CN112119356A - Toner for developing electrostatic image and method for producing toner for developing electrostatic image - Google Patents
Toner for developing electrostatic image and method for producing toner for developing electrostatic image Download PDFInfo
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- CN112119356A CN112119356A CN201980030990.4A CN201980030990A CN112119356A CN 112119356 A CN112119356 A CN 112119356A CN 201980030990 A CN201980030990 A CN 201980030990A CN 112119356 A CN112119356 A CN 112119356A
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- toner
- crystalline polyester
- polyester resin
- resin
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy 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
- G03G9/087—Binders for toner 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
- G03G9/087—Binders for toner particles
- G03G9/08742—Binders for toner particles comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- G03G9/08755—Polyesters
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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
- G03G9/097—Plasticisers; Charge controlling agents
Abstract
A toner for developing electrostatic images, comprising toner particles and an external additive, wherein the toner particles comprise a binder resin containing a crystalline polyester resin, a colorant and a release agent, the crystalline polyester resin comprises sebacic acid as an acid component and 1, 10-decanediol as an alcohol component, and has a mass average molecular weight of 3000 to 5000, and the toner particles contain 5 to 10% by mass.
Description
Technical Field
The present invention relates to a toner for developing electrostatic images and a method for producing the toner for developing electrostatic images. More specifically, the present invention relates to a toner for developing electrostatic images which exhibits excellent storage stability and can be fixed at low temperatures, and a method for producing the toner for developing electrostatic images.
Background
Conventionally, in electrophotographic printers and copiers, reduction in fixing temperature and reduction in standby time have been required from the viewpoint of energy saving. Accordingly, excellent low-temperature fixing performance is required for the toner to be used. When the resin is made to have a low melting point in order to improve the low-temperature fixing performance, the glass transition temperature of the toner decreases, and the storage stability deteriorates. Patent document 1 proposes a method of preventing a decrease in glass transition temperature by performing a heating treatment at the time of manufacturing a toner. Patent document 2 proposes a method of achieving both low-temperature fixability and storage stability by pulverizing a toner and classifying the toner into a core-shell structure.
Documents of the prior art
Patent document
Patent document 1: japanese patent application laid-open No. 2010-139752
Patent document 2: japanese laid-open patent publication No. 2015-157715
Disclosure of Invention
Here, in order to obtain low-temperature fixability, use of a crystalline resin having sharp melting properties is being studied. However, in particular, in the case of a toner obtained through a step of cooling and solidifying after kneading, followed by pulverization and classification, when an amorphous resin and a crystalline resin are melt-kneaded, if the amorphous resin and the crystalline resin are polyester or the like, the glass transition temperature is greatly lowered, and the storage stability is liable to be deteriorated. If the dispersibility of the amorphous resin and the crystalline resin is reduced, the charge amount of the toner tends to become uneven. Further, when the glass transition temperature is lowered, the toner is likely to be blocked during storage. In addition, the methods described in patent documents 1 to 2 require new facilities, and are liable to lower productivity and increase costs. Therefore, a toner that can utilize existing equipment and that can achieve both low-temperature fixability and storage stability is required.
The present invention has been made in view of the above-described conventional problems, and an object thereof is to provide a toner for developing an electrostatic image and a method for producing a toner for developing an electrostatic image, which can achieve both low-temperature fixability and storage stability by using existing equipment.
The present inventors have conducted extensive studies to solve the above problems, and as a result, have found that the molecular weight of the crystalline polyester resin and the carbon chain of the diol or dicarboxylic acid monomer molecule constituting the crystalline polyester resin affect the low-temperature fixing property and the storage stability. The present inventors have also found that the above problems can be solved by blending a predetermined amount of a crystalline polyester resin having a predetermined molecular weight, which contains sebacic acid as an acid component and 1, 10-decanediol as an alcohol component, into toner particles, and have completed the present invention.
The toner for electrostatic image development according to one embodiment of the present invention for solving the above problems includes toner particles and an external additive, the toner particles include a binder resin containing a crystalline polyester resin, a colorant, and a release agent, the crystalline polyester resin includes sebacic acid as an acid component, 1, 10-decanediol as an alcohol component, and has a mass average molecular weight of 3000 to 5000, and the toner particles include 5 to 10 mass%.
A method for producing a toner for electrostatic image development according to an aspect of the present invention to solve the above problems includes a step of kneading, cooling and solidifying the kneaded product, and then pulverizing and classifying the kneaded product.
Detailed Description
< toner for developing electrostatic image >
A toner for electrostatic image development (hereinafter also referred to as a "toner") according to an embodiment of the present invention includes toner particles and an external additive. The toner particles contain a binder resin containing a crystalline polyester resin, a colorant, and a release agent. The crystalline polyester resin contains sebacic acid as an acid component and 1, 10-decanediol as an alcohol component, has a mass average molecular weight of 3000 to 5000, and is contained in 5 to 10 mass% in the toner particles. The toner used in the image forming method of the electrophotographic system may be a two-component toner used together with a carrier or a one-component toner not using a carrier. The following description is made separately.
(toner particles)
The toner particles contain a binder resin containing a crystalline polyester resin, a colorant, and a release agent.
Binder resin
The binder resin is compounded for the following purposes: the colorant contained in the toner is dispersed, and is solidified after being melted on the surface of the recording medium by the heat of the fixing roller in the fixing process at the time of printing, so that the colorant is fixed on the surface of the recording medium.
As the binder resin, the crystalline polyester resin of the present embodiment and a binder resin other than the crystalline polyester resin of the present embodiment are used in combination.
The crystalline polyester resin of the present embodiment is blended to improve both low-temperature fixability and storage stability of the toner. The crystalline polyester resin of the present embodiment contains sebacic acid as an acid component and 1, 10-decanediol as an alcohol component.
By including 1, 10-decanediol as the alcohol component, both low-temperature fixability and storage stability of the obtained toner can be improved.
The mass average molecular weight of the crystalline polyester resin is preferably 3000 or more. The crystalline polyester resin preferably has a mass average molecular weight of 5000 or less. When the mass average molecular weight is less than 3000, the storage stability of the toner is likely to be lowered. On the other hand, when the mass average molecular weight exceeds 5000, the low-temperature fixability of the toner is likely to be reduced.
The content of the crystalline polyester resin in the toner particles is preferably 5% by mass or more. In addition, the content of the crystalline polyester resin in the toner particles is preferably 10% by mass or less. When the content is less than 5% by mass, the low-temperature fixability of the toner is poor. On the other hand, when the content exceeds 10 mass%, the storage stability of the toner is poor.
The melting point of the crystalline polyester resin is not particularly limited. For example, the melting point is preferably 70 ℃ or higher. The melting point is preferably 76 ℃ or lower. When the melting point is within the above range, the fixability of the toner is good. In the present embodiment, the melting point can be calculated by measuring the melting temperature in thermal analysis using a differential scanning calorimeter. The binder resin is not particularly limited.
The method for producing the crystalline polyester resin is not particularly limited, and can be produced by a conventional polyester polymerization method in which an acid component and an alcohol component are reacted, and examples thereof include direct polycondensation, a transesterification method, and the like.
The crystalline polyester resin can be produced at a polymerization temperature of 180 ℃ or higher and 230 ℃ or lower, and the reaction can be carried out while removing water and alcohol generated during condensation by reducing the pressure in the reaction system as necessary. When the monomers are insoluble or incompatible at the reaction temperature, solvents having a high boiling point may be added as dissolution aids to dissolve them. In the polycondensation reaction, the dissolution assisting solvent is distilled off. In the copolymerization, when a monomer having poor compatibility is present, it is preferable to previously condense the monomer having poor compatibility with an acid or alcohol to be condensed with the monomer and then to perform condensation polymerization together with the main component.
As a catalyst that can be used in the production of the crystalline polyester resin, there can be mentioned: alkali metal compounds such as sodium and lithium; alkaline earth metal compounds such as magnesium and calcium; metal compounds such as zinc, manganese, antimony, titanium, tin, zirconium and germanium; phosphorus oxide compounds, amine compounds, and the like, and specific examples thereof include the following compounds.
Examples thereof include: sodium acetate, sodium carbonate, lithium acetate, lithium carbonate, calcium acetate, calcium stearate, magnesium acetate, zinc stearate, zinc naphthenate, zinc chloride, manganese acetate, manganese naphthenate, titanium tetraethoxide, titanium tetrapropoxide, titanium tetraisopropoxide, titanium tetrabutoxide, antimony trioxide, triphenylantimony, tributylantimony, tin formate, tin oxalate, tetraphenyltin, dibutyltin dichloride, dibutyltin oxide, diphenyltin oxide, zirconium tetrabutoxide, zirconium naphthenate, zirconyl carbonate, zirconyl acetate, zirconyl stearate, zirconyl octoate, germanium oxide, triphenyl phosphite, tris (2, 4-t-butylphenyl) phosphite, ethyltriphenylphosphonium bromide, triethylamine, triphenylamine, and the like.
The binder resin that can be used in combination with the crystalline polyester resin of the present embodiment is not particularly limited. As an example, the binder resin is a styrene-based copolymer such as polystyrene, a styrene-methyl acrylate copolymer, or a styrene-acrylonitrile copolymer, or a resin material such as a polyester resin or an epoxy resin other than the crystalline polyester resin of the present embodiment. These binder resins may also be used in combination. Among these, polyesters are preferable as the binder resin to be used in combination from the viewpoint of easy coloring and obtaining a vivid color toner.
The binder resin of the present embodiment preferably contains an amorphous resin among the above resin materials. The amorphous resin preferably has a mass average molecular weight of 4000 to 150000 and a softening point of 95 to 125 ℃. The mass average molecular weight is preferably 4000 or more, more preferably 5000 or more. The mass average molecular weight is preferably 150000 or less, more preferably 12000 or less. The softening point is preferably 90 ℃ or higher, more preferably 95 ℃ or higher. The softening point is preferably 125 ℃ or lower, more preferably 120 ℃ or lower. When the mass average molecular weight and the softening point are within the above ranges, the obtained toner exhibits excellent low-temperature fixability and storage stability. In the present embodiment, the mass average molecular weight can be determined by measuring with Gel Permeation Chromatography (GPC) and converting to polystyrene, for example. Examples of the apparatus for measuring the mass average molecular weight by GPC in terms of polystyrene include, for example, Water 2690 (manufactured by Watts corporation) and PLgel 5. mu.L MIXED-D (manufactured by Polymer Laboratories, Inc.) as a column. In addition, the softening point can be determined based on ASTM E28-92.
The content of the binder resin other than the crystalline polyester resin in the present embodiment is not particularly limited. For example, the content of the binder resin is preferably 75% by mass or more in the toner. The content of the binder resin in the toner is preferably 85 mass% or less. When the content of the binder resin is within the above range, the obtained toner can easily disperse the colorant appropriately and can be easily fixed on a recording medium.
Colorants
The colorant is incorporated to provide coloring power to the toner.
The colorant is not particularly limited. For example, the colorant is a colorant such as magnetic powder exhibiting black color, such as carbon black; colorants exhibiting cyan color such as copper phthalocyanine, methylene blue, victoria blue and the like; magenta coloring agents such as rhodamine dyes, dimethylquinacridone, dichloroquinacridone, and carmine; and colorants exhibiting yellow color such as benzidine yellow, chrome yellow, naphthol yellow and diazo yellow. The colorants may be used in combination.
The content of the colorant is not particularly limited. For example, the content of the colorant in the toner is preferably 0.1 parts by mass or more and 30 parts by mass or less with respect to 100 parts by mass of the binder resin. Since a master batch in which a pigment is dispersed in a resin at a high concentration in advance is commercially available, the master batch can be purchased and used as a colorant. In this case, the amount of pigment used may be determined in consideration of the concentration of the pigment contained in the master batch so that the concentration of the pigment contained in the toner falls within the above range.
Mold release agent
The release agent is not particularly limited, and various known waxes can be used. Examples of such a method include: polyolefin waxes such as polyethylene wax and polypropylene wax; branched hydrocarbon waxes such as microcrystalline wax, and long-chain hydrocarbon waxes such as paraffin wax and saso wax; dialkyl ketone waxes such as distearyl ketone; ester waxes such as carnauba wax, montan wax, behenyl behenate, trimethylolpropane tribehenate, pentaerythritol tetrabehenate, pentaerythritol diacetate dibehenate, glycerol tribehenate, 1, 18-octadecanediol distearate, tristearate trimellitate, and distearate maleate; amide waxes such as ethylene bis behenamide and tristearamide trimellitate. A combination of release agents may be used. Of these, ester-based waxes and hydrocarbon-based waxes are preferable as the release agent.
The content of the release agent is not particularly limited. For example, the content of the release agent may be generally in the range of 1 to 30 parts by mass, preferably 5 to 20 parts by mass, per 100 parts by mass of the binder resin. The content of the release agent in the toner particles is preferably in the range of 3 to 15 mass%. By setting the content of the release agent within the above range, the obtained toner can obtain good releasability of the fixing roller from the printing surface in the fixing process at the time of printing. Further, the toner is less likely to bleed out of the release agent, and is less likely to cause charging failure, filming, and the like.
Other ingredients
The toner particles are, for example, a charge control agent other than the above. The charge control agent is preferably blended to adjust the charge amount of the toner.
The charge control agent is not particularly limited. Examples of the charge control agent include metal complexes such as nigrosine, basic dyes, and monoazo dyes; salts or complexes of carboxylic acids such as salicylic acid and dicarboxylic acids with metals such as chromium, zirconium, and aluminum; an organic dye; naphthenic acid, metal salts of higher fatty acids; and resin type charge control agents such as alkoxylated amines, quaternary ammonium salt compounds, and aromatic polycondensates. The charge control agent may be used in combination. Among these, from the viewpoint of stability of charging, it is preferable that the toner contains a resin-type charge control agent.
The content of the charge control agent is not particularly limited. For example, the toner particles may contain no charge control agent, and the content of the charge control agent is preferably 0.5 mass% or more. The content of the charge control agent in the toner particles is preferably 8 mass% or less. When the content of the charge control agent is within the above range, the obtained toner is more excellent in charging property.
(external additive)
The external additive is added to the surface of the toner particles to improve the charging characteristics of the toner particles, to improve the fluidity of the toner particles in a state of being separated from the toner particles, or to improve the printability.
The external additive is not particularly limited. Examples of the external additive include negatively charged lubricant particles, positively charged lubricant particles, and inorganic oxide particles. External additives may also be used in combination. The external additive can be suitably selected and used according to the kind and purpose of the equipment.
The positively charged lubricant particles are lubricant particles that are positively charged by frictional electrification with a carrier or a charged sheet. Such lubricant particles are well known, and metal salt particles of fatty acid can be preferably exemplified. Examples of such metal salts of fatty acids include zinc stearate, aluminum stearate, calcium stearate, magnesium stearate, zinc laurate, zinc myristate, zinc palmitate, and zinc oleate, and zinc stearate and magnesium stearate are more preferable. The positively charged lubricant particles may be of a single kind or a combination of two or more kinds.
The negatively charged lubricant particles are lubricant particles that are negatively charged by frictional electrification with a carrier or a charged sheet. Such lubricant particles are well known, and Polytetrafluoroethylene (PTFE), silicone, boron nitride, polymethyl methacrylate (PMMA), and polyvinylidene fluoride are preferable examples, and among them, boron nitride and Polytetrafluoroethylene (PTFE) are more preferable examples. The negatively charged lubricant particles may be of a single kind or a combination of two or more kinds.
The inorganic oxide particles are not particularly limited. Examples of the inorganic oxide particles include silica, alumina, titania, zirconia, zinc oxide, chromium oxide, cerium oxide, antimony oxide, tungsten oxide, tin oxide, tellurium oxide, manganese oxide, and boron oxide. Inorganic oxide particles may be used in combination. Among these, silica and titania are preferable as the inorganic oxide particles in terms of excellent fluidity and excellent chargeability of the toner.
The inorganic oxide particles are preferably surface-hydrophobized. The method of the hydrophobization treatment is not particularly limited. As an example, the hydrophobization treatment method is a method comprising: a method of bringing a conventionally known hydrophobizing agent into contact with the surface of the inorganic oxide particles before the hydrophobizing treatment to bond or attach a hydrophobic functional group or a compound of components to the surface of the inorganic oxide particles. The hydrophobizing agent for hydrophobizing the inorganic oxide particles is not particularly limited. Examples of the hydrophobizing agent include octyl triethoxysilane, polydimethylsiloxane, dimethyldichlorosilane, hexamethyldisilazane, and the like. The hydrophobizing treatment agent may be used in combination.
The amount of the external additive (the total amount of the external additives when a plurality of external additives are used) in the present embodiment is preferably in the range of 0.05 to 5 parts by mass, and more preferably in the range of 0.1 to 3 parts by mass, per 100 parts by mass of the toner. When the content of the external additive is within the above range, the obtained toner is excellent in fluidity, charging property, cleaning property, and the like.
As described above, the toner of the present embodiment includes the crystalline polyester resin, the crystalline polyester resin includes sebacic acid as an acid component and 1, 10-decanediol as an alcohol component, and has a mass average molecular weight of 3000 to 5000, and is included in the binder resin by 5 to 10 mass%. This toner can achieve both excellent low-temperature fixability and storage stability.
< method for producing toner for developing electrostatic image >
A method for producing a toner for electrostatic image development (hereinafter also referred to as a toner production method) according to an embodiment of the present invention is a method for producing the toner for electrostatic image development, and includes a step of kneading, cooling and solidifying the kneaded product, and then pulverizing and classifying the kneaded product. The above-described steps are all steps employed in a conventionally known toner manufacturing method. That is, the method for producing a toner according to the present embodiment can produce a toner by a conventionally known method using a conventionally known production apparatus.
More specifically, first, in the kneading step, each component of the toner particles is melt-kneaded to prepare a kneaded product. Various conventionally known mixing devices (for example, a double cone mixer, a V-type mixer, a tumbler mixer, a super mixer, a Henschel mixer, a nauta mixer, and a Mechano Hybrid (manufactured by COKE industries, Ltd.) can be used for mixing the components). In melt kneading, a batch kneader such as a pressure kneader or a banbury mixer or a continuous kneader can be used, and a single-screw or twin-screw extruder has been mainly used because of its advantage of enabling continuous production. Examples thereof include a KTK type twin screw extruder (manufactured by KANSHEN Co., Ltd.), a TEM type twin screw extruder (manufactured by TOYOBO MACHINES, Ltd.), a PCM Kneader (manufactured by KARSU CULTIVA, Ltd.), a twin screw extruder (manufactured by KCK Co., Ltd.), a Ko-Kneader (manufactured by BUSS Co., Ltd.), and a Kneadex (manufactured by COKE INDUSTRIAL CO Ltd.). As the toner material, a master batch containing the binder resin and the colorant may be used.
The kneaded mixture is then cooled, and the cooled kneaded mixture is pulverized (for example, coarsely pulverized by a pulverizer such as a crusher, a hammer mill, or a Feather, and then finely pulverized by, for example, a Kryptron system (manufactured by kawasaki heavy industries), a super rotor (manufactured by Nisshin Engineering, inc.), a Turbo mixer (manufactured by Freund Turbo), or a jet type micro pulverizer). The powder (pulverized material) obtained in the pulverization step is classified (for example, by using a classifier or a sieving machine such as an Elbow Jet (manufactured by Nippon iron mining Co., Ltd.) of an inertial classification system, a Turbo Plex (manufactured by Hosokawa Micron) of a centrifugal classification system, a TSP separator (manufactured by Hosokawa Micron) or a Faculty (manufactured by Hosokawa Micron)). The volume median particle diameter (D50) of the pulverized and classified toner particles is preferably 4 to 10 μm. In the present embodiment, the volume median diameter (D50) is also referred to as a volume-based median diameter, and indicates that the volume total of particles having a diameter smaller than this value and the volume total of particles having a diameter larger than this value account for 50% of the volume total of the whole. The volume median particle diameter (D50) can be calculated by performing particle size distribution measurements. The particle size distribution measuring apparatus may be exemplified by "Multisizer 3" manufactured by Beckmann Coulter.
As described above, the method for producing a toner according to the present embodiment does not require a special apparatus, and can produce a toner using the same apparatus as the conventional apparatus. As described above, the obtained toner can achieve both excellent low-temperature fixability and storage stability. Therefore, according to the present manufacturing method, the cost increase of the toner can be prevented.
The above description has been directed to an embodiment of the present invention. The present invention is not particularly limited to the above embodiments. The above embodiments mainly explain the invention having the following configurations.
(1) A toner for developing an electrostatic image, comprising toner particles and an external additive, wherein the toner particles comprise a binder resin containing a crystalline polyester resin, a colorant and a release agent, the crystalline polyester resin comprises sebacic acid as an acid component and 1, 10-decanediol as an alcohol component, and has a mass average molecular weight of 3000 to 5000, and the toner particles contain 5 to 10% by mass.
With this configuration, the obtained toner for developing electrostatic images can achieve both low-temperature fixing properties and storage stability.
(2) The toner for developing electrostatic images according to (1), wherein the crystalline polyester resin has a melting point of 70 to 76 ℃.
With this configuration, the electrostatic image developing toner can be favorably fixed at a low temperature.
(3) The toner for developing an electrostatic image according to (1) or (2), wherein the binder resin comprises an amorphous resin, and the amorphous resin has a mass average molecular weight of 4000 to 150000 and a softening point of 90 to 125 ℃.
With this configuration, the electrostatic image developing toner can achieve both excellent low-temperature fixing properties and excellent storage stability.
(4) The electrostatic image developing toner according to any one of (1) to (3), further comprising a resin-type charging control agent.
With this configuration, the electrostatic image developing toner is more excellent in charging performance.
(5) A method for producing the toner for electrostatic image development according to any one of (1) to (4), comprising a step of kneading, cooling and solidifying the kneaded product, and then pulverizing and classifying the kneaded product.
With this configuration, the obtained toner for developing electrostatic images can achieve both low-temperature fixing properties and storage stability. In addition, the toner for electrostatic image development can be manufactured using the same apparatus as the existing apparatus. Therefore, according to the present manufacturing method, the cost increase of the toner can be prevented.
Examples
The present invention will be described more specifically with reference to examples. The present invention is not limited to these examples in any way. Unless otherwise specified, "%" represents "% by mass" and "parts" represents "parts by mass".
The raw materials used and the preparation method are shown below.
< Binder resin >
Crystalline polyester resin
Crystalline polyester resin 1: polyesters of sebacic acid with 1, 10-decanediol. Mass-average molecular weight 3000 and melting point 74 ℃.
Crystalline polyester resin 2: polyesters of sebacic acid with 1, 10-decanediol. Mass average molecular weight of 5000, melting point of 74 ℃.
Crystalline polyester resin 3: polyesters of sebacic acid with 1, 10-decanediol. Mass average molecular weight 5000, melting point 75 ℃.
Crystalline polyester resin 4: polyesters of sebacic acid with 1, 6-hexanediol. Mass average molecular weight 2600, melting point 66 ℃.
Crystalline polyester resin 5: polyesters of sebacic acid with 1, 6-hexanediol. Mass average molecular weight 5000, melting point 67 ℃.
Crystalline polyester resin 6: polyesters of sebacic acid with 1, 6-hexanediol. Mass average molecular weight 10000, melting point 69 ℃.
Crystalline polyester resin 7: polyesters of sebacic acid with 1, 10-decanediol. Mass average molecular weight 10000, melting point 74 ℃.
Crystalline polyester resin 8: polyesters of 1, 12-dodecanedioic acid with 1, 6-hexanediol. Mass average molecular weight 3500 and melting point 71 ℃.
Crystalline polyester resin 9: polyesters of 1, 12-dodecanedioic acid with 1, 10-decanediol. Mass-average molecular weight 3000 and melting point 78 ℃.
Amorphous binder resins used in combination
Amorphous binder 1: commercially available noncrystalline polyester resin (Tg64 ℃, molecular weight 5500)
Amorphous binder 2: commercially available amorphous polyester resin (Tg65 ℃, molecular weight 110,000)
< Charge control agent >
Under the trade name Copy Charge N5P-01 (manufactured by Clariant Chemicals Co., Ltd.)
< coloring agent >
Carbon black
< Release agent >
Mold release agent 1: fatty acid ester wax (melting point 69 ℃ C.)
And (2) release agent: hydrocarbon wax
< external additive >
External additive 1: silica particles surface-treated with Silicone oil (particle diameter: 22nm)
External additive 2: silica particles surface-treated with dimethyldichlorosilane (particle size 12nm)
External additive 3: titanium oxide particles surface-treated with alkylsilane (particle diameter: 14nm)
< examples 1 to 4, comparative examples 1 to 14 >
(preparation of toner)
Crystalline polyester resin, commercially available polyester resin (Tg64 ℃, molecular weight 5500, non-crystalline), commercially available polyester resin (Tg65 ℃, molecular weight 110,000, non-crystalline), fatty acid ester wax (melting point 69 ℃), hydrocarbon wax, charge control agent, and carbon black were mixed in the mass ratios (mass%) shown in Table 1 below, and then melt-kneaded with a twin-screw kneader. The resulting kneaded product was coarsely pulverized by Rotoplex, finely pulverized by a jet mill, and classified by an air classifier to obtain toner base particles having a charged volume average particle diameter of 6.5 μm. 1.0% of silica particles surface-treated with silicone oil (particle diameter: 22nm), 0.5% of silica particles surface-treated with dimethyldichlorosilane (particle diameter: 12nm), and 0.5% of titanium oxide particles surface-treated with alkylsilane (particle diameter: 14nm) were added to 100 parts by mass of the toner base particles, and the mixture was stirred with a Henschel mixer for 10 minutes to obtain toners of examples and comparative examples.
[ TABLE 1 ]
TABLE 1
With respect to the toners of the examples and comparative examples obtained above, printed matters were produced under the following conditions, and the fixing property, the releasing property, and the storage stability were evaluated. The results are shown in Table 1.
< evaluation of fixing ratio >
Using a non-magnetic two-component type negatively charged printer for evaluation, plain paper (80 g/m) was set at a temperature of 25 ℃ and a humidity of 50%2) A plain image (solid image) was printed thereon, and the plain image was subjected to a rubbing test under the following conditions using a shaking resistance rubbing fastness tester (NR-100, manufactured by Daorhiki Kaisha Seisaku Kogyo Co., Ltd.). The image density of the image before and after rubbing was measured using a reflection densitometer (manufactured by Macbeth corporation), and the fixing ratio was calculated by the following equation.
Friction surface: nonwoven (product name COTTON PADS manufactured by Honeylon corporation)
Loading: 500g
The reciprocating times are as follows: 5 times (twice)
Horizontal reciprocating distance: 10cm
Fixing ratio (%): (image density after rubbing/image density before rubbing) × 100
O: the fixing ratio is 85% or more.
And (delta): the fixing ratio is 80% or more and less than 85%.
X: the fixing ratio was less than 80%.
< evaluation of paper end fixability (N/N Environment) >)
10 sheets of 100% covered blanket images were continuously printed at 25 ℃ and 50% humidity using a nonmagnetic two-component negatively charged printer for evaluation.
O: in all the portions from the center to the end of the sheet, peeling due to scratching of the image did not occur.
And (delta): only the end of the paper is peeled off by scratching the image.
X: peeling occurred at both the center and the end of the paper due to scratching of the image.
< evaluation of paper end fixability (L/L Environment) >)
10 sheets of 100% covered blanket images were continuously printed at 10 ℃ and 20% humidity using a nonmagnetic two-component negatively charged printer for evaluation.
O: in all the portions from the center to the end of the sheet, peeling due to scratching of the image did not occur.
And (delta): only the end of the paper is peeled off by scratching the image.
X: peeling occurred at both the center and the end of the paper due to scratching of the image.
< evaluation of releasability >
Using a nonmagnetic two-component type negatively charged printer for evaluation, a full-print image with 100% coverage was printed on plain paper (64g/m2), and the paper was wound around a fixing device to evaluate the occurrence of peeling marks and offset stains on the fixing roller.
O: the sheet was wound around a fixing device, and no peeling mark or offset dirt was generated on the fixing roller.
X: the sheet was wound around a fixing device, and either a peeling mark of the fixing roller or offset dirt was generated.
< storage stability 50 ℃/8 h >
20g of the toner was put in a sealed plastic container and stored at 50 ℃ for 8 hours, and then evaluated by a powder tester (made by Hosokawa Micron Co., Ltd.). A sieve A (mesh size: 355 μm), a sieve B (mesh size: 250 μm) and a sieve C (mesh size: 150 μm) were placed one on top of the other in this order, 20g of the toner was put on the sieve A, and the resultant toner was vibrated at an amplitude of 1mm for 30 seconds to measure the weight of the remaining toner.
The degree of aggregation calculated as follows was evaluated.
Degree of aggregation%: (toner (g) remaining on Screen A) + toner (g) remaining on Screen B. times.0.6 + toner (g) remaining on Screen A. times.0.2)/20X 100
O: the aggregation degree is less than 10%.
And (delta): the degree of aggregation is 10% or more and less than 20%.
X: the aggregation degree is more than 20%.
< storage stability 55 ℃/8 h >
20g of the toner was put in a sealed plastic container and stored at 55 ℃ for 8 hours, and then evaluated by a powder tester (made by Hosokawa Micron Co., Ltd.). A sieve A (mesh size: 355 μm), a sieve B (mesh size: 250 μm) and a sieve C (mesh size: 150 μm) were placed one on top of the other in this order, 20g of the toner was placed on the sieve A, and the resultant toner was vibrated at an amplitude of 1mm for 30 seconds to measure the weight of the remaining toner.
The degree of aggregation calculated as follows was evaluated.
Degree of aggregation%: (toner (g) remaining on Screen A) + toner (g) remaining on Screen B. times.0.6 + toner (g) remaining on Screen A. times.0.2)/20X 100
O: the aggregation degree is less than 10%.
And (delta): the degree of aggregation is 10% or more and less than 20%.
X: the aggregation degree is more than 20%.
As shown in Table 1, the toners of examples 1 to 4 were excellent in fixability, offset and storage stability. On the other hand, the toners of comparative examples 1 to 8 using the crystalline polyester containing the alcohol component having a small carbon number did not satisfy both of the fixing property and the storage stability. The toner of comparative example 9 using the crystalline polyester having a large molecular weight had poor fixing ability to the end of the paper in an environment of 10 ℃ and 20% humidity. The toners of comparative examples 10 and 11 using the crystalline polyester containing the carboxylic acid component having a large number of carbon atoms and the alcohol component having a small number of carbon atoms did not satisfy both the fixing property and the storage stability. In addition, the toner of comparative example 12 using the crystalline polyester containing the carboxylic acid component having a large number of carbon atoms and the alcohol component having a large number of carbon atoms was inferior in the fixing property to the paper edge portion in the environment of 10 ℃ temperature and 20% humidity. Further, the toner of comparative example 13 containing a small amount of the crystalline polyester resin of the present invention is inferior in fixability, and the toner of comparative example 14 containing a large amount thereof is inferior in storage stability.
Claims (5)
1. A toner for developing an electrostatic image, comprising toner particles and an external additive,
the toner particles contain a binder resin containing a crystalline polyester resin, a colorant, and a release agent,
the crystalline polyester resin:
comprising sebacic acid as an acid component, 1, 10-decanediol as an alcohol component,
the mass-average molecular weight is 3000-5000,
the toner particles contain 5 to 10 mass%.
2. The electrostatic image developing toner according to claim 1, wherein,
the crystalline polyester resin has a melting point of 70-76 ℃.
3. The toner for developing electrostatic images according to claim 1 or 2, wherein,
the binder resin comprises an amorphous resin and a binder resin,
the mass average molecular weight of the amorphous resin is 4000-150000, and the softening point is 90-125 ℃.
4. The electrostatic image developing toner according to any one of claims 1 to 3, further comprising a resin-type charge control agent.
5. A method for producing the toner for developing electrostatic images according to any one of claims 1 to 4,
comprises a step of kneading, cooling and solidifying, and then crushing and classifying.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2018092544A JP2019197195A (en) | 2018-05-11 | 2018-05-11 | Toner for electrostatic charge image development and method for producing toner for electrostatic charge image development |
| JP2018-092544 | 2018-05-11 | ||
| PCT/JP2019/018763 WO2019216420A1 (en) | 2018-05-11 | 2019-05-10 | Toner for electrostatic charge image development and process for producing toner for electrostatic charge image development |
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| CN112119356A true CN112119356A (en) | 2020-12-22 |
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| CN201980030990.4A Pending CN112119356A (en) | 2018-05-11 | 2019-05-10 | Toner for developing electrostatic image and method for producing toner for developing electrostatic image |
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| Country | Link |
|---|---|
| JP (1) | JP2019197195A (en) |
| KR (1) | KR102563008B1 (en) |
| CN (1) | CN112119356A (en) |
| TW (1) | TWI719475B (en) |
| WO (1) | WO2019216420A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR890002505B1 (en) * | 1986-03-19 | 1989-07-10 | 유니온케미칼 주식회사 | Manufacture of toner for developing of a static electric charge |
| JP3633137B2 (en) * | 1996-09-02 | 2005-03-30 | 東洋紡績株式会社 | Toner for developing electrostatic image and fixing method of toner for developing electrostatic image |
| JP4973129B2 (en) * | 2006-11-02 | 2012-07-11 | 富士ゼロックス株式会社 | Method for producing toner for developing electrostatic image |
| JP5361046B2 (en) | 2008-12-11 | 2013-12-04 | 花王株式会社 | Method for producing toner for developing electrostatic image |
| JP5987590B2 (en) * | 2012-09-21 | 2016-09-07 | 富士ゼロックス株式会社 | Electrostatic image developing toner, electrostatic image developer, toner cartridge, process cartridge, image forming apparatus, and image forming method |
| JP2014077934A (en) * | 2012-10-11 | 2014-05-01 | Fuji Xerox Co Ltd | Toner for electrostatic charge image development, electrostatic charge image developer, toner cartridge, process cartridge, image forming apparatus, and image forming method |
| JP6304584B2 (en) | 2014-02-21 | 2018-04-04 | 学校法人慶應義塾 | Dispersion solution and method for producing the same, coating solution and method for producing mesoporous silica porous membrane |
| JP6439708B2 (en) * | 2016-01-20 | 2018-12-19 | 京セラドキュメントソリューションズ株式会社 | Magnetic toner |
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2019
- 2019-05-10 TW TW108116288A patent/TWI719475B/en active
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| Publication number | Publication date |
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| JP2019197195A (en) | 2019-11-14 |
| KR20210008332A (en) | 2021-01-21 |
| TWI719475B (en) | 2021-02-21 |
| TW202001449A (en) | 2020-01-01 |
| WO2019216420A1 (en) | 2019-11-14 |
| KR102563008B1 (en) | 2023-08-03 |
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