WO2015129448A1 - 静電荷像現像用トナー - Google Patents
静電荷像現像用トナー Download PDFInfo
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- WO2015129448A1 WO2015129448A1 PCT/JP2015/053621 JP2015053621W WO2015129448A1 WO 2015129448 A1 WO2015129448 A1 WO 2015129448A1 JP 2015053621 W JP2015053621 W JP 2015053621W WO 2015129448 A1 WO2015129448 A1 WO 2015129448A1
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- toner
- resin
- shell layer
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- 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
- G03G9/093—Encapsulated toner particles
- G03G9/09307—Encapsulated toner particles specified by the shell material
- G03G9/09314—Macromolecular compounds
- G03G9/09328—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
- G03G9/0819—Developers with toner particles characterised by the dimensions of the particles
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- 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
- G03G9/0821—Developers with toner particles characterised by physical parameters
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- 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
- G03G9/0825—Developers with toner particles characterised by their structure; characterised by non-homogenuous distribution of components
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- 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
- G03G9/087—Binders for toner particles
- G03G9/08784—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775
- G03G9/08795—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775 characterised by their chemical properties, e.g. acidity, molecular weight, sensitivity to reactants
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- 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
- G03G9/087—Binders for toner particles
- G03G9/08784—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775
- G03G9/08797—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775 characterised by their physical properties, e.g. viscosity, solubility, melting temperature, softening temperature, glass transition temperature
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- 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
- G03G9/09—Colouring agents for toner particles
- G03G9/0906—Organic dyes
- G03G9/0918—Phthalocyanine dyes
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- 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
- G03G9/093—Encapsulated toner particles
- G03G9/0935—Encapsulated toner particles specified by the core material
- G03G9/09357—Macromolecular compounds
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- 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
- G03G9/093—Encapsulated toner particles
- G03G9/0935—Encapsulated toner particles specified by the core material
- G03G9/09357—Macromolecular compounds
- G03G9/09371—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
- G03G9/093—Encapsulated toner particles
- G03G9/09392—Preparation thereof
Definitions
- the present invention relates to an electrostatic image developing toner.
- toner for developing an electrostatic charge image is fixed on a recording medium such as paper by heating and pressing using a fixing roller.
- a toner for developing an electrostatic image having excellent low-temperature fixability that can be fixed at a lower temperature is required.
- a binder resin having a low softening point (Tm) and a glass transition point (Tg) and a release agent having a low softening point are used.
- the electrostatic image developing toner when the electrostatic image developing toner is stored at a high temperature, there may be a problem that the toner particles contained in the electrostatic image developing toner tend to aggregate. Since the charge amount of the aggregated toner tends to be lower than the charge amount of the non-aggregated toner, the aggregated toner is easily developed unnecessarily. As a result, image defects may occur.
- the electrostatic image developing toner includes a plurality of toner particles.
- Each toner particle is generally obtained through a mixing process, a kneading process, a pulverizing process, and a classification process in which components such as a release agent, a colorant, a charge control agent, and a magnetic powder are mixed with a binder resin. It is done.
- the present invention has been made in view of the above problems, and provides an electrostatic image developing toner excellent in both low-temperature fixability and toner blocking properties.
- the electrostatic image developing toner of the present invention contains a plurality of toner particles.
- Each of the plurality of toner particles includes a toner core and a shell layer that covers the toner core.
- the shell layer includes a thermosetting resin.
- the content of the tetrahydrofuran insolubles in the toner is 90% by mass or more based on the mass of the toner.
- the toner has a melt viscosity at 75 ° C. of 1.0 ⁇ 10 4 Pa ⁇ s to 1.0 ⁇ 10 5 Pa ⁇ s.
- the present invention it is possible to provide a toner for developing an electrostatic image that is excellent in both low-temperature fixing property and toner blocking property.
- the electrostatic image developing toner according to the exemplary embodiment includes a plurality of toner particles.
- Each of the plurality of toner particles is composed of toner base particles and an optional external additive.
- the toner base particles are composed of a toner core and a shell layer. The surface of the toner core is covered with a shell layer.
- the toner core can include, for example, a binder resin.
- the toner core may contain an optional component (for example, a release agent, a colorant, a charge control agent, and / or a magnetic powder) in addition to the binder resin as necessary.
- an optional component for example, a release agent, a colorant, a charge control agent, and / or a magnetic powder
- the binder resin contained in the toner core is not particularly limited as long as it is a binder resin for toner.
- the binder resin include styrene resin, acrylic resin, styrene- (meth) acrylic resin, polyethylene resin, polypropylene resin, vinyl chloride resin, polyester resin, polyamide resin, urethane resin, and polyvinyl alcohol.
- thermoplastic resins such as resins, vinyl ether resins, N-vinyl resins, or styrene-butadiene resins.
- thermoplastic resins from the viewpoint of improving the dispersibility of the colorant in the toner, the charging property of the toner, or the fixing property of the toner to the recording medium, a styrene- (meth) acrylic resin or polyester Resins are preferred.
- a styrene- (meth) acrylic resin or the polyester resin will be described.
- acrylic and methacryl may be collectively referred to as “(meth) acryl”.
- the styrene- (meth) acrylic resin is a copolymer of a styrene monomer and a (meth) acrylic monomer.
- examples of the styrene monomer include styrene, ⁇ -methylstyrene, vinyl toluene, ⁇ -chlorostyrene, o-chlorostyrene, m-chlorostyrene, p-chlorostyrene, and p-ethylstyrene.
- (meth) acrylic monomers examples include methyl acrylate, ethyl acrylate, n-propyl acrylate, iso-propyl acrylate, n-butyl acrylate, iso-butyl acrylate, 2-ethylhexyl acrylate, and methacrylic acid.
- (meth) acrylic acid alkyl esters such as methyl acid, ethyl methacrylate, n-butyl methacrylate, or iso-butyl methacrylate.
- the polyester resin can be obtained, for example, by polycondensation or copolycondensation of a divalent or trivalent or higher alcohol component and a divalent or trivalent or higher carboxylic acid component.
- examples of the components used when synthesizing the polyester resin include the following divalent or trivalent or higher alcohol components and divalent or trivalent or higher carboxylic acid components.
- divalent alcohol component examples include diols or bisphenols.
- diol examples include ethylene glycol, diethylene glycol, triethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, neopentyl glycol, 1,4-butenediol, 1, Examples include 5-pentanediol, 1,6-hexanediol, 1,4-cyclohexanedimethanol, dipropylene glycol, polyethylene glycol, polypropylene glycol, or polytetramethylene glycol.
- bisphenols include bisphenol A, hydrogenated bisphenol A, polyoxyethylenated bisphenol A, and polyoxypropylenated bisphenol A.
- trivalent or higher alcohol component include sorbitol, 1,2,3,6-hexanetetrol, 1,4-sorbitan, pentaerythritol, dipentaerythritol, tripentaerythritol, 1,2,4-butanetriol. 1,2,5-pentanetriol, glycerol, diglycerol, 2-methylpropanetriol, 2-methyl-1,2,4-butanetriol, trimethylolethane, trimethylolpropane, or 1,3,5-triol Hydroxymethylbenzene is mentioned.
- divalent carboxylic acid component examples include maleic acid, fumaric acid, citraconic acid, itaconic acid, glutaconic acid, phthalic acid, isophthalic acid, terephthalic acid, cyclohexanedicarboxylic acid, succinic acid, alkyl succinic acid, alkenyl succinic acid, Examples include adipic acid, sebacic acid, azelaic acid, or malonic acid.
- alkyl succinic acid examples include n-butyl succinic acid, isobutyl succinic acid, n-octyl succinic acid, n-dodecyl succinic acid, and isododecyl succinic acid.
- alkenyl succinic acid examples include n-butenyl succinic acid, isobutenyl succinic acid, n-octenyl succinic acid, n-dodecenyl succinic acid, and isododecenyl succinic acid.
- Examples of the trivalent or higher carboxylic acid component include 1,2,4-benzenetricarboxylic acid (for example, trimellitic acid), 1,2,5-benzenetricarboxylic acid, 2,5,7-naphthalenetricarboxylic acid, , 2,4-naphthalenetricarboxylic acid, 1,2,4-butanetricarboxylic acid, 1,2,5-hexanetricarboxylic acid, 1,3-dicarboxyl-2-methyl-2-methylenecarboxypropane, 1,2, Examples include 4-cyclohexanetricarboxylic acid, tetra (methylenecarboxyl) methane, 1,2,7,8-octanetetracarboxylic acid, pyromellitic acid, or empole trimer acid.
- 1,2,4-benzenetricarboxylic acid for example, trimellitic acid
- 1,2,5-benzenetricarboxylic acid 2,5,7-naphthalenetricarboxylic acid
- divalent or trivalent or higher carboxylic acid components may be used by transforming them into ester-forming derivatives such as acid halides, acid anhydrides, or lower alkyl esters.
- ester-forming derivatives such as acid halides, acid anhydrides, or lower alkyl esters.
- lower alkyl means an alkyl group having 1 to 6 carbon atoms.
- the softening point (Tm) of the binder resin is preferably 85 ° C. or higher and 95 ° C. or lower.
- the glass transition point (Tg) of the binder resin is preferably 50 ° C. or higher and 65 ° C. or lower, and more preferably 50 ° C. or higher and 60 ° C. or lower.
- the toner core may contain a release agent as necessary.
- the release agent is generally used for the purpose of improving the low-temperature fixability and offset resistance of the toner.
- the type of the release agent is not particularly limited as long as it is a release agent used as a known release agent for toner.
- Suitable release agents include, for example, aliphatic hydrocarbon waxes (eg, low molecular weight polyethylene, low molecular weight polypropylene, polyolefin copolymer, polyolefin wax, microcrystalline wax, paraffin wax, or Fischer-Tropsch wax), aliphatic Oxides of hydrocarbon wax (eg, oxidized polyethylene wax or block copolymer of oxidized polyethylene wax), plant wax (eg, candelilla wax, carnauba wax, wood wax, jojoba wax, or rice wax), animal Waxes (eg, beeswax, lanolin, or whale wax), mineral waxes (eg, ozokerite, ceresin, or petrolatum), waxes based on fatty acid esters (eg, montanate ester wax) Box, or castor wax), or wax deoxidizing a part or the whole of fatty esters (e.g., deoxidized carnauba wax) and the like.
- hydrocarbon waxes
- the amount of the release agent used is preferably 1 part by mass or more and 30 parts by mass or less, and more preferably 5 parts by mass or more and 20 parts by mass or less with respect to 100 parts by mass of the binder resin.
- the toner core may contain a colorant as necessary.
- a colorant known pigments and dyes can be used according to the color of the toner particles.
- suitable colorants include the following colorants.
- black colorants include carbon black.
- a colorant that is toned to black using a colorant such as a yellow colorant, a magenta colorant, and a cyan colorant, which will be described later, can also be used.
- examples of the colorant blended in the toner core include a yellow colorant, a magenta colorant, and a cyan colorant.
- yellow colorant examples include condensed azo compounds, isoindolinone compounds, anthraquinone compounds, azo metal complexes, methine compounds, and arylamide compounds.
- C.I. I. Pigment Yellow (3, 12, 13, 14, 15, 17, 62, 74, 83, 93, 94, 95, 97, 109, 110, 111, 120, 127, 128, 129, 147, 151, 154, 155 168, 174, 175, 176, 180, 181, 191 or 194)
- Neftol Yellow S Hansa Yellow G
- C.I. I. Bat yellow is mentioned.
- magenta colorant examples include condensed azo compounds, diketopyrrolopyrrole compounds, anthraquinone compounds, quinacridone compounds, basic dye lake compounds, naphthol compounds, benzimidazolone compounds, thioindigo compounds, and perylene compounds.
- cyan colorant examples include copper phthalocyanine compounds, copper phthalocyanine derivatives, anthraquinone compounds, and basic dye lake compounds. Specifically, C.I. I. Pigment blue (1, 7, 15, 15: 1, 15: 2, 15: 3, 15: 4, 60, 62, or 66), phthalocyanine blue, C.I. I. Bat Blue, or C.I. I. Acid blue.
- the amount of the colorant used is preferably 1 part by mass or more and 20 parts by mass or less, and more preferably 3 parts by mass or more and 10 parts by mass or less with respect to 100 parts by mass of the binder resin.
- the toner core may contain a negatively chargeable charge control agent.
- a charge control agent is used for the purpose of improving the charge stability or charge rising property of the toner and obtaining a toner having excellent durability or stability.
- the charge rising characteristic of the toner is an index as to whether or not the toner can be charged to a predetermined charge level in a short time.
- the toner core may contain magnetic powder as necessary.
- Suitable magnetic powders include, for example, ferrite, magnetite, iron, ferromagnetic metals (cobalt and nickel), alloys (iron and / or alloys containing ferromagnetic metals), compounds (iron and / or ferromagnetic metals) Compound), a ferromagnetic alloy (a ferromagnetic alloy subjected to ferromagnetization treatment such as heat treatment), or chromium dioxide.
- the average particle size of the magnetic powder is preferably 0.1 ⁇ m or more and 1.0 ⁇ m or less, and more preferably 0.1 ⁇ m or more and 0.5 ⁇ m or less. When the average particle diameter of the magnetic powder is within such a range, it is easy to uniformly disperse the magnetic powder in the binder resin.
- the amount of magnetic powder used is preferably 35 parts by weight or more and 60 parts by weight or less, and 40 parts by weight or more and 60 parts by weight or less with respect to 100 parts by weight of the total amount of toner when the electrostatic image developing toner is used as a one-component developer. It is more preferable that the amount is not more than part by mass.
- the shell layer covers the surface of the toner core. Below, the component contained in a shell layer is demonstrated.
- the resin constituting the shell layer contains a thermosetting resin in order to improve the strength. It is preferable that the resin constituting the shell layer has a sufficient cationic property (positive chargeability).
- thermosetting resin examples include a thermosetting resin having a cationic property (positive charging property) or a thermosetting resin having a nitrogen atom in a molecular skeleton.
- thermosetting resin having a cationic property (positive charging property) examples include a thermosetting resin having an amino group (—NH 2 ).
- thermosetting resins having an amino group include melamine resins, melamine resin derivatives, guanamine resins, guanamine resin derivatives (for example, benzoguanamine resins, acetoguanamine resins, or spiroguanamine resins), sulfonamide resins, urea resins.
- derivatives of urea resin eg, glyoxal resin
- aniline resin examples include a thermosetting resin having a cationic property (positive charging property) or a thermosetting resin having a nitrogen atom in a molecular skeleton.
- thermosetting resin having a cationic property (positive charging property) examples include a thermosetting resin having an
- thermosetting resin having a nitrogen atom in the molecular skeleton a thermosetting polyimide resin (for example, a maleimide polymer, a bismaleimide polymer, an amino bismaleimide polymer, or a bismaleimide triazine copolymer) is used. ).
- a thermosetting resin may be used individually by 1 type, and may be used in combination of 2 or more type.
- thermosetting resin melamine resin or urea resin is preferable.
- Melamine resin is a polycondensate of melamine and formaldehyde.
- the monomer used to form the melamine resin is melamine.
- Urea resin is a polycondensate of urea and formaldehyde.
- the monomer used to form the urea resin is urea.
- Glyoxal resin which is a derivative of urea resin, is a polycondensate of a reaction product of glyoxal and urea with formaldehyde.
- the monomer used to form the glioxal resin is the reaction product of glyoxal and urea.
- the urea that reacts with melamine, urea, and glyoxal may undergo known modification.
- the monomer of the thermosetting resin can be used by being transformed into a derivative by methylolation with formaldehyde before reacting with the thermoplastic resin.
- melamine can be transformed into methylolmelamine by use of formaldehyde to form methylol.
- the monomer of the thermosetting resin (for example, a reaction product of melamine, urea, or glyoxal and urea) may be used in the form of a prepolymer.
- the prepolymer of the thermosetting resin is a state before the polymer in which the degree of polymerization of the monomer of the thermosetting resin is increased to some extent.
- the prepolymer of the thermosetting resin is also referred to as an initial polymer or an initial condensate.
- the shell layer preferably contains nitrogen atoms derived from melamine resin or urea resin. Materials containing nitrogen atoms are easily positively charged. Therefore, the content of nitrogen atoms in the shell layer is preferably 10% by mass or more with respect to the mass of the shell layer.
- the film thickness of the shell layer is preferably 1 nm or more and 20 nm or less, and more preferably 1 nm or more and 10 nm or less.
- the shell layer is easily broken by heating and pressurization when fixing the toner to the recording medium.
- the binder resin contained in the toner core softens and melts rapidly, and the toner can be fixed on the recording medium in a low temperature range.
- the charge amount of the toner particles does not become too high, an image is properly formed.
- the thickness of the shell layer is 1 nm or more, the shell layer has sufficient strength, and the shell layer is prevented from being broken by an impact during transportation.
- the component of the release agent easily oozes out on the surface of the toner particles through the portion where the shell layer is broken under a high temperature condition. For this reason, when the toner is stored under high temperature conditions, the toner particles tend to aggregate. Furthermore, since the charge amount of the toner particles does not become too low when the thickness of the shell layer is 1 nm or more, it is possible to suppress the occurrence of image defects in the formed image.
- the film thickness of the shell layer can be measured by analyzing a TEM image of the cross section of the toner particles using commercially available image analysis software (for example, “WinROOF” manufactured by Mitani Corporation).
- the toner particles may have a structure in which a plurality of shell layers are formed on the surface of the toner core.
- the shell layer formed on the outermost part of the toner core is preferably cationic.
- the shell layer has a cationic property (positive charging property). Therefore, a positively chargeable charge control agent may be included in the shell layer.
- the toner particles may contain an external additive.
- an external additive can be attached to the surface of the toner base particles.
- the surface of the shell layer may be externally treated with, for example, an external additive in order to improve the fluidity and handleability of the toner particles.
- an external additive for example, a known external addition method is used.
- the toner base particles are adjusted by adjusting the external addition conditions so that the external additive is not buried in the shell layer, and using a mixer (for example, FM mixer or Nauter mixer (registered trademark)) Externally added.
- a mixer for example, FM mixer or Nauter mixer (registered trademark)
- the type of external additive can be appropriately selected from external additives for toner.
- the external additive include silica or metal oxide (alumina, titanium oxide, magnesium oxide, zinc oxide, strontium titanate, or barium titanate). These external additives may be used individually by 1 type, and may be used in combination of 2 or more type.
- the external additive can be hydrophobized using an aminosilane coupling agent or a hydrophobizing agent such as silicone oil.
- a hydrophobized external additive it is possible to suppress a decrease in the charge amount of the toner under high temperature and high humidity, and to improve the fluidity of the toner.
- the addition amount of the external additive is preferably 0.1 parts by mass or more and 10 parts by mass or less, and more preferably 0.2 parts by mass or more and 5 parts by mass or less with respect to 100 parts by mass of the toner base particles. .
- the average particle diameter of the external additive is preferably 0.01 ⁇ m or more and 1.0 ⁇ m or less. When the added amount of the external additive and the average particle diameter are within such ranges, the fluidity and handling properties of the toner particles can be improved.
- thermosetting resin contained in the shell layer As an index of the degree of cross-linking of the thermosetting resin contained in the shell layer, there is a content ratio of insoluble content of toner particles in tetrahydrofuran. When the degree of crosslinking of the thermosetting resin contained in the shell layer is sufficient, the toner particles are hardly dissolved in tetrahydrofuran. A method for measuring the content ratio of the toner insoluble matter in the toner will be described below.
- An electrostatic charge image developing toner (mass: W 1 ) is added to tetrahydrofuran (THF).
- THF tetrahydrofuran
- the slurry is stirred to dissolve a THF-soluble component (resin mass: W 2 ) in THF. Thereafter, components dissolved in THF are extracted from the slurry.
- the content ratio of the toner insoluble matter in the toner was calculated.
- Content of THF-insoluble matter (mass%) (W 1 ⁇ W 2 ) / W 1 ⁇ 100
- the content ratio of the toner insoluble matter in the toner is preferably 90% by mass or more with respect to the mass of the toner.
- melt viscosity of the electrostatic image developing toner is measured using a Koka flow tester. Specifically, the melt viscosity of the toner is measured as follows. Mold the toner into pellets. The pellet is set in a Koka type flow tester, heated to 200 ° C. while applying a load with a plunger, the pellet-like toner is extruded from a nozzle, and the melt viscosity of the toner at 75 ° C. is measured. .
- the melt viscosity at 75 ° C. of the toner is 1.0 ⁇ 10 4 Pa ⁇ s or more and 1.0 ⁇ 10 5 Pa ⁇ s or less.
- the melt viscosity of the toner is within such a range, the low-temperature fixability of the toner can be improved.
- the method for producing a toner for developing an electrostatic charge image can include, for example, a toner core preparation step and a shell layer formation step.
- a toner core preparation step a toner core is prepared.
- a shell layer is formed on the surface of the toner core.
- the toner core preparation process includes an aggregation process and a coalescence process.
- the aggregation step one or more kinds of fine particles containing one or more components selected from a binder resin, a colorant, and a release agent are aggregated in an aqueous medium to form aggregated particles.
- the coalescence process the components contained in the aggregated particles obtained in the aggregation process are heat-processed and coalesced.
- an external additive is attached to the surface of the toner base particles.
- Toner core preparation process In order to execute the toner core preparation step, an optional component (for example, a release agent, a colorant, a charge control agent, and / or a magnetic powder) can be satisfactorily dispersed in the binder resin as necessary. Is used.
- a release agent for example, a release agent, a colorant, a charge control agent, and / or a magnetic powder
- a method for executing the toner core preparation step an aggregation method is exemplified.
- the coagulation process and the coalescence process are performed.
- a toner core is prepared using an agglomeration method, toner particles having a uniform shape and uniform particle diameter can be obtained.
- the aggregating step fine particles containing the components constituting the toner core are aggregated in an aqueous medium to form aggregated particles.
- the components contained in the aggregated particles obtained in the aggregation step are united in an aqueous medium to obtain a toner core.
- aggregated particles are prepared.
- fine particles containing a component constituting the toner core are obtained by finely forming a binder resin or a composition containing the binder resin in an aqueous medium into a desired particle size, thereby including fine particles containing the binder resin (binder resin fine particles).
- binder resin fine particles Is prepared as a binder resin fine particle dispersion in which is dispersed in an aqueous medium.
- the dispersion of the binder resin fine particles includes an aqueous dispersion (for example, a colorant fine particle dispersion or a release agent fine particle dispersion) of fine particles of an optional component (for example, a release agent or a colorant) other than the binder resin. But you can.
- the particles are aggregated in such a binder resin particle dispersion to obtain aggregated particles.
- Preparation method 1 a preparation method of the binder resin fine particle dispersion
- preparation method 2 a preparation method of the release agent fine particle dispersion
- preparation method 3 a preparation method of the colorant fine particle dispersion
- the binder resin is pulverized using a pulverizer (for example, a turbo mill) to obtain a pulverized product.
- the obtained pulverized product is dispersed in an aqueous medium such as ion-exchanged water, heated, and then subjected to a high shearing force using a high-speed shearing emulsifier (for example, “Cleamix (registered trademark)” manufactured by M Technique Co., Ltd.).
- a dispersion containing binder resin fine particles can be obtained.
- the heating temperature is preferably a temperature that is 10 ° C. higher than the softening point (Tm) of the binder resin (a temperature up to about 200 ° C. at the highest).
- the average particle diameter of the binder resin fine particles is preferably 1 ⁇ m or less, and more preferably 0.05 ⁇ m or more and 0.50 ⁇ m or less. When the average particle size of the binder resin fine particles is within such a range, the particle size distribution of the toner core is sharp and the shape of the toner core is uniform.
- the average particle size of the binder resin fine particles can be measured using a laser diffraction particle size distribution measuring device (for example, “SALD-2200” manufactured by Shimadzu Corporation).
- the dispersion containing the binder resin fine particles may contain a surfactant.
- the surfactant is used, the binder resin fine particles are stably and uniformly dispersed in the aqueous medium.
- the specific surface area of the binder resin increases if the binder resin is directly atomized in an aqueous medium. Therefore, when the acidic groups exposed on the surface of the binder resin fine particles increase, the pH of the aqueous medium may be lowered from about 3 to about pH 4. When the pH of the aqueous medium is lowered from about 3 to about pH 4, the binder resin may be hydrolyzed, or the particle diameter of the binder resin fine particles may not be reduced to a desired particle diameter.
- a basic substance may be added to the aqueous medium.
- any basic substance may be added as long as it is a basic substance capable of suppressing the above-mentioned problems.
- the basic substance include alkali metal hydroxide (sodium hydroxide, potassium hydroxide, or lithium hydroxide), alkali metal carbonate (sodium carbonate or potassium carbonate), alkali metal hydrogen carbonate (sodium bicarbonate).
- nitrogen-containing basic organic compound N, N-dimethylethanolamine, N, N-diethylethanolamine, triethanolamine, tripropanolamine, tributanolamine, triethylamine, n-propylamine, n-butylamine, isopropylamine, monomethanolamine, morpholine, methoxypropylamine, pyridine, or vinylpyridine).
- the surfactant examples include an anionic surfactant, a cationic surfactant, and a nonionic surfactant.
- examples of the anionic surfactant include sulfate ester type surfactants, sulfonate type surfactants, phosphate ester type surfactants, and soaps.
- Examples of the cationic surfactant include amine salt type surfactants and quaternary ammonium salt type surfactants.
- Nonionic surfactants include, for example, polyethylene glycol type surfactants, alkylphenol ethylene oxide adduct type surfactants, or polyhydric alcohol type surfactants (polyhydric alcohol derivatives such as glycerin, sorbitol, or sorbitan). ).
- anionic surfactants are preferable. These surfactants may be used individually by 1 type, and may be used in combination of 2 or more type.
- the amount of the surfactant used is preferably 0.01% by mass or more and 10% by mass or less based on the mass of the binder resin. When the amount of the surfactant used is within such a range, the dispersibility of the binder resin fine particles in the aqueous dispersion can be improved.
- the preparation method 2 will be described below.
- the release agent is pulverized in advance to an average particle size of 100 ⁇ m or less to obtain a release agent powder.
- the obtained release agent powder is added to an aqueous medium to prepare a slurry.
- the aqueous medium contains a surfactant in advance.
- the amount of the surfactant used is preferably 0.01% by mass or more and 10% by mass or less with respect to the mass of the release agent. When the amount of the surfactant used is within such a range, the dispersibility of the release agent fine particles in the aqueous dispersion can be improved.
- the slurry is heated to a temperature equal to or higher than the melting point of the release agent.
- a disperser such as a homogenizer (for example, “Ultra Turrax T50” manufactured by IKA Co., Ltd.) or a pressure discharge type disperser to the heated slurry.
- a disperser such as a homogenizer (for example, “Ultra Turrax T50” manufactured by IKA Co., Ltd.) or a pressure discharge type disperser to the heated slurry.
- a disperser such as a homogenizer (for example, “Ultra Turrax T50” manufactured by IKA Co., Ltd.) or a pressure discharge type disperser to the heated slurry.
- a disperser such as a homogenizer (for example, “Ultra Turrax T50” manufactured by IKA Co., Ltd.) or a pressure discharge type disperser to the heated slurry.
- a disperser such as a homogenizer (for example, “
- Examples of the device that gives a strong shearing force to the dispersion include NANO3000 (manufactured by Miki Co., Ltd.), Nanomizer (manufactured by Yoshida Kikai Kogyo Co., Ltd.), Microfullizer (registered trademark) (manufactured by Microfluidics), Gorin type A homogenizer (manufactured by SPX) or Claremix (registered trademark) W motion (manufactured by M Technique Co., Ltd.) may be mentioned.
- NANO3000 manufactured by Miki Co., Ltd.
- Nanomizer manufactured by Yoshida Kikai Kogyo Co., Ltd.
- Microfullizer registered trademark
- Gorin type A homogenizer manufactured by SPX
- Claremix registered trademark
- W motion manufactured by M Technique Co., Ltd.
- the average particle diameter of the release agent fine particles contained in the release agent fine particle dispersion is preferably 1 ⁇ m or less, more preferably 0.1 ⁇ m or more and 0.7 ⁇ m or less, and 0.28 ⁇ m or more and 0.55 ⁇ m. It is particularly preferred that When the average particle diameter of the release agent fine particles is within such a range, the release agent is uniformly dispersed in the binder resin.
- the average particle size of the release agent fine particles can be measured by the same method as the average particle size of the binder resin fine particles.
- a colorant and components such as a dispersant containing a colorant are dispersed by using a known disperser.
- a aqueous dispersion containing colorant fine particles (dispersion of colorant fine particles) is prepared.
- the surfactant as the dispersant the surfactant used in the preparation of the binder resin fine particles can be used.
- the amount of the surfactant used is preferably 0.01 parts by mass or more and 10 parts by mass or less with respect to 100 parts by mass of the colorant. When the amount of the surfactant used is within such a range, the dispersibility of the colorant fine particles in the aqueous dispersion can be improved.
- Examples of the disperser used for the dispersion treatment include a pressure disperser and a medium disperser.
- Examples of the pressure disperser include a mechanical homogenizer, a gorin homogenizer, a pressure homogenizer, and a high-pressure homogenizer (manufactured by Yoshida Kikai Kogyo Co., Ltd.).
- Examples of the medium type disperser include a sand grinder, a horizontal or vertical bead mill, an ultra apex mill (manufactured by Kotobuki Industries Co., Ltd.), a dyno (registered trademark) mill (manufactured by WAB Co., Ltd.), or an MSC mill (Nippon Coke Kogyo Co., Ltd.). Manufactured).
- Examples of the disperser other than the above include an ultrasonic disperser.
- the average particle diameter of the colorant fine particles is preferably 0.01 ⁇ m or more and 0.2 ⁇ m or less. When the average particle diameter of the colorant fine particles is within such a range, the colorant is uniformly dispersed in the binder resin.
- the average particle size of the colorant fine particles can be measured by the same method as the average particle size of the binder resin fine particles.
- the prepared binder resin fine particle dispersion is appropriately combined with the release agent fine particle dispersion and / or the colorant fine particle dispersion so that the predetermined component is contained in the toner core. And mix. Subsequently, these fine particles are aggregated in the mixed dispersion to obtain an aqueous dispersion containing aggregated particles containing the binder resin.
- Examples of the flocculant include inorganic metal salts, inorganic ammonium salts, and bivalent or higher-valent metal complexes.
- examples of inorganic metal salts include metal salts (sodium sulfate, sodium chloride, calcium chloride, calcium nitrate, barium chloride, magnesium chloride, zinc chloride, aluminum chloride, or aluminum sulfate), or inorganic metal salt polymers (polyaluminum chloride). Or polyaluminum hydroxide).
- Examples of the inorganic ammonium salt include ammonium sulfate, ammonium chloride, and ammonium nitrate.
- a quaternary ammonium salt type cationic surfactant or a nitrogen-containing compound for example, polyethyleneimine
- a nitrogen-containing compound for example, polyethyleneimine
- a divalent metal salt or a monovalent metal salt can be used as the flocculant.
- These flocculants may be used individually by 1 type, and may be used in combination of 2 or more type.
- the pH of the aqueous dispersion when adding the aggregating agent is adjusted to be 8 or more alkaline.
- the flocculant may be added at once or sequentially.
- the amount of the flocculant added is preferably 1 part by mass or more and 50 parts by mass or less with respect to 100 parts by mass of the solid content of the aqueous dispersion.
- the addition amount of the flocculant can be appropriately adjusted according to the type and amount of the dispersant contained in the fine particle dispersion.
- the temperature of the aqueous dispersion when the fine particles are aggregated is preferably in the temperature range of the glass transition point (Tg) of the binder resin or more and less than 10 ° C. of the binder resin.
- Tg glass transition point
- the temperature of the aqueous dispersion is within such a range, aggregation of fine particles contained in the aqueous dispersion can be favorably progressed.
- An aggregation stopper may be added after the aggregation has progressed until the aggregated particles have a desired average particle size.
- Examples of the aggregation terminator include sodium chloride, potassium chloride, or magnesium chloride. These aggregation terminators may be used individually by 1 type, and may be used in combination of 2 or more type.
- the components contained in the aggregated particles obtained in the aggregation process are integrated in an aqueous medium to form a toner core.
- the aqueous dispersion containing the aggregated particles obtained by the aggregation process may be heated. Thereby, an aqueous dispersion containing a toner core can be obtained.
- the heating temperature of the aqueous dispersion containing aggregated particles is preferably within the temperature range of the glass transition point (Tg) of the binder resin + 10 ° C. or higher and the melting point of the binder resin or lower.
- Tg glass transition point
- the heating temperature of the aqueous dispersion containing aggregated particles is within such a temperature range, the coalescence of the components contained in the aggregated particles can be favorably advanced.
- the aqueous dispersion containing the toner core after the coalescence process may be subjected to a washing process and a drying process as necessary.
- the toner core obtained by the aggregation method is washed with water.
- the washing method include a method of recovering a wet cake containing a toner core from a dispersion containing a toner core by solid-liquid separation, and washing the collected wet cake with water.
- the toner core in the aqueous dispersion containing the toner core is precipitated, the supernatant liquid is replaced with water, and the toner core is redispersed in water after the replacement.
- the toner core that has undergone the cleaning process is dried.
- the dryer used in the drying step include a spray dryer, a fluidized bed dryer, a vacuum freeze dryer, and a vacuum dryer.
- the shell layer forming step includes a supply step and a resinification step.
- a shell layer forming solution containing a monomer and / or a prepolymer of a thermosetting resin is supplied to the surface of the toner core.
- the resinification step is a step of polymerizing or condensing a thermosetting resin monomer and / or prepolymer contained in the shell layer forming solution.
- Examples of the method of supplying the shell layer forming solution to the toner core include a method of spraying the shell layer forming solution on the surface of the toner core, or a method of immersing the toner core in the shell layer forming solution.
- a dispersant may be added to the shell layer forming solution.
- dispersant examples include sodium polyacrylate, polyparavinylphenol, partially saponified polyvinyl acetate, isoprene sulfonic acid, polyether, isobutylene / maleic anhydride copolymer, sodium polyaspartate, starch, gum arabic, Examples include polyvinyl pyrrolidone or sodium lignin sulfonate. These dispersing agents may be used individually by 1 type, and may be used in combination of 2 or more type.
- a solvent for example, a solvent, a thermosetting resin monomer and / or prepolymer, and other additives (for example, a dispersant described later) are mixed by stirring. do it.
- the solvent include toluene, acetone, methyl ethyl ketone, tetrahydrofuran, methanol, ethanol, or water.
- the solution for forming the shell layer may contain a known dispersant in order to improve the dispersibility of the thermosetting resin monomer and / or prepolymer in the solvent.
- the content of the dispersant in the shell layer forming solution is preferably 0.1 parts by mass or more and 15 parts by mass or less with respect to 100 parts by mass of the shell layer forming solution.
- the content of the dispersant in the shell layer forming solution is 0.1 parts by mass or more with respect to 100 parts by mass of the shell layer forming solution, the dispersibility of the toner particles can be improved.
- the content of the dispersant in the shell layer forming solution is 15 parts by mass or less with respect to 100 parts by mass of the shell layer forming solution, the environmental load due to the amount of the dispersant used can be reduced.
- the dispersant remaining in the toner can be removed by a cleaning process.
- thermosetting resin monomer and / or prepolymer have a sufficiently high degree of polymerization, but also the degree of polymerization of the thermosetting resin monomer and / or prepolymer is moderate. This includes partial resinization.
- thermosetting resin in the resinification step examples include an in-situ polymerization method, a submerged curing coating method, and a coacervation method. From the viewpoint of the reactivity of the thermosetting resin, a uniformly coated shell layer can be obtained by the in-situ polymerization method.
- the in-situ polymerization method there is a resin raw material that forms a shell layer only in an aqueous medium, and this raw material reacts on the surface of the toner core to form a resin, thereby forming a shell layer.
- the temperature at the time of forming the shell layer is preferably 60 ° C. or higher and 70 ° C. or lower.
- the temperature at the time of forming the shell layer is preferably 60 ° C. or higher and 70 ° C. or lower.
- the temperature rising rate for raising the temperature to the temperature at which the shell layer is formed is 1 ° C./min to 3 ° C./min. If the heating rate is too high, polymerization or condensation of the thermosetting resin contained in the shell layer starts before the toner core is spheroidized by surface tension, and it may be difficult to obtain spherical toner particles. If the rate of temperature increase is too slow, the toner core may soften and the toner cores may aggregate before the thermosetting resin contained in the shell layer is polymerized or condensed.
- one or more steps selected from a washing step, a drying step, and an external addition step may be performed as necessary.
- the toner base particles obtained by executing the shell layer forming step are washed with water.
- the washing method include a method of collecting a wet cake containing toner mother particles from a dispersion containing toner mother particles by solid-liquid separation, and washing the collected wet cake with water.
- a toner is dried using a dryer (for example, a spray dryer, a fluidized bed dryer, a vacuum freeze dryer, or a vacuum dryer).
- a spray dryer for example, a spray dryer, a fluidized bed dryer, a vacuum freeze dryer, or a vacuum dryer.
- an external addition step described later can be performed simultaneously.
- external addition conditions are prepared so that the external additive is not embedded in the shell layer, and a mixer (for example, FM mixer or Nauter mixer (registered trademark)) is used. Then, the toner base particles and the external additive are mixed, and the external additive is adhered to the surface of the shell layer.
- a mixer for example, FM mixer or Nauter mixer (registered trademark)
- a mechanical pulverizer (“Turbo Mill” manufactured by Freund Turbo, Inc.)
- a coarsely pulverized product was obtained by pulverizing to an average particle size of 30 ⁇ m. 200 g of the coarsely pulverized product obtained, 30 g of 1N sodium hydroxide aqueous solution, and 770 g of ion
- the obtained slurry was put into a 2 L round bottom stainless steel container equipped with a condenser, and stirred at a liquid temperature of 95 ° C. and a rotation speed of 200 rpm for 30 minutes. Then, it cooled to room temperature and solid-liquid-separated using the 300 mesh filter, and obtained the solid substance. The obtained solid was washed with water and dried to obtain an alkali-treated product of polyester resin A. In the same manner as above, the polyester resin A was alkali-treated to obtain a total of 1000 g of an alkali-treated product of polyester resin A.
- the binder resin fine particles in the dispersion had a solid content concentration of 25% by mass and a volume median diameter (D 50 ) of 115 nm.
- a release agent (“WEP-3” manufactured by NOF Corporation, melting point: 73 ° C.), 20 g of sodium lauryl sulfate, and 780 g of ion-exchanged water were mixed and heated to 90 ° C., and then a homogenizer (manufactured by IKA) "Ultra Turrax T50") and mixed for 5 minutes. Further, using a high-pressure homogenizer (“NV-200” manufactured by Yoshida Kikai Kogyo Co., Ltd.), the mixture was heated and mixed at a discharge pressure of 100 MPa and 100 ° C. to obtain a dispersion of release agent fine particles.
- the release agent fine particles in the dispersion had a solid content concentration of 10% by mass and a volume median diameter (D 50 ) of 120 nm.
- a colorant (CI Pigment Blue 15: 3), 20 g of a polyoxyethylene lauryl ether sodium sulfate aqueous solution (“Emar E-27C” manufactured by Kao Corporation) having a concentration of 27% by mass, and 380 g of ion-exchanged water
- a wet fine dispersion treatment was performed using a bead mill ("Dyno (registered trademark) mill” manufactured by WAB) to obtain a dispersion of colorant fine particles.
- the colorant fine particles in the dispersion had a solid content concentration of 20% by mass, a total solid content concentration of 21% by mass, and a volume median diameter (D 50 ) of 113 nm.
- ⁇ Shell layer formation process> A 1 L three-necked flask equipped with a thermometer, a stirrer, and a condenser was set in a 30 ° C. water bath. Into the flask, 300 mL of ion-exchanged water was added, and hydrochloric acid was further added to adjust the pH to 4. Hexamethylol melamine precursor as a melamine resin precursor (an aqueous solution of hexamethylol melamine initial polymer, “Milben (registered trademark) Resin SM-607” manufactured by Showa Denko KK, solid concentration 80 mass% ) 2 mL was added and mixed and dissolved.
- “Milben (registered trademark) Resin SM-607” manufactured by Showa Denko KK, solid concentration 80 mass%
- the flask contents were then cooled to 25 ° C. and then neutralized with sodium hydroxide. Thereafter, suction filtration was performed using a Buchner funnel, and a wet cake containing toner mother particles was collected by filtration. Furthermore, the toner base particles were washed by dispersing the wet cake containing the toner base particles after filtration using ion-exchanged water. The same washing of the toner base particles with ion exchange water was repeated 6 times. The wet cake containing the toner base particles after washing is dispersed in an aqueous ethanol solution having a concentration of 50% by mass, and hot air is used using a fine particle surface modification device (“Coat Mizer (registered trademark)” manufactured by Freund Turbo). The film was dried at a temperature of 45 ° C. and a blower air volume of 2 m 3 / min. Table 1 shows the volume median diameter (D 50 ) and sphericity of the toner particles obtained.
- the electrostatic charge image developing toner of Example 2 was obtained in the same manner as in Example 1 except for the above.
- the electrostatic charge image developing toner of Example 3 was obtained in the same manner as in Example 1 except for the above.
- Example 4 An electrostatic image developing toner of Example 4 was obtained in the same manner as in Example 1 except that the temperature at the time of forming the shell layer was changed from 60 ° C. to 62 ° C.
- Example 5 An electrostatic charge image developing toner of Example 5 was obtained in the same manner as in Example 1 except that the temperature at the time of forming the shell layer was changed from 60 ° C. to 64 ° C.
- Example 6 An electrostatic charge image developing toner of Example 6 was obtained in the same manner as in Example 1 except that the temperature at the time of forming the shell layer was changed from 60 ° C. to 66 ° C.
- Example 7 An electrostatic charge image developing toner of Example 7 was obtained in the same manner as in Example 1 except that the temperature at the time of forming the shell layer was changed from 60 ° C. to 68 ° C.
- Example 8 To a 2 L flask equipped with a stirrer, thermometer, condenser, and nitrogen inlet tube, 250 g of isobutanol was added and 155 g of styrene, 75 g of butyl acrylate, and t-butylperoxy 2-ethylhexano were introduced while introducing nitrogen. Eate (manufactured by Arkema Yoshitomi Co., Ltd.) 36 g was added, the temperature was raised to 100 ° C, and the mixture was stirred at that temperature for 3 hours. Further, 12 g of t-butylperoxy 2-ethylhexanoate was added and stirred for 3 hours.
- Eate manufactured by Arkema Yoshitomi Co., Ltd.
- the obtained slurry was put into a pressure-resistant round bottom stainless steel container, and a high-speed shear emulsification apparatus (“CLEARMIX (registered trademark) CLM-2.2S” manufactured by M Technique Co., Ltd.) was used.
- the slurry was shear-dispersed for 30 minutes at 0.5 MPa, 140 ° C., and a rotor rotational speed of 20000 rpm. Thereafter, the mixture was cooled to 50 ° C. while stirring at a rotational speed of 15000 rpm, and the temperature was lowered at a rate of 5 ° C./min to obtain a dispersion of styrene-acrylic resin A fine particles.
- An electrostatic charge image developing toner of Example 8 was obtained in the same manner as in Example 1 except that the polyester resin A was replaced with styrene-acrylic resin A.
- An electrostatic charge image developing toner of Comparative Example 2 was obtained in the same manner as in Example 1 except that the toner was replaced.
- Comparative Example 3 An electrostatic charge image developing toner of Comparative Example 3 was obtained in the same manner as in Example 1 except that the temperature at the time of forming the shell layer was changed from 60 ° C. to 59 ° C.
- the obtained slurry was put into a pressure-resistant round bottom stainless steel container, and a high-speed shear emulsification apparatus (“CLEARMIX (registered trademark) CLM-2.2S” manufactured by M Technique Co., Ltd.) was used.
- the slurry was shear-dispersed for 30 minutes at 0.5 MPa, 140 ° C., and a rotor rotational speed of 20000 rpm. Thereafter, the mixture was cooled to 50 ° C. at a rotation speed of 15,000 rpm and cooled at a temperature drop rate of 5 ° C./min to obtain a dispersion of fine particles of styrene-acrylic resin fine B.
- the electrostatic charge image developing toner of Comparative Example 4 was prepared in the same manner as in Example 1 except that 2 mL of the hexamethylolmelamine precursor used for forming the shell layer was replaced with 190 g of styrene-acrylic resin B. Got.
- the content ratio of THF-insoluble matter was calculated using the following formula.
- the mass of the toner is W 1 and the mass of the resin soluble in THF is W 2 .
- Content of THF-insoluble matter (mass%) (W 1 ⁇ W 2 ) / W 1 ⁇ 100
- Table 1 shows the measurement results of the content ratio of the THF-insoluble matter.
- melt viscosity of toner 1.4 g of the electrostatic charge image developing toners of Examples 1 to 8 and Comparative Examples 1 to 4 were molded into cylindrical pellets of about 1.9 cm 3 .
- the obtained pellet was set in a flow tester (manufactured by Shimadzu Corporation). While heating from 35 ° C. to 200 ° C. at a rate of temperature increase of 2 ° C./min, a load of 30 kg / cm 2 is applied by a plunger to extrude the pelletized toner from the nozzle, and the melt viscosity of the toner at 75 ° C. is adjusted. It was measured. A die having a height of 1.0 mm and a diameter of 1.0 mm was used. Table 1 shows the measurement results of the melt viscosity of the toner at 75 ° C.
- the volume median diameters (D 50 ) of the toners obtained in Examples 1 to 8 and Comparative Examples 1 to 4 were measured using a particle size distribution measuring apparatus (“Multisizer 3” manufactured by Beckman Coulter, Inc.). Table 1 shows the measurement results of the volume median diameter (D 50 ) of the toner.
- the average particle diameter of the manganese-based ferrite particles was 35 ⁇ m, and the saturation magnetization when the applied magnetic field was 3000 (1000 / 4 ⁇ ⁇ A / m) was 70 A ⁇ m 2 / kg.
- a polyamideimide resin which is a copolymer of trimellitic anhydride and 4,4'-diaminodiphenylmethane was diluted with methyl ethyl ketone to prepare a resin solution.
- a copolymer (FEP) of tetrafluoroethylene and propylene hexafluoride is dispersed, and further 2% by mass of silicon oxide is dispersed with respect to the total amount of the resin, thereby obtaining 150 g of a carrier coating solution in terms of solid content. It was.
- the weight composition ratio of the polyamideimide resin and FEP is 2: 8, and the solid content concentration in the carrier coat liquid is 10% by mass.
- a two-component developer was filled in a black developing device of a color printer (“TASKalfa 5550ci” manufactured by Kyocera Document Solutions Inc.).
- the toner obtained in Examples 1 to 8 and Comparative Examples 1 to 4 was filled in a black toner container.
- a toner image (patch sample) of 2 cm ⁇ 3 cm was output as an unfixed image on an evaluation paper (“Color Copy (registered trademark) 90” manufactured by Mondi) so that the toner loading amount was 1.67 mg / cm 2 .
- an evaluation paper (“Color Copy (registered trademark) 90” manufactured by Mondi)
- the fixing jig is a jig modified so that the fixing temperature and linear velocity of the fixing device of the color printer (“TASKalfa 5550ci” manufactured by Kyocera Document Solutions Co., Ltd.) can be varied.
- the surface material of the heating roll was PFA
- the thickness of the heating roll was 30 ⁇ m ⁇ 10 ⁇ m
- the surface roughness (Ra) was 5 ⁇ m.
- the evaluation sheet on which the fixed image was fixed was visually observed to measure the minimum fixable temperature. When the minimum fixable temperature of the toner exceeded 100 ° C., the toner fixability was insufficient. When the minimum fixable temperature of the toner is 100 ° C. or lower, the toner has good fixability. Table 1 shows the measurement results of the minimum fixable temperature of the toner.
- a sieve having an opening of 45 ⁇ m was placed at the bottom, and a sieve having an opening of 63 ⁇ m and an opening of 105 ⁇ m was sequentially stacked.
- the overlapped sieve was attached to a powder tester (“TYPE PT-E” manufactured by Hosokawa Micron Corporation). Then, the toner was wiped for 30 seconds under the condition of 5 memories of a powder tester. Next, the weight of the toner remaining on the sieve was measured, and the degree of aggregation of the toner was determined by the following formula.
- Aggregation degree (mass%) (a) + (b) + (c) (A): (Weight of toner remaining on sieve having aperture of 105 ⁇ m) / 3 ⁇ 100 (B): (Weight of toner remaining on sieve having aperture of 63 ⁇ m) / 3 ⁇ 3/5 ⁇ 100 (C): (Weight of toner remaining on sieve having aperture of 45 ⁇ m) / 3 ⁇ 1/5 ⁇ 100
- the aggregation degree of the toner is 15% by mass or more, the blocking property of the toner is insufficient. However, when the aggregation degree of the toner is less than 15% by mass, the blocking property of the toner is good. Table 1 shows the measurement results of the degree of aggregation of the toner.
- Table 1 shows the measurement results and evaluation results of the toners obtained in Examples 1 to 8 and Comparative Examples 1 to 4.
- the melt viscosity at 75 ° C. of the toner is as low as 9500 Pa ⁇ s, 1.0 ⁇ 10 4 Pa ⁇ s or more and 1.0 ⁇ 10 5 Pa ⁇ s. It was not within the following range. Therefore, the degree of aggregation of the toner is increased, and the toner blocking property is insufficient.
- the temperature at the time of forming the shell layer was as low as 59 ° C.
- the thermosetting resin contained in the shell layer has a low degree of cross-linking, and the toner insoluble content of the toner is less than 90% by mass. Therefore, the degree of aggregation of the toner is increased, and the toner blocking property is insufficient.
- the toner for developing an electrostatic charge image of this embodiment can be suitably used in an image forming apparatus.
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Abstract
Description
トナーコアは、例えば、結着樹脂を含むことができる。トナーコアは、必要に応じて結着樹脂以外に任意成分(例えば、離型剤、着色剤、電荷制御剤、及び/又は磁性粉)を含んでもよい。以下にトナーコアに含まれる成分について説明する。
トナーコアに含まれる結着樹脂は、トナー用の結着樹脂である限り、特に限定されない。結着樹脂としては、例えば、スチレン系樹脂、アクリル系樹脂、スチレン-(メタ)アクリル系樹脂、ポリエチレン系樹脂、ポリプロピレン系樹脂、塩化ビニル系樹脂、ポリエステル樹脂、ポリアミド樹脂、ウレタン樹脂、ポリビニルアルコール系樹脂、ビニルエーテル系樹脂、N-ビニル系樹脂、又はスチレン-ブタジエン樹脂のような熱可塑性樹脂が挙げられる。これらの熱可塑性樹脂の中でも、トナー中での着色剤の分散性、トナーの帯電性、又はトナーの記録媒体に対する定着性を良好にするという観点から、スチレン-(メタ)アクリル系樹脂、又はポリエステル樹脂が好ましい。以下、スチレン-(メタ)アクリル系樹脂、又はポリエステル樹脂について説明する。
トナーコアは、必要に応じて離型剤を含んでもよい。離型剤は、一般的に、トナーの低温定着性及び耐オフセット性を向上させる目的で使用される。離型剤の種類は、公知のトナー用の離型剤として使用される離型剤である限り、特に限定されない。
トナーコアは、必要に応じて着色剤を含んでもよい。トナーコアに含有させる着色剤としては、トナー粒子の色に合わせて、公知の顔料や染料を用いることができる。トナーコアに含有させることができる好適な着色剤の具体例としては、以下の着色剤が挙げられる。
以下、トナーコアに含まれる電荷制御剤について説明する。
トナーコアは、必要に応じて磁性粉を含んでもよい。好適な磁性粉としては、例えば、フェライト、マグネタイト、鉄、強磁性金属(コバルト、及びニッケル)、合金(鉄、及び/又は強磁性金属を含む合金)、化合物(鉄、及び/又は強磁性金属を含む化合物)、強磁性合金(熱処理のような強磁性化処理を行った強磁性合金)、又は二酸化クロムが挙げられる。
本実施形態の静電荷像現像用トナーにおいて、シェル層がトナーコアの表面を被覆する。以下に、シェル層に含まれる成分について説明する。
本実施形態では、シェル層がカチオン性(正帯電性)を有することが好ましい。そのため、シェル層に、正帯電性の電荷制御剤を含んでもよい。
トナー粒子は、外添剤を含んでもよい。本実施形態の静電荷像現像用トナーにおいて、外添剤を、トナー母粒子の表面に付着させることができる。
THF不溶分の含有割合(質量%)=(W1-W2)/W1×100
静電荷像現像用トナーの製造方法は、例えば、トナーコア調製工程とシェル層形成工程とを含むことができる。トナーコア調製工程において、トナーコアを調製する。シェル層形成工程において、トナーコアの表面にシェル層を形成する。
トナーコア調製工程を実行するために、結着樹脂中に、必要に応じて任意成分(例えば、離型剤、着色剤、電荷制御剤、及び/又は磁性粉)を良好に分散させることができる方法を用いる。トナーコア調製工程を実行する方法としては、凝集法が挙げられる。
以下に凝集工程について説明する。凝集工程では、凝集粒子を調製する。一般にトナーコアを構成する成分を含む微粒子は、水性媒体中で結着樹脂又は結着樹脂を含む組成物を所望の粒子径に微粒子化することで、結着樹脂を含む微粒子(結着樹脂微粒子)を水性媒体中で分散させる結着樹脂微粒子分散液として調製される。結着樹脂微粒子の分散液は、結着樹脂以外の任意成分(例えば、離型剤又は着色剤)の微粒子の水性分散液(例えば、着色剤微粒子分散液又は離型剤微粒子分散液)を含んでもよい。凝集工程では、このような結着樹脂微粒子分散液中で微粒子を凝集させて凝集粒子を得る。
次いで、合一化工程では、凝集工程によって得られた凝集粒子に含まれる成分を水性媒体中で合一化させて、トナーコアを形成させる。凝集粒子に含まれる成分を合一化させるためには、凝集工程によって得られる凝集粒子を含む水性分散液を加熱すればよい。これによりトナーコアを含む水性分散液を得ることができる。
シェル層形成工程は、供給工程と樹脂化工程とを含む。供給工程では、トナーコアの表面に熱硬化性樹脂のモノマー及び/又はプレポリマーを含むシェル層の形成溶液を供給する。樹脂化工程では、シェル層の形成溶液に含まれる熱硬化性樹脂のモノマー及び/又はプレポリマーを重合又は縮合することにより樹脂化する工程である。
シェル層の表面に外添剤を付着させることで、トナー粒子が得られる。以下、本実施形態に係る外添方法について説明する。
〈トナーコア調製工程〉
機械式粉砕機(フロイント・ターボ株式会社製「ターボミル」)を用いて、ポリエステル樹脂A(Mn=2500、Mw=5000、Mw/Mn=2.0、Tm=85℃、Tg=43℃)を、平均粒子径30μmに粉砕して粗粉砕物を得た。得られた粗粉砕物200gと、1N-水酸化ナトリウム水溶液30gと、イオン交換水770gとを混合して、全量1000gのスラリーを調整した。次いで、得られたスラリーをコンデンサーを装着した容量2Lの丸底ステンレス容器に投入し、液温95℃、回転数200rpmで30分間攪拌した。その後、室温まで冷却して、300メッシュのフィルターを用いて固液分離して固形物を得た。得られた固形物を水洗浄、乾燥して、ポリエステル樹脂Aのアルカリ処理品を得た。上記と同様にポリエステル樹脂Aをアルカリ処理して合計1000gのポリエステル樹脂Aのアルカリ処理品を得た。
容量2Lのステンレス製丸底フラスコ容器に、上記の結着樹脂微粒子の分散液340gと、上記の離型剤微粒子の分散液50gと、上記の着色剤微粒子の分散液25gと、イオン交換水500gとを投入した。その分散液を、攪拌羽根を用いて回転数200rpmで攪拌した。その後、水酸化ナトリウム水溶液を添加してpHを10に調整して、25℃で10分間攪拌した。その後、濃度50質量%の塩化マグネシウム六水和物水溶液10gを5分かけて滴下した。その分散液を昇温速度0.2℃/分で50℃まで昇温した後、その温度で30分間攪拌しながら、微粒子同士を凝集させた。濃度20質量%の塩化ナトリウム水溶液50gを一度に添加して、微粒子同士の凝集を停止させた。
次いで、濃度5質量%のラウリル硫酸ナトリウム水溶液100gを添加した。得られた分散液を昇温速度0.2℃/分で65℃まで昇温した後、その温度で1時間攪拌した。その後、降温速度10℃/分の速度で25℃まで冷却して、トナーコアを得た。トナーコアは、体積中位径(D50)6.0μm、球形化度0.941であった。
温度計と攪拌機と冷却器とを備えた容量1Lの三つ口フラスコを30℃のウォーターバス中にセットした。フラスコ内にイオン交換水300mLを投入して、更に、塩酸を添加して、pHを4に調整した。得られた酸性水溶液にメラミン樹脂前駆体としてのヘキサメチロールメラミン前駆体(ヘキサメチロールメラミン初期重合体の水溶液、昭和電工株式会社製「ミルベン(登録商標)レジンSM-607」、固形分濃度80質量%)2mLを添加して、混合、溶解させた。得られた混合溶液を、シェル層の膜厚が6nmとなるように上記トナーコア300gを添加して、攪拌した。更に、イオン交換水300mLを添加して、攪拌しながら昇温速度5℃/分で60℃まで昇温した後、その温度で2時間攪拌して、トナーコアの表面にシェル層を形成した。
ポリエステル樹脂Aをポリエステル樹脂B(Mn=3200、Mw=6400、Mw/Mn=2.0、Tm=95℃、Tg=48℃)に代え、シェル層形成時の温度を60℃から70℃に代えた以外は、実施例1と同様の操作を行って、実施例2の静電荷像現像用トナーを得た。
ポリエステル樹脂Aをポリエステル樹脂C(Mn=2800、Mw=5600、Mw/Mn=2.0、Tm=90℃、Tg=45℃)に代え、シェル層形成時の温度を60℃から65℃に代えた以外は、実施例1と同様の操作を行って、実施例3の静電荷像現像用トナーを得た。
シェル層形成時の温度を60℃から62℃に代えた以外は、実施例1と同様の操作を行って、実施例4の静電荷像現像用トナーを得た。
シェル層形成時の温度を60℃から64℃に代えた以外は、実施例1と同様の操作を行って、実施例5の静電荷像現像用トナーを得た。
シェル層形成時の温度を60℃から66℃に代えた以外は、実施例1と同様の操作を行って、実施例6の静電荷像現像用トナーを得た。
シェル層形成時の温度を60℃から68℃に代えた以外は、実施例1と同様の操作を行って、実施例7の静電荷像現像用トナーを得た。
攪拌機と温度計とコンデンサーと窒素導入管とを備えた容量2Lのフラスコにイソブタノール250gを投入して、窒素を導入しながら、スチレン155gとブチルアクリレート75gとt-ブチルパーオキシ2-エチルヘキサノエート(アルケマ吉富株式会社製)36gとを添加して、100℃まで昇温して、その温度で3時間攪拌した。更に、t-ブチルパーオキシ2-エチルヘキサノエート12gを添加して、3時間攪拌した。その後、10kPa、140℃で減圧乾燥してイソブタノールを留去して乾燥物を得た。得られた乾燥物を解砕して平均粒子径10μm以下の粉砕物を得た。得られた粉砕物100gとアニオン系界面活性剤(花王株式会社製「エマール0」)1gと0.1N-水酸化ナトリウム水溶液25gとを配合した。そして、溶液の全量400gとなるようにイオン交換水を添加してスラリーを得た。次いで、得られたスラリーを耐圧丸底ステンレス製容器に投入して、高速せん断乳化装置(エム・テクニック株式会社製「クレアミックス(登録商標)CLM-2.2S」)を用いて、容器内のスラリーを、0.5MPa、140℃、ローター回転数20000rpmで30分間せん断分散した。その後、50℃まで回転数15000rpmで攪拌しながら降温速度5℃/分で冷却を行って、スチレン-アクリル樹脂Aの微粒子の分散液を得た。分散液中のスチレン-アクリル樹脂Aは、体積中位径(D50)120nm、固形分濃度29.8質量%、Mn=7000、Mw=16000、Mw/Mn=2.29、Tm=90.0℃、Tg=45.2℃であった。
ポリエステル樹脂Aをポリエステル樹脂D(Mn=2400、Mw=4800、Mw/Mn=2.0、Tm=83℃、Tg=42℃)に代えた以外は、実施例1と同様の操作を行って、比較例1の静電荷像現像用トナーを得た。
ポリエステル樹脂Aをポリエステル樹脂E(Mn=3400、Mw=6800、Mw/Mn=2.0、Tm=97℃、Tg=49℃)に代え、シェル層形成時の温度を60℃から70℃に代えた以外は、実施例1と同様の操作を行って、比較例2の静電荷像現像用トナーを得た。
シェル層形成時の温度を60℃から59℃に代えた以外は、実施例1と同様の操作を行って、比較例3の静電荷像現像用トナーを得た。
攪拌機と温度計とコンデンサーと窒素導入管とを備えた容量2Lのフラスコにn-プロピルアルコール240gを投入して、窒素を導入しながら、スチレン67.5gとブチルメタクリレート22.5gとを添加して、65℃まで加熱した。更に、t-ヘキシルパーオキシピバレートの炭化水素希釈品(日油株式会社製「パーヘキシルPV」)1gをn-プロピルアルコール40gに溶解させた溶液を、65℃で3時間かけて滴下して、その後5時間攪拌した。更に、80℃まで昇温して、80℃で1時間攪拌した。その後、10kPa、140℃で減圧乾燥してn-プロピルアルコールを留去して乾燥物を得た。得られた乾燥物を解砕して平均粒子径10μm以下の粉砕物を得た。得られた粉砕物100gとカチオン系界面活性剤(花王株式会社製「コータミン24P」)1gと0.1N-水酸化ナトリウム水溶液25gとを配合した。そして、溶液の全量が400gとなるようにイオン交換水を添加してスラリーを得た。次いで、得られたスラリーを耐圧丸底ステンレス製容器に投入して、高速せん断乳化装置(エム・テクニック株式会社製「クレアミックス(登録商標)CLM-2.2S」)を用いて、容器内のスラリーを、0.5MPa、140℃、ローター回転数20000rpmで30分間せん断分散した。その後、50℃まで回転数15000rpmで攪拌しながら降温速度5℃/分で冷却を行って、スチレン-アクリル樹脂微Bの微粒子の分散液を得た。分散液中のスチレン-アクリル樹脂Bは、体積中位径(D50)130nm、固形分濃度20.3質量%、Mn=50000、Mw=100000、Mw/Mn=2.0、Tm=150℃、Tg=73℃であった。
実施例1~8及び比較例1~4の静電荷像現像用トナーの測定方法及び評価方法は以下の通りである。
実施例1~8及び比較例1~4の静電荷像現像用トナー1.0g(W1)を、テトラヒドロフラン(THF)200mL中に添加した。そのスラリーを12時間攪拌して、THFに可溶な樹脂(W2)を溶解した。その後、スラリーを円筒ろ紙(アドバンテック株式会社製「No.86R」)を備えたソックスレー抽出器に投入して、THFに溶解した樹脂を、6時間抽出した。抽出されたTHFに可溶な樹脂をエバポレートした後、100℃で1時間、減圧乾燥して、THFに可溶な樹脂を得た。以下の式を用いてTHF不溶分の含有割合を算出した。トナーの質量をW1として、THFに可溶な樹脂の質量をW2とした。
THF不溶分の含有割合(質量%)=(W1-W2)/W1×100
表1にTHF不溶分の含有割合の測定結果を示す。
実施例1~8及び比較例1~4の静電荷像現像用トナー1.4gを、約1.9cm3の円柱状のペレットに成形した。得られたペレットをフローテスター(株式会社島津製作所製)にセットした。昇温速度2℃/分で35℃から200℃まで加熱しながら、プランジャーによる30kg/cm2の荷重を加えて、ノズルからペレット状のトナーを押し出して、75℃でのトナーの溶融粘度を測定した。高さが1.0mmで直径1.0mmのダイを使用した。表1に75℃でのトナーの溶融粘度の測定結果を示す。
実施例1~8及び比較例1~4にて得られたトナーの体積中位径(D50)を粒度分布測定装置(ベックマン・コールター株式会社製「Multisizer3」)を用いて測定した。表1にトナーの体積中位径(D50)の測定結果を示す。
実施例1~8及び比較例1~4にて得られたトナーの球形化度を湿式フロ-式粒子径/形状分析装置(シスメックス株式会社製「FPIA(登録商標)-3000」)を用いて測定した。表1にトナーの球形化度の測定結果を示す。
常温硬化性のエポキシ樹脂中にシェル化した乾式シリカとトナーとを十分に分散させた後、40℃の雰囲気下で2日間硬化させた。得られた硬化物を四酸化オスミウムで染色した後、ダイヤモンドナイフをセットしたミクロトームで薄片状のサンプルを切り出し、透過型電子顕微鏡(TEM)を用いてトナーの断面形態を観察して、シェル層の膜厚を測定した。表1にシェル層の膜厚の測定結果を示す。
実施例1~8及び比較例1~4にて得られたトナーの吸熱ピークを示差走査熱量計(セイコーインスツル株式会社製「DSC-6220」)を用いて測定した。60℃以上80℃以下の温度範囲での吸熱ピークを、測定試料と基準物質との間の熱量差から求めた。実施例1~8及び比較例1~4にて得られたトナーの吸熱ピークが一定である場合は、トナーに含まれる離型剤の含有量が一定とした。表1にトナーのDSC吸熱ピークの測定結果を示す。
MnO換算で39.7mol%、MgO換算で9.9mol%、Fe2O3換算で49.6mol%、SrO換算で0.8mol%となるように配合した粉体にイオン交換水を添加して、湿式ボールミルを用いて10時間、粉砕し、混合し、乾燥させて、950℃で4時間保持した。その後、湿式ボールミルを用いて24時間粉砕を行って粉砕品を得た。得られた粉砕品を造粒乾燥して、酸素濃度2vol%の雰囲気下1270℃で6時間保持した。その後、解砕して、粒度調整を行い、マンガン系フェライト粒子を得た。マンガン系フェライト粒子の平均粒子径は35μmであり、印加磁場が3000(1000/4π・A/m)の時の飽和磁化が70A・m2/kgであった。
カラープリンター(京セラドキュメントソリューションズ株式会社製「TASKalfa5550ci」)の黒色用の現像装置に、2成分現像剤を充填した。そして、実施例1~8及び比較例1~4にて得られたトナーを黒色用のトナーコンテナに充填した。評価用紙(モンディ社製「Color Copy(登録商標) 90」)に、トナー載せ量1.67mg/cm2となるように、2cm×3cmのトナー画像(パッチサンプル)を未定着画像として出力した。次に、定着治具を用いて、25℃、50%RHの環境下で、定着温度80℃以上200℃以下の温度範囲で5℃毎にパッチサンプルの未定着画像を、線速300mm/秒で60枚の評価用紙を定着させた。なお、定着治具は、カラープリンター(京セラドキュメントソリューションズ株式会社製「TASKalfa5550ci」)の定着装置の定着温度と線速とを可変できるように改造した治具である。また、加熱ロールの表面材質はPFAであり、加熱ロールの膜厚は30μm±10μmであり、面粗度(Ra)は5μmであった。次に、定着後の画像が定着された評価用紙を目視で観察して、最低定着可能温度を測定した。トナーの最低定着可能温度が100℃を超えると、トナーの定着性が不十分であった。トナーの最低定着可能温度が100℃以下であると、トナーの定着性が良好であった。表1にトナーの最低定着可能温度の測定結果を示す。
実施例1~8及び比較例1~4にて得られたトナー3gを容量20mLのポリ容器に投入した。トナーが投入されたポリ容器を恒温槽(三洋電機株式会社製「CONVECTION OVEN」)を用いて60℃で3時間及び48時間の2段加熱を行った。その後、25℃、65%RHでの環境下で30分間静置した。恒温槽から取り出されたポリ容器に入っているトナーを質量既知のメッシュ目開き105μmの篩に投入し、篩前の篩の質量を測定することで、篩上のトナーの重量を測定した。次に、目開き45μmの篩を一番下にして、目開き63μm及び目開き105μmの篩を順に重ねた。次に重ねた篩をパウダーテスター(ホソカワミクロン株式会社製「TYPE PT-E」)に取り付けた。そして、パウダーテスターの5メモリーの条件で30秒間、トナーをふるった。次いで、篩上に残存したトナーの重量を測定し、以下の式によりトナーの凝集度を求めた。
凝集度(質量%)=(a)+(b)+(c)
(a):(目開き105μmの篩上に残存したトナーの重量)/3×100
(b):(目開き63μmの篩上に残存したトナーの重量)/3×3/5×100
(c):(目開き45μmの篩上に残存したトナーの重量)/3×1/5×100
トナーの凝集度が15質量%以上であると、トナーのブロッキング性は不十分であったが、トナーの凝集度が15質量%未満であると、トナーのブロッキング性は良好であった。表1にトナーの凝集度の測定結果を示す。
Claims (3)
- 複数のトナー粒子を含む静電荷像現像用トナーであって、
前記複数のトナー粒子の各々は、トナーコアと、前記トナーコアを被覆するシェル層とを含み、
前記シェル層は、熱硬化性樹脂を含み、
前記トナーのテトラヒドロフラン不溶分の含有割合が、前記トナーの質量に対して90質量%以上であり、
前記トナーの75℃での溶融粘度が1.0×104Pa・s以上1.0×105Pa・s以下である、静電荷像現像用トナー。 - 前記熱硬化性樹脂は、メラミン樹脂又は尿素樹脂である、請求項1に記載の静電荷像現像用トナー。
- 前記トナーコアは、結着樹脂を含み、
前記結着樹脂の軟化点(Tm)は、85℃以上95℃以下である、請求項1に記載の静電荷像現像用トナー。
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JP2016505133A JP6256589B2 (ja) | 2014-02-25 | 2015-02-10 | 静電荷像現像用トナー |
CN201580009944.8A CN106030419B (zh) | 2014-02-25 | 2015-02-10 | 静电荷像显影用调色剂 |
US15/120,715 US9964885B2 (en) | 2014-02-25 | 2015-02-10 | Electrostatic charge image developing toner |
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US (1) | US9964885B2 (ja) |
JP (1) | JP6256589B2 (ja) |
CN (1) | CN106030419B (ja) |
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CN107153332B (zh) * | 2017-06-29 | 2021-01-26 | 邯郸汉光办公自动化耗材有限公司 | 一种核壳结构的墨粉制备方法 |
JP2022022128A (ja) * | 2020-07-22 | 2022-02-03 | キヤノン株式会社 | トナー |
JP2022022127A (ja) | 2020-07-22 | 2022-02-03 | キヤノン株式会社 | トナー |
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JPH02162355A (ja) * | 1988-12-16 | 1990-06-21 | Canon Inc | 加熱定着方法及び該方法に使用される加熱定着用カプセルトナー |
JP2004294469A (ja) * | 2003-03-25 | 2004-10-21 | Toppan Forms Co Ltd | 薄膜被覆トナー、薄膜被覆トナーの製造方法 |
JP2008261948A (ja) * | 2007-04-10 | 2008-10-30 | Fuji Xerox Co Ltd | 静電荷像現像用トナー、静電荷像現像用トナーの製造方法、静電荷像現像用現像剤及び画像形成装置 |
JP2009237110A (ja) * | 2008-03-26 | 2009-10-15 | Toppan Forms Co Ltd | 低温定着性トナーおよびその製造方法 |
JP2013228556A (ja) * | 2012-04-25 | 2013-11-07 | Kyocera Document Solutions Inc | 静電荷像現像用トナー |
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JPH09258480A (ja) * | 1996-03-21 | 1997-10-03 | Fuji Xerox Co Ltd | 静電荷現像用トナー及びその製造方法と画像形成方法 |
EP1091258B1 (en) * | 1998-05-12 | 2006-10-25 | Nippon Zeon Co., Ltd. | Polymerization toner and process for producing the same |
US6686112B2 (en) * | 2000-03-10 | 2004-02-03 | Seiko Epson Corporation | Electrophotographing dry-type toner and production method therefor |
US20050271964A1 (en) | 2002-08-23 | 2005-12-08 | Toppan Forms Co., Ltd. | Toner coated with thin film |
JP4326245B2 (ja) | 2003-03-25 | 2009-09-02 | トッパン・フォームズ株式会社 | 薄膜被覆重合トナー、薄膜被覆重合トナーの製造方法 |
JP4732241B2 (ja) | 2006-05-30 | 2011-07-27 | キヤノン株式会社 | トナー |
JP2009139933A (ja) * | 2007-11-14 | 2009-06-25 | Konica Minolta Business Technologies Inc | 静電潜像現像用トナーと画像形成方法 |
JP2010113112A (ja) | 2008-11-06 | 2010-05-20 | Panasonic Corp | トナー及びトナーの製造方法 |
JP5919693B2 (ja) | 2011-09-09 | 2016-05-18 | コニカミノルタ株式会社 | 静電荷像現像用トナー |
US8951708B2 (en) * | 2013-06-05 | 2015-02-10 | Xerox Corporation | Method of making toners |
-
2015
- 2015-02-10 CN CN201580009944.8A patent/CN106030419B/zh not_active Expired - Fee Related
- 2015-02-10 US US15/120,715 patent/US9964885B2/en active Active
- 2015-02-10 JP JP2016505133A patent/JP6256589B2/ja not_active Expired - Fee Related
- 2015-02-10 WO PCT/JP2015/053621 patent/WO2015129448A1/ja active Application Filing
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JPH02162355A (ja) * | 1988-12-16 | 1990-06-21 | Canon Inc | 加熱定着方法及び該方法に使用される加熱定着用カプセルトナー |
JP2004294469A (ja) * | 2003-03-25 | 2004-10-21 | Toppan Forms Co Ltd | 薄膜被覆トナー、薄膜被覆トナーの製造方法 |
JP2008261948A (ja) * | 2007-04-10 | 2008-10-30 | Fuji Xerox Co Ltd | 静電荷像現像用トナー、静電荷像現像用トナーの製造方法、静電荷像現像用現像剤及び画像形成装置 |
JP2009237110A (ja) * | 2008-03-26 | 2009-10-15 | Toppan Forms Co Ltd | 低温定着性トナーおよびその製造方法 |
JP2013228556A (ja) * | 2012-04-25 | 2013-11-07 | Kyocera Document Solutions Inc | 静電荷像現像用トナー |
Also Published As
Publication number | Publication date |
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CN106030419B (zh) | 2019-08-27 |
US9964885B2 (en) | 2018-05-08 |
JPWO2015129448A1 (ja) | 2017-03-30 |
CN106030419A (zh) | 2016-10-12 |
JP6256589B2 (ja) | 2018-01-10 |
US20170010552A1 (en) | 2017-01-12 |
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