DE1243643B - Process for the production of microcapsules - Google Patents

Process for the production of microcapsules

Info

Publication number
DE1243643B
DE1243643B DEJ20137A DEJ0020137A DE1243643B DE 1243643 B DE1243643 B DE 1243643B DE J20137 A DEJ20137 A DE J20137A DE J0020137 A DEJ0020137 A DE J0020137A DE 1243643 B DE1243643 B DE 1243643B
Authority
DE
Germany
Prior art keywords
microcapsules
polar
solution
production
freezing
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.)
Pending
Application number
DEJ20137A
Other languages
German (de)
Inventor
Mary H Huff
Henry P Marshall
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
International Business Machines Corp
Original Assignee
International Business Machines Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from US11286A external-priority patent/US3173878A/en
Application filed by International Business Machines Corp filed Critical International Business Machines Corp
Publication of DE1243643B publication Critical patent/DE1243643B/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • 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
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C1/00—Photosensitive materials
    • G03C1/002—Photosensitive materials containing microcapsules
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C5/00—Photographic processes or agents therefor; Regeneration of such processing agents
    • G03C5/18—Diazo-type processes, e.g. thermal development, or agents therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/16—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates the magnetic material being applied in the form of particles, e.g. by serigraphy, to form thick magnetic films or precursors therefor
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S101/00—Printing
    • Y10S101/29—Printing involving a color-forming phenomenon

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Color Printing (AREA)
  • Heat Sensitive Colour Forming Recording (AREA)

Description

Verfahren zur Herstellung von Mikrokapseln Zusatz zum Patent: 7 999 Gegenstand des Hauptpatents ist ein Verfahren zur Herstellung von im Inneren eine polare Lösung enthaltenden Mikrokapseln mit polymerer Kapselwand. Sie werden hergestellt, indem die polare Lösung in einer unpolaren Lösung hydrophober Polymerer dispergiert wird, eine unpolare Flüssigkeit, in der das Polymere unlöslich ist, unter Rühren zugegeben wird und die gebildeten Mikrokapseln gehärtet und von der Suspension abgetrennt werden.Process for the production of microcapsules. Patent addition: 7 999 The subject of the main patent is a process for the production of inside one polar solution containing microcapsules with a polymeric capsule wall. They are made by dispersing the polar solution in a non-polar solution of hydrophobic polymers becomes, a non-polar liquid in which the polymer is insoluble, with stirring is added and the microcapsules formed are hardened and separated from the suspension will.

Gegenstand der vorliegenden Erfindung ist nun, daß man die Mikrokapseln durch Gefrieren härtet. The present invention is now that the microcapsules hardens by freezing.

Der Gefrierprozeß kann auf verschiedene übliche Weisen erfolgen. So kann die Mikrokapselsuspension in indirekten oder direkten Kontakt mit einem Kältemittel, z. B. Trockeneis, gebracht werden. Es kann auch die Konvektionsmethode angewendet werden, bei der z. B. Trockeneisdämpfe oder tiefgekühlte Luft durch die Mischung geblasen werden. The freezing process can be accomplished in a number of conventional ways. So the microcapsule suspension can be in direct or indirect contact with a Refrigerants, e.g. B. dry ice, are brought. It can also be the convection method be used in the z. B. dry ice vapors or frozen air through the Mixture to be blown.

Nach der Gefrierhärtung können die gefrorenen Mikrokapseln auf verschieden übliche Art von dem Lösungsmittel getrennt werden. Bei einer erfindungsgemäß bevorzugten Arbeitsweise wird die gefrorene Mischung zur Trennung und Freisetzung der Mikrokapseln unter stark herabgesetztem Druck getrocknet. After freeze hardening, the frozen microcapsules can be used in different ways usual way to be separated from the solvent. In a preferred according to the invention The frozen mixture works to separate and release the microcapsules dried under reduced pressure.

Dadurch wird das Zusammenballen der einzelnen Mikrokapseln verhindert. Die Mikrokapseln mit ihrer eingekapselten Lösung bekommen das Aussehen und die Konsistenz eines trockenen Pulvers.This prevents the individual microcapsules from clumping together. The microcapsules with their encapsulated solution get their appearance and consistency of a dry powder.

Beispiel Eine Emulsion von Wasser (polares Lösungsmittel) in einer Benzollösung von Polystyrol (unvermischbare Polymerlösung) mit im wesentlichen der folgenden Zusammensetzung wird hergestellt: Gewichtsteile Polystyrol ........................ 45,0 Benzol ........................... 45,0 Dioctylnatriumsulfosuccinat ......... 2,0 Wasser ........................... 8,0 100,0 Bei der langsamen Zugabe von Cyclohexan wird Polystyrol um die sidpergierten Wassertröpfchen herum ausgefällt, und auf diese Weise wird eine Vielzahl von winzigen Polymermikrokapseln (0,5 bis 5 µ) gebildet. Nach Umrühren und Abkühlen auf etwa 15°C werden die Mikrokapseln von der Gleichgewichtsflüssigkeit durch Abgießen getrennt und durch Gefrieren gehärtet, indem ein Kolben, der die zurückbleibende Gleichgewichtsflüssigkeit enthält, in Trockeneis (etwa 570 C) gestellt wird. Danach werden die gefrorenen Mikrokapseln durch Verdunstung unter vermindertem Druck (20 mm Hg) getrocknet, wobei pulverförmige Mikrokapseln, die Wasser enthalten, erhalten werden. Example An emulsion of water (polar solvent) in one Benzene solution of polystyrene (immiscible polymer solution) with essentially the The following composition is produced: parts by weight of polystyrene ........................ 45.0 Benzene ........................... 45.0 Dioctyl Sodium Sulphosuccinate ......... 2.0 Water ........................... 8.0 100.0 With the slow addition of cyclohexane polystyrene is precipitated around the dispersed water droplets and onto them A multitude of tiny polymer microcapsules (0.5 to 5 µ) are formed. After stirring and cooling to about 15 ° C, the microcapsules are released from the equilibrium liquid separated by decantation and hardened by freezing by adding a plunger to the contains remaining equilibrium liquid, placed in dry ice (about 570 C) will. After that, the frozen microcapsules by evaporation under reduced Pressure (20 mm Hg) dried, taking powdered microcapsules containing water, can be obtained.

Die erhaltenen Mikrokapseln können in einem Überzugsmittel, wie beispielsweise einer Lösung von mit Kolophonium modifizierten Phenol-Formaldehyd-und Maleinsäure-Glycerid-Harzen in Erdölnaphtha oder einem mineralischen Verdünner, dispergiert werden und entweder auf ozalidartiges Diazopapier oder gewöhnliches Papier als Überzug aufgetragen werden. Auf diese Weise wird ein selbstentwickelndes Diazopapier erhalten, auf welchem Zeichen durch einfache Anwendung von Druck erzeugt werden können. The microcapsules obtained can be in a coating agent, such as a solution of phenol-formaldehyde and maleic acid-glyceride resins modified with rosin dispersed in petroleum naphtha or a mineral thinner, and either can be coated onto ozalide-like diazo paper or ordinary paper. In this way a self-developing diazo paper is obtained, on which characters can be generated by the simple application of pressure.

Claims (1)

Patentanspruch: Verfahren zum Herstellen von im Inneren eine polare Lösung enthaltenden Mikrokapseln mit polymerer Kapselwand durch Dispergieren der polaren Lösung in einer unpolaren Lösung hydrophober Polymerer, Zugabe einer unpolaren Flüssigkeit, in der das Polymere unlöslich ist, unter Rühren, Härten der gebildeten Mikrokapseln und Abtrennen derselben von der Suspension nach Patent 1 209 999, d a d u r c h g e k e n n z e i c n e t, daß man die Mikrokapseln durch Gefrieren härtet. Claim: Method for producing a polar inside Solution-containing microcapsules with polymeric capsule wall by dispersing the polar solution in a non-polar solution more hydrophobic Polymeric, Adding a non-polar liquid in which the polymer is insoluble, with stirring, Hardening of the microcapsules formed and separation of the same from the suspension Patent 1 209 999, d u r c h e k e n n n z e i c n e t that you can get the microcapsules hardens by freezing. In Betracht gezogene Druckschriften: USA.-Patentschrift Nr. 2 800 457. References considered: U.S. Patent No. 2,800 457
DEJ20137A 1960-02-26 1961-06-24 Process for the production of microcapsules Pending DE1243643B (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US1134160A 1960-02-26 1960-02-26
US11286A US3173878A (en) 1960-02-26 1960-02-26 Process of making microcapsules
US11287A US3111407A (en) 1960-02-26 1960-02-26 Methods for making record materials
US3915060A 1960-06-27 1960-06-27

Publications (1)

Publication Number Publication Date
DE1243643B true DE1243643B (en) 1967-07-06

Family

ID=27486076

Family Applications (2)

Application Number Title Priority Date Filing Date
DEJ19475A Pending DE1209999B (en) 1960-02-26 1961-02-23 Process for the production of microcapsules
DEJ20137A Pending DE1243643B (en) 1960-02-26 1961-06-24 Process for the production of microcapsules

Family Applications Before (1)

Application Number Title Priority Date Filing Date
DEJ19475A Pending DE1209999B (en) 1960-02-26 1961-02-23 Process for the production of microcapsules

Country Status (4)

Country Link
US (1) US3111407A (en)
DE (2) DE1209999B (en)
GB (2) GB898668A (en)
IT (1) IT631615A (en)

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GB898668A (en) 1962-06-14
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DE1209999B (en) 1966-02-03
IT631615A (en)

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