EP0898206B1 - Procédé pour enrober des particules porteuses pour développateurs électrostatiques - Google Patents

Procédé pour enrober des particules porteuses pour développateurs électrostatiques Download PDF

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Publication number
EP0898206B1
EP0898206B1 EP19980202689 EP98202689A EP0898206B1 EP 0898206 B1 EP0898206 B1 EP 0898206B1 EP 19980202689 EP19980202689 EP 19980202689 EP 98202689 A EP98202689 A EP 98202689A EP 0898206 B1 EP0898206 B1 EP 0898206B1
Authority
EP
European Patent Office
Prior art keywords
particles
carrier particles
vessel
coating
solvent
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
Application number
EP19980202689
Other languages
German (de)
English (en)
Other versions
EP0898206A2 (fr
EP0898206A3 (fr
Inventor
Raphael Voets
Serge C/O Agfa-Gevaert N.V. Tavernier
Gerrit c/o Agfa-Gevaert N.V. Delen
Rainer Bellinghausen
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.)
Xeikon Manufacturing NV
Original Assignee
Xeikon International NV
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
Application filed by Xeikon International NV filed Critical Xeikon International NV
Priority to EP19980202689 priority Critical patent/EP0898206B1/fr
Publication of EP0898206A2 publication Critical patent/EP0898206A2/fr
Publication of EP0898206A3 publication Critical patent/EP0898206A3/fr
Application granted granted Critical
Publication of EP0898206B1 publication Critical patent/EP0898206B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00—Developers
    • G03G9/08—Developers with toner particles
    • G03G9/10—Developers with toner particles characterised by carrier particles
    • G03G9/113—Developers with toner particles characterised by carrier particles having coatings applied thereto
    • G03G9/1131—Coating methods; Structure of coatings
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00—Developers
    • G03G9/08—Developers with toner particles
    • G03G9/10—Developers with toner particles characterised by carrier particles
    • G03G9/113—Developers with toner particles characterised by carrier particles having coatings applied thereto
    • G03G9/1132—Macromolecular components of coatings
    • G03G9/1135—Macromolecular components of coatings obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • G03G9/1136—Macromolecular components of coatings obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon atoms

Definitions

  • This invention relates to a method for coating carrier particles. It relates especially to a method for coating carrier particles to be used as carrier particles in multi-component developers for electrostatic imaging with magnetic brush development as well in cascade development. The invention is also very suitable to prepare coated glass beats for chromatographic purposes.
  • the carrier particles can be added to a fluidised bed and the coating solution of a chemical substance in a solvent is then added to the fluidised bed and the solvent evaporated.
  • This method gives good coating results, but the amount of air needed to form the fluidised bed is such that the evaporated solvent (which in most cases is an organic solvent) contaminates a large volume of air, which can not without further treatment be vented in the open atmosphere. Therefore the installations for fluidised bed coating are quite large and expensive.
  • the carrier particles are strongly agitated and many collisions occur which damage the coating around the carrier particles.
  • the carrier particles are mixed (dispersed) in a solution of the chemical compound or compounds that are to be applied on the surface of the carrier particles and the particles are spray-dried. Again this method gives good coating results, but the installation needed for spray drying is expensive.
  • the coating has to be very homogenous over the surface of the particles to be coated.
  • the carrier particles are mixed with toner particles (and with other ingredients) to form a developer.
  • the carrier particles are magnetic
  • the carrier particles can be coated glass beads.
  • the rubbing of the carrier particles and the toner particles induce a tribo-electric charge in the toner particles and the nature of the coating on the carrier particles determines, together with the toner ingredients, the polarity of the charge on the tone particles as well as the amount of the charge.
  • Very homogenous coating of particles are not only desirable for carrier particles to be used in an electrostatic developer, but also for other particles, e.g., particles that are used in absorption chromatography.
  • the objects of the invention are realised by providing a method for coating carrier particles, having a volume average diameter between 20 and 200 ⁇ m, for use in electrostatic developers, comprising the steps of :
  • the particles to be coated are brought in a stationary vessel equipped with a mechanical stirrer, in a second embodiment, no stirrer is present in the vessel, but the vessel is vibrated by vibrating means, e.g. the vessel is mounted on a vibrating table.
  • the vessel is a tube, capped on both ends and after filling the tube with carrier particles to be coated, the tube is agitated, e.g., by rolling the tube parallel to its cylindrical axis.
  • a vessel for implementing the method of this invention can be of any type and the stirring of the carrier particles in the vessel can proceed by any means, e.g., by internal stirrers of any type, by external vibrating of the vessel or by rolling the vessel, as long as in the vessel the mechanical agitation of the carrier particles is described by a Froude number between 0.2 and 20, preferably between 0.5 and 8, both limits included. When the Froude number was out side of these limits the carrier particles tend to aggregate or the agitation is too heavy, so that damaging of the carrier particles and the coating can be introduced.
  • the Froude number is a description of a specific ratio of inertia versus gravity forces, both forces being of importance in the description of agitation, as is discussed in the publication entitled KENZAHLEN UND ⁇ HNLICHKEITSGESETZE IM INGENIEURWESEN, by J. Stichlmair, p 33, published by Altos-Verlag Doris Stichlmair Essen 1990.
  • the vessel for implementing the method of this invention is equipped with a stirrer of which the blades are essentially perpendicular (i.e. a deviation of 10 degrees is acceptable) to the bottom of the vessel. It was possible in such a device to mix enough air with the carrier particles to form a loose bed of particles. It was found that an adequate loose bed of particles could be produced when the carrier particles occupied at most 85 % by volume of the vessel. It is preferred to rotate the stirrer at such a velocity that within the vessel the mechanical agitation of the particles is described by a Froude number between 0.2 and 20, preferably between 0.5 and 8, both limits included.
  • the vessel is basically cylindrical and that walls of the cylinder are placed in a basically horizontal plane and that the shaft of the stirrer is mounted essentially parallel to the walls of the cylinder and the blades perpendicular to these walls.
  • a very useful type of mixing apparatus to form a loose bed of particles in the method according to this invention is a ploughshare mixer.
  • a ploughshare mixer is, e.g., commercially available from Gebrüder Lödige Maschinenbau GmbH, D33050 Paderborn, Germany.
  • the blades on the shaft of the stirrer have the shape of a ploughshare.
  • Another interesting embodiment is the use of a vessel, mounted on a vibrating stage, as sold by Fritsch GmbH, Industriestrasse 8, Idar-Oberstein, W-Germany
  • a solution of a coating compound containing between 6 and 60 % by weight with respect to the total volume of said solution in a solvent, preferably between 15 and 40 % by weight with respect to the total volume of said solution is added at such a rate that at any time of the coating process in the method of this invention for every cm 2 of the surface of all particles present in the vessel at most 1.25 10 -4 ml of solvent is present in the vessel a good coating of the particles could be assured.
  • the rate of addition of the solution containing the coating compound is such that for every cm 2 of the surface of all particles present in the vessel at most 0.6 10 -4 ml of solvent is present in the vessel.
  • the surface of the particles is calculated from the average volume diameter of the particles, (measured by sieve analysis) assuming the particles are a spherical, this amount boils down to particles having a layer of solvent that is at most about 1 ⁇ m thick.
  • the coating compounds once adhered to the particles are almost immediately dry and no or very low adherence of the particles to each other due to possible adhesive forces of the coating compounds occurs.
  • the addition of the solution in the method of this invention can proceed by any means for rate-controlled injection of fluids known in the art. In can be single or multiple injection, multiple injection (i.e. injection over several nozzles) is preferred in the method of this invention since it gives even better homogeneity of the coating on the particles.
  • the temperature of the loose bed of particles i.e. the temperature of the particles in the vessel
  • the temperature of the loose bed of particles is held at a temperature that is at most 10 °C higher than the boiling point of the solvent that is used in the solution containing the coating compound.
  • the temperature of the loose bed i.e. the particles in the vessel
  • the temperature of the loose bed of particles is held at a temperature that is at most (A + 10) °C, preferably the temperature in the vessel is at most (A + 5) °C.
  • the temperature of the loose bed of particles is held at a temperature that is at most 10 °C higher, preferably at most 5 °C higher, than the boiling point of the solvent with the lowest boiling point.
  • the boiling point means the boiling point at the atmospheric pressure at which the coating is carried out.
  • the boiling point to be considered is the boiling point at normal atmospheric pressure
  • the boiling point to be considered is the boiling point at that lowered pressure.
  • the solvent is continuously evaporated.
  • the apparatus is preferably a closed system, and the solvent is evaporated from the agitated vessel, and is recovered by trapping the solvent in a cooler.
  • the method according to the present invention works very well when the particles to be coated have an average weight, W avg , calculated by multiplying the specific gravity of the particles - expressed in Kg/m 3 - with the average volume of the particle calculated from the average volume diameter - expressed in m - of the particle while considering the particles as a sphere) such that 1 10 -11 Kg ⁇ W avg ⁇ 5 10 -8 Kg.
  • the method of this invention is especially well suited for coating particles with an average weight W avg such that 1 10 -10 Kg ⁇ W avg ⁇ 1 10 -8 Kg.
  • the coated particles can be post-treated in the vessel and the temperature, stirring speed, etc. can be adjusted to assure a good post-treatment.
  • a post-treatment can, e.g., be desirable to evacuate traces of solvent, of moisture, etc.
  • the post-treatment can also be desirable to harden the coating.
  • the post-treatment can proceed inside the vessel wherein the coating by the method of this invention has been carried out, as well as outside the vessel, if so desired, in a rolling drum, an oven etc.
  • the coated particles can be agitated as well as not.
  • the method of this invention is very well suited to produce particles with a layered coating.
  • the method of this invention makes it possible to coat particles with a very thin, homogeneous layer of chemical compounds and thus the application of several such layers by this method poses little or no problems. It is, e.g., possible to coat particles in a method according to this invention with a primer layer designed to help the adherence of the functional layer to the particles.
  • This primer layer can then, if desired receive a post-treatment as described above, and then the particles with the primer layer are further coated with a functional layer in a method according to this invention. Then, if desired, the particles with primer layer and functional layer can receive a post-treatment as described above.
  • the method according to the present invention is also very suited to coat particles for use in chromatography.
  • Carrier particles coated in a method of the present invention can be used to prepare multi-component developers for use in electrostatographic methods were an electrostatic latent image has to be developed, e.g., ionography, electrophotography as well as in electrostatographic methods were toner particles are directly imagewise applied to a final image receiving substrate as in Direct Electrostatic Printing, described in e.g. EP-A-675 417.
  • the carrier particles can be glass particles that have been coated in the method according to this invention, when the developer is used in magnetic brush development, the carrier particles contain magnetic material or are magnetic particles.
  • the method of this invention can be used to coat composite carriers (carrier wherein a magnetic pigment is incorporated in a matrix, this matrix being e.g. a resin, glass, etc...) as well as carriers composed of pure magnetic material.
  • magnetic material as well metal metaloxides, as any magnetisable material can be used, the metal and metal derivatives of metals typically selected from the group of Ca, Cr, Mn, Fe, Co, Ni, Cu, and Zn.
  • the method according to the present invention can be used for any type of coating, it can be used to coat polymers on the particles, e.g., addition polymers comprising styrene moieties, acrylic moieties, etc., addition polymers, e.g., polyesters, polyamides, polyimides etc., polymers comprising fluor containing moieties, silicon containing polymers, etc.
  • the method can as well be used to coat particles with mixtures of polymers.
  • the method of this invention can also be used to coat reactive mixtures on the particles, e.g., silicone polymers together with functional organosilanes as disclosed in US-A-4 977 054.
  • the method of this invention is very well suited for coating particles with a solution of chemical compounds that are selected from the group consisting of a monomeric, polyfunctional organosilane, a product of the hydrolysis of a monomeric, polyfunctional organosilane, a reaction product of a monomeric, polyfunctional organosilane and a organosilane containing an hetero-atom and a reaction product of a monomeric, polyfunctional organosilane and an alkoxide.
  • These compounds have been disclosed as carrier coating in the German Application 19721626.9 of May 23, 1997, titled coated particles, that is incorporated by reference.
  • a small laboratory equipment comprising a 2 l three-neck glass vessel, equipped with a mechanical stirrer, a condenser and an injection system for the coating solution.
  • the vessel is filled with 1 kg of ferrite powder, with a specific gravity of 5 g/cm 3 and a volume average particle size, determined by sieve analysis of 50 ⁇ m, thus giving a W avg -value of 3.3 10 -10 Kg.
  • 100 ml of coating solution containing 10 g of a styrene/acrylic copolymer in methylenechloride is added drop-wise over 60 minutes.
  • the product temperature (the temperature of the particles) is set at 45 °C, and a small underpressure is used to remove evaporated solvent.
  • the particles are stirred at 300 rpm.
  • the radius of the stirring blade being 5 cm.
  • This set-up is characterised by a Froude number equal to 5.
  • the temperature is risen to 75 °C for 2 hours to remove all solvent and harden the coating.
  • Visual inspection by microscope reveals high quality of the coating.
  • An electrophotographic developer was prepared by admixing 5% of toner. Good performance was observed in a copying device.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Developing Agents For Electrophotography (AREA)

Claims (9)

  1. Procédé de revêtement de particules porteuses, présentant un diamètre moyen en volume compris entre 20 et 200 µm, pour une utilisation dans des révélateurs électrostatiques, comprenant les étapes consistant à :
    amener lesdites particules porteuses à revêtir dans un récipient équipé de moyens permettant d'agiter lesdites particules porteuses, de façon à ce que lesdites particules porteuses occupent moins de 85% en volume dudit récipient, et à ce que l'agitation des particules porteuses soit décrites à l'aide d'un nombre de Froude compris entre 0,2 et 20,
    ajouter une solution contenant entre 6 et 60% en poids par rapport au volume total de ladite solution de composés chimiques pour le revêtement desdites particules porteuses dans un solvant ayant un point d'ébullition de A °C dans ledit récipient à un taux tel que, à tout moment, ledit solvant est présent en une quantité inférieure à 1,25 x 10-4 ml par cm2 de surface desdites particules porteuses à revêtir,
    conserver lesdites particules porteuses dans ledit récipient à une température d'au plus (A + 10) °C, et
    évacuer en continu ledit solvant.
  2. Procédé selon la revendication 1, dans lequel ledit nombre de Froude est compris entre 0,5 et 8, les deux limites comprises.
  3. Procédé selon la revendication 1 ou 2, dans lequel ladite solution contient entre 15 et 40% en poids par rapport au volume total de ladite solution de composés chimiques pour le revêtement desdites particules.
  4. Procédé selon l'une quelconque des revendications 1 à 3, dans lequel on ajoute ladite solution dans ledit récipient à un taux tel que, à tout moment, ledit solvant est présent en une quantité inférieure à 0,6 x 10-4 ml par cm2 de surface desdites particules à revêtir.
  5. Procédé selon l'une quelconque des revendications 1 à 4, dans lequel lesdites particules porteuses ont un poids moyen Mmoy tel que 1 x 10-11 kg ≤ Mmoy ≤ 5 x 10-8 kg.
  6. Procédé selon l'une quelconque des revendications 1 à 4, dans lequel lesdites particules porteuses ont un poids moyen Mmoy tel que 1 x 10-10 kg ≤ Mmoy ≤ 1 x 10-8 kg.
  7. Procédé selon l'une quelconque des revendications 1 à 6, dans lequel ledit récipient ayant un mélangeur mécanique est un mélangeur à socs de charrue.
  8. Procédé selon l'une quelconque des revendications 1 à 7, dans lequel lesdits composés chimiques sont choisis dans le groupe comprenant un organosilane polyfonctionnel monomère, un produit d'hydrolyse d'un organosilane polyfonctionnel monomère, un produit de réaction d'un organosilane polyfonctionnel monomère et un organosilane contenant un hétéroatome et un produit de réaction d'un organosilane polyfonctionnel monomère et d'un alcoolate.
  9. Procédé selon l'une quelconque des revendications précédentes, dans lequel lesdites particules porteuses comprennent un matériau magnétique.
EP19980202689 1997-08-20 1998-08-08 Procédé pour enrober des particules porteuses pour développateurs électrostatiques Expired - Lifetime EP0898206B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP19980202689 EP0898206B1 (fr) 1997-08-20 1998-08-08 Procédé pour enrober des particules porteuses pour développateurs électrostatiques

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP97202551 1997-08-20
EP97202551 1997-08-20
EP19980202689 EP0898206B1 (fr) 1997-08-20 1998-08-08 Procédé pour enrober des particules porteuses pour développateurs électrostatiques

Publications (3)

Publication Number Publication Date
EP0898206A2 EP0898206A2 (fr) 1999-02-24
EP0898206A3 EP0898206A3 (fr) 1999-03-17
EP0898206B1 true EP0898206B1 (fr) 2003-02-19

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EP19980202689 Expired - Lifetime EP0898206B1 (fr) 1997-08-20 1998-08-08 Procédé pour enrober des particules porteuses pour développateurs électrostatiques

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6420029B1 (en) 1998-11-26 2002-07-16 Xeikon International Hybrid carrier coating containing a silane network and a polymeric compound not containing silicon atoms
US6551754B2 (en) 2000-04-11 2003-04-22 Xeikon, N.V. Method for coating carrier particles
EP1146398A3 (fr) * 2000-04-11 2003-04-09 Xeikon Nv Procédé de revêtement de particules d' agent de véhiculation

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3507686A (en) * 1967-06-23 1970-04-21 Xerox Corp Method of coating carrier beads
US3947271A (en) * 1972-02-14 1976-03-30 International Business Machines Corporation Electrostatic imaging method using a polytetrafluoroethylene coated carrier particle
US4297427A (en) * 1978-01-26 1981-10-27 Xerox Corporation Polyblend coated carrier materials
US5102769A (en) * 1991-02-04 1992-04-07 Xerox Corporation Solution coated carrier particles
US5340677A (en) * 1991-04-26 1994-08-23 Canon Kabushiki Kaisha Carrier for electrophotography, two-component type developer for electrostatic images, process for producing carrier for electrophotography, and image forming method

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Publication number Publication date
EP0898206A2 (fr) 1999-02-24
EP0898206A3 (fr) 1999-03-17

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