vitamin E powder thereby, the improvement comprising B. metering into said chamber in a concentration of from about 1% to about 2% by weight, based on the weight of the spraydried powder, of a dry particulate absorbent consisting of a mixture of a. from about 4% to about 12% of a calcium silicate having: i. an average particle size of 3.4 microns, ii. an oil absorption capacity of 100-300 pounds of oil per 100 pounds of calcium silicate, and iii. a surface area of 175 square meters per gram and b. from about 96% to about 88% of a spray-dried Vitamin E composition, prepared without absorbent in the dryer chamber, having: i. a particle size range of from about 20 to about 30 microns, ii. from about 15% to about 20% of dl-α-tocopheryl acetate, iii. from about 80% to about 85% of hydrolyzed gelatin of O Bloom and a molecular weight of about 7,000 to about 11,000, iv. about 1% of sodium benzoate and v. about 0.7% of sorbic acid said absorbent contacting said spray droplets in a semi-dry condition to coat said droplets and form a dry agglomerated powder thereof, wherein said absorbent minimizes the development of static electricity during step A and on the resulting dried agglomerated powder.
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) | 1979-06-08 | 1979-12-08 | 1980-06-08 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-06-08 | 1983-12-08 | 1984-06-08 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-06-08 | 1987-12-08 | 1988-06-08 | $7700.00 | Window Closed / Lapsed |