US3406119A - Encapsulation - Google Patents
Encapsulation Download PDFInfo
- Publication number
- US3406119A US3406119A US437464A US43746465A US3406119A US 3406119 A US3406119 A US 3406119A US 437464 A US437464 A US 437464A US 43746465 A US43746465 A US 43746465A US 3406119 A US3406119 A US 3406119A
- Authority
- US
- United States
- Prior art keywords
- capsules
- oil
- albumin
- particles
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/124—Duplicating or marking methods; Sheet materials for use therein using pressure to make a masked colour visible, e.g. to make a coloured support visible, to create an opaque or transparent pattern, or to form colour by uniting colour-forming components
- B41M5/165—Duplicating or marking methods; Sheet materials for use therein using pressure to make a masked colour visible, e.g. to make a coloured support visible, to create an opaque or transparent pattern, or to form colour by uniting colour-forming components characterised by the use of microcapsules; Special solvents for incorporating the ingredients
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/08—Simple coacervation, i.e. addition of highly hydrophilic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/26—Thermography ; Marking by high energetic means, e.g. laser otherwise than by burning, and characterised by the material used
- B41M5/28—Thermography ; Marking by high energetic means, e.g. laser otherwise than by burning, and characterised by the material used using thermochromic compounds or layers containing liquid crystals, microcapsules, bleachable dyes or heat- decomposable compounds, e.g. gas- liberating
- B41M5/287—Thermography ; Marking by high energetic means, e.g. laser otherwise than by burning, and characterised by the material used using thermochromic compounds or layers containing liquid crystals, microcapsules, bleachable dyes or heat- decomposable compounds, e.g. gas- liberating using microcapsules or microspheres only
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2984—Microcapsule with fluid core [includes liposome]
Definitions
- One prior art material provides for two layers of reactants separated by a third fusible intermediate layer. Heating the composite layers causes melting of the fusible intermediate layer, thereby allowing the two outer layers to commingle and react. The reactants are thus separated by the intermediate layer until needed. This provides convenience for the user since one of the reactants need not be held in reserve and added at the desired time.
- Another method of isolating at least one of the reactants is to encapsulate the item in a shell or envelope of unreactive material. When needed, the reactant is made available by breaking the shell.
- One form of capsule is the developer pod used in the photographic art. These pods or capsules contain the active ingredients necessary to rapidly develop exposed photographic images. The capsules are broken physically by squeezing.
- capsules presents a handicap for some applications, and therefore, capsules of fine size have been developed. These find use in such specific and varied applications as food flavorings, medicines, and photography. Some of the advantages afforded by the use of such capsules in the photographic art are isolation of reactants until desired, coating simplicity, convenience in development, indefinitely long storage life for sensitized materials, (and fine resolutions).
- the present invention provides a novel method for making simple capsules.
- This method involves the discovery that certain materials can be dissolved in water at room temperature and be precipitated from the water at elevated temperatures.
- polymer A is dissolved in water at one temperature.
- Water-immiscible material B is then added to the solution and dispersed to a fine size.
- the dispersion is then heated until the polymer coagulates around the particles or globules.
- the resuplting capsules may then be filtered, hardened, and dried.
- one object of the present invention is to provide capsules and novel methods for making capsules.
- Another object is to provide methods for encapsulating material by means of heat, and providing capsules so formed.
- the objects of the present invention may be realized by dissolving a heat-coagulatable polymer or colloid in cold water, dispersing a water-immiscible oil or solid in the solution, and then heating the dispersion to coagulate the polymer around the particles in the form of a shell.
- FIGURE 1 is a flow sheet of the present method.
- FIGURE 2 is a capsule of the present invention.
- step 1A a water-immiscible material is dispersed in an aqueous solution of heat-coagulateable polymer to form a dispersion of particles.
- step 1B the dispersion is heated to coagulate polymer on the particles as shells, thereby producing discrete capsules.
- Optional steps not shown in FIGURE 1 include separation of the capsules from the solution, washing the capsules, and drying the capsules.
- the capsule 20 of FIGURE 2 comprises core 21 and shell 22.
- Core 21 comprises water-immiscible material which may be solid or liquid.
- Shell 22 comprises heatcoagulated polymer completely surrounding core 21 and substantially impervious to the core material 21.
- Egg albumin coagulates at temperatures of 60-70 C., but it was found that lower temperatures are suitable for the present invention. Blood albumin was also suitable.
- Albumin capsules do not form the hard agglomerates that casein capsules do and therefore offer greater advantages in coating applications where uniformity is desirable. As with casein capsules, however, use of an antifoaming agent is helpful. Silicones have served effectively as an anti-foam agents for albumin sols.
- Ratios of 7.5 parts oil to one part albumin have been successfully used.
- the range may vary from 1:1 to 10:1.
- coagulation by means of heat can be effected in any of several ways.
- the size of the capsule is determined by the size of the oil droplet in the oil-in-water emulsion. Particle sizes preferably range [from 1 micron to 50 microns in diameter. The particles may be solid or liquid at the time of shell-formation.
- Example 1 10 grams of egg albumin were dissolved in 200 ml. of water at room temperature. Seven drops of a 30% silicone anti-foam (Antifoam 60) were added to the albumin s01. Added next was 20 ml. of cotton seed oil in which was dissolved 0.5 gram of an oil black dye (CI Solvent Black 12). An emulsion was made using an air-powered mechanical stirrer. An electrical hot plate was used to heat the emulsion to 70 C. and thereby form capsules. Stirring was continued throughout the heating process. The capsules were then filtered from the solution.
- Antifoam 60 a 30% silicone anti-foam
- CI Solvent Black 12 an oil black dye
- the capsules were spherical and ranged from 5 to 50 microns in diameter. They were placed in acetone to test the imperviousness of the capsule shell. No color was imparted to the acetone phase. The capsules were then crushed to release the dyed oil. The acetone then took on the color of the dye.
- oil soluble dye is not necessary for the encapsulation of material. It was used here to show that the oil could be a carrier for another material and as a marking material to demonstrate the imperviousness of the capsule shell.
- Example 2 grams of egg albumin were dissolved in cold water and 7 drops of a silicone anti-foam agent were added. 0.5 gram of carbon tetrabromide and 0.2 gram of Cyasorb IR-117 infrared radiation absorber were dissolved in 20 ml. of cotton seed oil and added to the albumin sol. An air powered stirrer was used to emulsify the oil in the aqueous phase. With continued stirring, the emulsion was exposed to an infrared lamp (reflecting drying lamp, 250 watt) in order to cause coagulation of the egg albumin as shells around the oil droplets. Samples to be inspected under the microscope were obtained with a pipette.
- infrared lamp reflecting drying lamp, 250 watt
- Capsules were already present when the temperature of the aqueous phase reached C. When the temperature of the aqueous phase reached C., the mixture was filtered. The capsules thus obtained were washed with acetone and the filtrate mixed with diphenylamine and exposed to a UV light source (500 watt projection lamp). No color developed. The capsules were then crushed in acetone, the filtrate mixed with diphenylamine, and the mixture exposed to the light source. A blue color was formed. Carbon black was also suitable and an infrared absorber.
- Example 3 10 grams of egg albumin were dissolved in 200 ml. of water. Five drops of a 30% silicone anti-foaming agent were added to the albumin sol. Two grams of carbon tetrabromide were dissolved in 20 ml. of Castor oil and placed, along with the albumin sol, into a Waring Blendor (model CB4). An oil in water emulsion was prepared by operating the blender at 17,000 rpm. After two minutes of operation, 500 ml. of boiling water were added to form the capsules and the stirring was continued for another 1 /2 minutes. The capsules were then filtered from the solution.
- a Waring Blendor model CB4
- the capsules were spherical and about 10 microns in diameter. They were washed with benzene and the filtrate was mixed with diphenylamine and exposed to a strong light source. No color was formed. The capsules were then crushed in the benzene and the filtrate was mixed with diphenylamine and exposed to light source. A deep blue color developed as in Example 2.
- a method of making capsules comprising:
- a method of making capsules comprising:
- a method of making capsules comprising:
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Description
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US437464A US3406119A (en) | 1965-03-05 | 1965-03-05 | Encapsulation |
DE19661542261 DE1542261A1 (en) | 1965-03-05 | 1966-03-03 | Process for the production of capsules containing liquids or solids |
GB9698/66A GB1126856A (en) | 1965-03-05 | 1966-03-04 | Improvements in and relating to encapsulation |
FR52142A FR1470723A (en) | 1965-03-05 | 1966-03-04 | Process for preparing capsules containing liquids or solids |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US437464A US3406119A (en) | 1965-03-05 | 1965-03-05 | Encapsulation |
Publications (1)
Publication Number | Publication Date |
---|---|
US3406119A true US3406119A (en) | 1968-10-15 |
Family
ID=23736565
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US437464A Expired - Lifetime US3406119A (en) | 1965-03-05 | 1965-03-05 | Encapsulation |
Country Status (4)
Country | Link |
---|---|
US (1) | US3406119A (en) |
DE (1) | DE1542261A1 (en) |
FR (1) | FR1470723A (en) |
GB (1) | GB1126856A (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3922379A (en) * | 1973-12-17 | 1975-11-25 | Abbott Lab | Microencapsulation process |
US4619904A (en) * | 1984-10-29 | 1986-10-28 | General Electric Company | Agglutinating immunoassay using protein-coated liquid droplets |
US4634681A (en) * | 1984-10-29 | 1987-01-06 | General Electric Company | Diagnostic method of determining the presence or absence of select proteins in a liquid sample |
US5418010A (en) * | 1990-10-05 | 1995-05-23 | Griffith Laboratories Worldwide, Inc. | Microencapsulation process |
US6610348B2 (en) | 1997-02-17 | 2003-08-26 | Fonterra Tech Limited | Gelling agents and gels containing them |
WO2009006792A1 (en) * | 2007-07-06 | 2009-01-15 | The University Of Hong Kong | Collagen-based microspheres and methods of preparation and use thereof |
EP4035655A1 (en) * | 2021-02-01 | 2022-08-03 | Oxford University Innovation Limited | Immune modulating particles |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0349428B1 (en) * | 1988-06-30 | 1993-01-20 | Centre National De La Recherche Scientifique (Cnrs) | Process for preparing colloidal dispersive protein systems in the shape of nanoparticles |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3137631A (en) * | 1959-12-01 | 1964-06-16 | Faberge Inc | Encapsulation in natural products |
US3190837A (en) * | 1958-12-31 | 1965-06-22 | Ncr Co | Making individual capsules by dual deposition |
-
1965
- 1965-03-05 US US437464A patent/US3406119A/en not_active Expired - Lifetime
-
1966
- 1966-03-03 DE DE19661542261 patent/DE1542261A1/en active Pending
- 1966-03-04 FR FR52142A patent/FR1470723A/en not_active Expired
- 1966-03-04 GB GB9698/66A patent/GB1126856A/en not_active Expired
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3190837A (en) * | 1958-12-31 | 1965-06-22 | Ncr Co | Making individual capsules by dual deposition |
US3137631A (en) * | 1959-12-01 | 1964-06-16 | Faberge Inc | Encapsulation in natural products |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3922379A (en) * | 1973-12-17 | 1975-11-25 | Abbott Lab | Microencapsulation process |
US4619904A (en) * | 1984-10-29 | 1986-10-28 | General Electric Company | Agglutinating immunoassay using protein-coated liquid droplets |
US4634681A (en) * | 1984-10-29 | 1987-01-06 | General Electric Company | Diagnostic method of determining the presence or absence of select proteins in a liquid sample |
US5418010A (en) * | 1990-10-05 | 1995-05-23 | Griffith Laboratories Worldwide, Inc. | Microencapsulation process |
US6610348B2 (en) | 1997-02-17 | 2003-08-26 | Fonterra Tech Limited | Gelling agents and gels containing them |
WO2009006792A1 (en) * | 2007-07-06 | 2009-01-15 | The University Of Hong Kong | Collagen-based microspheres and methods of preparation and use thereof |
CN101868298B (en) * | 2007-07-06 | 2013-02-06 | 香港大学 | Collagen-based microspheres and methods of preparation and use thereof |
EP4035655A1 (en) * | 2021-02-01 | 2022-08-03 | Oxford University Innovation Limited | Immune modulating particles |
Also Published As
Publication number | Publication date |
---|---|
GB1126856A (en) | 1968-09-11 |
DE1542261A1 (en) | 1970-03-26 |
FR1470723A (en) | 1967-02-24 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
AS | Assignment |
Owner name: SECURITY NATIONAL BANK, A NATIONAL BANKING ASSOCIA Free format text: SECURITY INTEREST;ASSIGNOR:KEUFFEL & ESSER COMPANY A.N.J. CORP;REEL/FRAME:003969/0808 Effective date: 19820323 Owner name: CHASE MANHATTAN BANK, N.A. THE; A NATIONAL BANKING Free format text: SECURITY INTEREST;ASSIGNOR:KEUFFEL & ESSER COMPANY A.N.J. CORP;REEL/FRAME:003969/0808 Effective date: 19820323 Owner name: CHEMICAL BANK, A BANKING INSTITUTION OF NY. Free format text: SECURITY INTEREST;ASSIGNOR:KEUFFEL & ESSER COMPANY A.N.J. CORP;REEL/FRAME:003969/0808 Effective date: 19820323 Owner name: CONTINENTAL ILLINOIS NATIONAL BANK & TRUST CO., OF Free format text: SECURITY INTEREST;ASSIGNOR:KEUFFEL & ESSER COMPANY A.N.J. CORP;REEL/FRAME:003969/0808 Effective date: 19820323 Owner name: BANK OF CALIFORNIA N.A. THE; A NATIONAL BANKING AS Free format text: SECURITY INTEREST;ASSIGNOR:KEUFFEL & ESSER COMPANY A.N.J. CORP;REEL/FRAME:003969/0808 Effective date: 19820323 Owner name: CHEMICAL BANK, A BANKING INSTITUTION OF, NEW YORK Free format text: SECURITY INTEREST;ASSIGNOR:KEUFFEL & ESSER COMPANY A.N.J. CORP;REEL/FRAME:003969/0808 Effective date: 19820323 |