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CN100432842C - Non-magnetic monocomponent toner having excellent developing property at low temperature condition - Google Patents

Non-magnetic monocomponent toner having excellent developing property at low temperature condition Download PDF

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Publication number
CN100432842C
CN100432842C CNB2004800028020A CN200480002802A CN100432842C CN 100432842 C CN100432842 C CN 100432842C CN B2004800028020 A CNB2004800028020 A CN B2004800028020A CN 200480002802 A CN200480002802 A CN 200480002802A CN 100432842 C CN100432842 C CN 100432842C
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CN
China
Prior art keywords
toner
organic fine
weight portion
particle
bma
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Expired - Fee Related
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CNB2004800028020A
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CN1742237A (en
Inventor
李源涉
李昶淳
林仁熙
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LG Corp
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LG Chemical Co Ltd
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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
    • G03G9/09708—Inorganic compounds
    • G03G9/09716—Inorganic compounds treated with organic compounds
    • 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
    • G03G9/083—Magnetic toner particles
    • G03G9/0831—Chemical composition of the magnetic components
    • G03G9/0832—Metals
    • 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
    • G03G9/083—Magnetic toner particles
    • G03G9/0831—Chemical composition of the magnetic components
    • G03G9/0834—Non-magnetic inorganic compounds chemically incorporated in magnetic components
    • 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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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Developing Agents For Electrophotography (AREA)

Abstract

The present invention relates to a non-magnetic mono-component toner composition and a preparation method thereof. Disclosed is a non- magnetic mono-component toner composition prepared by coating spherical organic fine particle having a weight-average molecular weight (Mw) of 250,000-1,600,000 and an average particle size of 50-500 nm, a hydrophobic silica, and a metal oxide fine particle on a toner mother particle. The non-magnetic mono-component toner composition of the present invention ensures smooth toner supply because of good fluidity, reduces PCR contamination and deterioration of image quality, enables uniform toner layer formation on the development roller, prevents blocking at the blade of the development roller, and solves the low temperature double image problemin the non-imaging region at a low temperature. Therefore, it can be useful for an image printing apparatus adopting the non-magnetic mono-component development system in which the developing roller contacts the photoreceptor.

Description

Non-magnetic monocomponent toner and preparation method thereof
Technical field
The present invention relates to a kind of non-magnetic monocomponent toner composition and method of making the same, this method for producing toner and toner is used to the non-magnetic mono-component toning system that wherein developer roll and photoreceptor are in contact with one another.
Background technology
Usually, the dry development method in the electrophotography (electrophotography) can mainly be divided into bi-component toning system that uses the two-component developing agent that comprises toner and carrier and the single component development system that uses the monocomponent toner that only comprises toner.Between, the single component development system is favourable on compactedness, cost and maintenance.The single component development system is according to using magnetic color tuner or nonmagnetic toner further to be classified.Use the system of nonmagnetic toner to be possible thereby to be favourable owing to colour print.Therefore, use the duplicating machine and the printer of non-magnetic mono-component toning system to begin to be widely used, and print speed significantly is improved.
Be different from the bi-component toner that uses the two-component developing agent that comprises the carrier that helps the toner-particle transfer or utilize magnetic force to shift the magnetic color tuner of toner-particle, in non-magnetic monocomponent toner, the flowability of toner itself has influenced transfer characteristics widely.That is to say that flowability is the most important physical properties of non-magnetic monocomponent toner.It influences greatly duplicates and the conversion characteristic of the quality of print image, image density, not fogging Chu (image contamination that causes from the toner of non-image areas transfer), toner etc.If toner-particle has inadequate flowability, then break in duplicating or print image (stripped line) pollutes.This is because non-magnetic monocomponent toner is stuck in developer roll and be used to developer roll that zone between the lower roll of toner is provided, and is not therefore successfully transferred to developing roller surface.
Except mobile and toner obstruction, the characteristic of toner that relates to the charging device of photoreceptor also is important characteristic.Usually, the charging device that duplicates or print is divided into charger wherein and does not contact the type (as charger) of photoreceptor contacts photoreceptor with charger wherein method (as the roller charging device).In both, the rod charging method is widely adopted owing to producing less ozone.In the rod charging method, former charging roller (PCR) contacts with photoreceptor to give the surface charging of photoreceptor.And if contaminated, then generation is as the image contamination of fuzzy and inhomogeneous image owing to toner attached thereto on the surface of PCR.Especially, because flowability reduces at low temperatures further, toner is easy to be firmly adhered on the surface of PCR, thereby weakens charge characteristic and transfer efficiency.
In order to improve the flowability and the charging ability of toner at low temperatures, the fine grained such as the silicon dioxide that are easy to move are included in the toner.Fine grained has reduced the clinging power of toner to drum, thereby has improved transfer efficiency.In order to obtain good transfer efficiency, many fine graineds have to be applied on the surface of toner, but this may cause the charging ability that reduces toner, and fine grained reduces the adhesiveness of carrier, thereby can cause electrostatic latent image etc., film formation, fixation problem etc.Especially, because silica dioxide granule depends on environment widely, inhomogeneous image can issue life at low temperature and low moisture, and can take place under high temperature and high humidity in the pollution of non-image areas.
In order to solve the environmental factor dependence of toner charging, the fine inorganic particles such as the titania that have than low resistance and good charge interchangeability with respect to silica dioxide granule are added into.But the CHARGE DISTRIBUTION of toner can easily change in this case.
In order to address this problem, be proposed by method with the increase resistance on processing fine inorganic particles surfaces such as silane coupling agent.In this case, fine grained has stronger congealing property, thereby reduces and the minimizing of electric charge interchangeability in the dispersiveness of toner surface, and this can cause reducing of toner flowability or the obstruction that is caused by the particle that freely condenses.
And, be different from toner wherein easily is transported to developer roll by magnetic pull magnetic mono-component toner, when using non-magnetic monocomponent toner, the thickness of toner layer is conditioned by being pressed onto on the developer roll by the blade that metal or rubber are made, and toner is recharged.Therefore, because pressure is applied on the non-magnetic monocomponent toner, so if service time is very long, then toner can block developer roll and blade, this makes the thickness of the toner layer on the developer roll and level of charge inhomogeneous, thereby causes the unclear or shade of image.
In order to stop toner to block, glass transition temperature (Tg) and its molecular weight of the adhesive resin that contains in the female particle of toner are increased.But this makes the pre-arcing characterisitics of toner inevitably and coagulates the smoothness of taking a group photo as (fused image) and worsens, and makes image inhomogeneous.Although this method prevents that at high temperature the obstruction of toner on developer roll is favourable, but owing to remove and do not remain in the lip-deep toner of photoreceptor, low temperature afterimage problem at low temperatures, especially take place in the non-magnetic mono-component toning system that omits cleaning course.
Therefore, for the non-magnetic mono-component toning system that the contact photoreceptor of developer roll wherein and cleaning course are omitted, the change of opposing environment and the non-magnetic monocomponent toner that can solve low temperature afterimage problem are necessary.
Summary of the invention
Technical scheme of the present invention provides a kind of non-magnetic monocomponent toner with good fluidity, thus glibly supplying toner, reduced PCR pollution and deterioration of image, make and forming uniform toner layer on the developer roll and preventing the obstruction on the blade at developer roll simultaneously and solve low temperature slur in the non-image areas at low temperatures as problem.
Embodiment
In following detailed description, embodiments of the invention are implemented the present inventor by explanation and are thought that optimum pattern is described and illustrates.Be appreciated that the present invention can be modified in many aspects, all such modifications do not break away from the present invention.Therefore, instructions is considered to explanation in itself, rather than restrictive.
In order to obtain this technical scheme, the invention provides a kind of non-magnetic monocomponent toner composition and comprise:
A) comprise the female particle of toner of adhesive resin, colorant and charge adjusting agent;
B) based on the female particle of the toner of per 100 weight portions, what contain 0.05～2.5 weight portion, preferred 0.1～2.0 weight portion has 1,000,000～1, the spherical organic fine grained of the particle mean size of 600,000 weight average molecular weight (Mw) and 50～500nm, preferred 100～300nm;
C), contain the 20～80m that has of 0.5～1.5 weight portion based on the female particle of the toner of per 100 weight portions 2/ g, preferred 30～50m 2The hydrophobic silica of the specific surface area of/g; With
D) based on the female particle of the toner of per 100 weight portions, contain the metal oxide fine particles of the particle mean size with 50～500nm, preferred 60～300nm of 0.3～2.5 weight portion, preferred 0.5～2.0 weight portion,
Wherein, spherical organic fine grained i) have and be at least 0.92 the circularity mean value R that equation is calculated that passes through:
R＝L 0/L 1
Wherein, L 1For being the girth of organic fine grain projection image of unit with nm, and L 0For with nm being the girth with organic fine grain projected area circle of the same area of having of unit.
More specifically, the non-magnetic monocomponent toner composition comprises:
A) the female particle of the toner of the charge adjusting agent of the colorant of the adhesive resin that comprises 100 weight portions of 100 weight portions, 3～20 weight portions and 0.5～5 weight portion;
B) 0.05～2.5 weight portion has (Mw) 1,000,000～1, a spherical organic fine grained of 600,000 weight average molecular weight and the particle mean size of 50～500nm;
C) 0.5～1.5 weight portion has 20～80m 2The hydrophobic silica of the specific surface area of/g; With
D) metal oxide fine particles of the particle mean size with 50～500nm of 0.3～2.5 weight portion,
Wherein, spherical organic fine grained i) have and be at least 0.92 the circularity mean value R that equation is calculated that passes through:
R＝L 0/L 1
Wherein, L 1For being the girth of organic fine grain projection image of unit with nm, and L 0For with nm being the girth with organic fine grain projected area circle of the same area of having of unit.
The present invention also provides the method for preparing non-magnetic monocomponent toner, comprises step:
Mix, mediate, pulverize and sieve adhesive resin, colorant and charge adjusting agent with the female particle (step 1) of preparation toner; With
Use stirrer with female particle of toner and i) have (Mw) 1,000,000～1, the spherical organic fine grained of 600,000 weight average molecular weight and the particle mean size of 50～500nm; Ii) has 20～80m 2The hydrophobic silica of the specific surface area of/g and the metal oxide fine particles mixing (step 2) that iii) has the particle mean size of 50～500nm:
Wherein, spherical organic fine grained i) have and be at least 0.92 the circularity mean value R that equation is calculated that passes through:
R＝L 0/L 1
Wherein, L 1For being the girth of organic fine grain projection image of unit with nm, and L 0For with nm being the girth with organic fine grain projected area circle of the same area of having of unit.
More specifically, this preparation method comprises step:
The charge adjusting agent that mixes, mediates, pulverizes and sieve the colorant of adhesive resin, 3～20 weight portions of 100 weight portions and 0.5～5 weight portion is with the female particle (step 1) of preparation toner; With
Use stirrer with female particle of the toner of 100 weight portions and i) 0.05～2.5 weight portion have (Mw) 1,000, the spherical organic fine grained of 000～1,600,000 weight average molecular weight and the particle mean size of 50～500nm, ii) 0.5～1.5 weight portion has 20～80m 2The hydrophobic silica of the specific surface area of/g and the iii) metal object fine grained mixing (step 2) of the particle mean size with 50～500nm of 0.3～2.5 weight portion:
Wherein, spherical organic fine grained i) have and be at least 0.92 the circularity mean value R that equation is calculated that passes through:
R＝L 0/L 1
Wherein, L 1For being the girth of organic fine grain projection image of unit with nm, and L 0For with nm being the girth with organic fine grain projected area circle of the same area of having of unit.
The female particle of toner has the particle mean size of 5～25 μ m, but is not restricted to this scope, and the female particle of toner can be mediated by fusing, pulverizes, polymerization etc. is produced.The female particle of toner can comprise further that separant is to stop the skew of particle.
The present inventor efforts be made so that the non-magnetic monocomponent toner that developer roll can contact with photoreceptor, and this non-magnetic monocomponent toner can be resisted the environment change in the cleaning abridged non-magnetic mono-component toning system wherein and can solve the low temperature slur as problem.In this process, they find comprising adhesive resin, comprise having (Mw) 250 on the female particle surface of the toner of colorant and charge adjusting agent, 000～1, the spherical organic fine grained of 600,000 weight average molecular weight and the particle mean size of 50～500nm, the non-magnetic monocomponent toner composition of hydrophobic silica and metal oxide fine particles is owing to good flowability is guaranteed supplying toner glibly, having reduced PCR pollutes and deterioration of image, make and on developer roll, form uniform toner layer, and prevented obstruction on the blade of developer roll, solved at low temperatures problem simultaneously at the low temperature slur picture of non-image areas.
To provide the detailed description of the present invention below.
Adhesive resin is any coating resin.Particularly, adhesive resin can be obtained by the polymerization of alcohol and carboxylic acid.
Alcohol is dibasic alcohol or polyvalent alcohol, as the derivant of ethylene glycol, diethylene glycol, triethylene glycol, polyglycol, propylene glycol, butylene glycol, pentanediol, hexanediol, cyclohexanedimethanol, Xylene glycol, bisphenol-A, bisphenol-A epoxy ethane, bisphenol-A epoxy propane, D-sorbite and glycerine, alcohol or and composition thereof.But carboxylic acid dicarboxylic acids or polybasic carboxylic acid, as maleic acid, fumaric acid, phthalic acid, m-phthalic acid, terephthalic acid (TPA), succinic acid, hexane diacid, trimer acid (trimeritic acid), cyclopentane dicarboxylic acid, succinic anhydride, trimerization acid anhydrides (trimeriticacid anhydride) and maleic anhydride, carboxylic acid derivates, carboxylic acid anhydride or and composition thereof.
The example of adhesive resin is acrylate polymer such as polyester, poly-(methyl acrylate), poly-(ethyl acrylate), gathers (butyl acrylate), poly-(2-EHA) and gather (lauryl acrylate); Methacrylate polymers is as poly-(methyl methacrylate), poly-(butyl methacrylate), poly-(hexyl methacrylate), poly-(methacrylic acid 2-Octyl Nitrite) and poly-(lauryl methacrylate); The multipolymer of acrylate and methacrylate; The multipolymer of styrene monomer and acrylate or methacrylate; Ethene polymers is as poly-(vinyl acetate), poly-(propionate), poly-(lactic acid vinyl acetate), tygon and polypropylene and multipolymer thereof; Styrol copolymer such as Styrene-Butadiene, styrene-isoprene multipolymer and styrene-maleic acid copolymer; Poly-(vinethene); Poly-(ketenes); Polyester; Polyamide; Polyurethane; Rubber; Epoxy resin; Poly-(ethene butyral) resin; Modified resin; Phenolics; And composition thereof.Wherein, special preferred polyester.
The content of colorant should be sufficient, so that can obtain sufficient visual picture.Preferably, the adhesive resin of per 100 weight portions contains the colorant of 3～20 weight portions.
Carbon black is preferably as black colorant, and yellow, magenta and green pigment are preferably as colour colouring pigment.
For yellow colorants, the nitrogen compound of condensation, isoindoline ketonic compound, anthracene compound, azo metal complex, allylamine compound etc. can be used.Preferred particularly C.I. pigment Yellow 12, C.I. pigment yellow 13, C.I. pigment Yellow 14, C.I. pigment yellow 15, C.I. pigment yellow 17, C.I. pigment yellow 62, C.I pigment yellow 74, C.I pigment yellow 83, C.I. pigment yellow 93, C.I pigment yellow 94, C.I. pigment yellow 95, C.I. pigment yellow 109, C.I. pigment yellow 110, C.I. pigment yellow 111, C.I. pigment Yellow 12 8, C.I. pigment Yellow 12 9, C.I. pigment yellow 147, C.I. pigment yellow 168 etc.
For pinkish red colorant, the nitrogen compound of condensation, anthracene, quinacridone compound, basic-dyeable fibre color lake compound (basic dye lake compound), naphthol compound, benzimidazole, thioindigo compound, perylene compound etc. can be used.Preferred especially particularly C.I. paratonere 2, C.I. pigment red 3, C.I. paratonere 5, C.I. paratonere 6, C.I. paratonere 7, C.I. paratonere 23, C.I. pigment red 4 8:2, C.I. pigment red 4 8:3, C.I. pigment red 4 8:4, C.I. paratonere 57:1, C.I. pigment red 81: 1, C.I. paratonere 144, C.I. pigment red 146, C.I. paratonere 166, C.I. paratonere 169, C.I. paratonere 177, C.I. paratonere 184, C.I. paratonere 185, C.I. paratonere 202, C.I. paratonere 206, C.I. paratonere 220, C.I. paratonere 221, C.I. paratonere 254 etc.
For cyan colorant, copper phthalocyanine compound and derivant thereof, anthracene compound, basic-dyeable fibre color lake compound etc. can be used.Preferred especially particularly C.I. pigment blue 1, C.I. alizarol saphirol 7, C.I. pigment blue 15, C.I. pigment blue 15: 1, C.I. pigment blue 15: 2, C.I. pigment blue 15: 3, C.I. pigment blue 15: 4, C.I. pigment blue 60, C.I. alizarol saphirol 62, C.I. alizarol saphirol 66 etc.
Colorant can separately or be used in combination.Colorant also can solid solution state use.Consider the tone, chromaticity, brightness, weatherability, OHP transparency, dispersiveness etc. of colorant and select colorant.
Charge adjusting agent is used for the containing metal azo dyes, salicylic acid compound of negative charge charging etc. and is used for the nigrosine of positive charge charging, quaternary ammonium salt etc.Though restriction especially based on the bonding agent of per 100 weight portions, does not contain the charge adjusting agent of 0.5～5 weight portion.
When only having hydrophobic silica to be used in the non-magnetic monocomponent toner, flowability is significantly improved, and still, toner may blocked after long-time the use, and PCR is polluted not improvement.Therefore, spherical organic fine grained and the hydrophobic silica with particle mean size of 250,000～1,600,000 weight average molecular weight (Mw) and 50～500nm is added into together.
When using together as spherical organic fine grained of the present invention and hydrophobic silica, the charging behavior of toner is subjected to the spherical organic fine grained that exists on the toner-particle surface and the influence of the silicon dioxide around the organic granular.And in the charging process between sleeve and charging blade, the frictional resistance that is applied to toner reduces, thereby the fusing of the toner on charging blade or solids adhering can be prevented from.Therefore, can obtain stable image for a long time.
In this manual, term " spherical " is meant that R (mean value of the circularity) value of calculating by equation is at least 0.92:
R＝L 0/L 1(1)
Wherein, L 1Be the girth (nm) of organic fine grain projection image, L 0For having the girth (nm) with organic fine grain projected area circle of the same area.
Therefore, when R=1.0, obtain round accurately.This situation can be known as spherical accurately.
The spherical organic fine grained preferably has 250,000～1,600,000 weight average molecular weight (Mw) and 50～500nm, the more preferably particle mean size of 100～300nm.If weight average molecular weight is lower than 250,000, then particle may melt and be attached to the fusing roller, thereby causes pollution.On the other hand, if weight average molecular weight greater than 1,600,000, then the triboelectric charging of toner is interrupted, this can cause the deterioration of background contamination and inhomogeneous image.In addition,, then on the surface of the female particle of toner, have not enough organic fine grained, block thereby toner takes place at low temperatures if particle mean size is lower than 50nm.On the other hand, if particle mean size surpasses 500nm, then organic fine grained can be from the female particle separation of toner, and this makes the pre-arcing characterisitics of toner-particle incomplete.
Based on the female particle of the toner of per 100 weight portions, preferably contain 0.05～2.5 weight portion, the more preferably spherical organic fine grained of 0.1～2.0 weight portion.If content is lower than 0.05 weight portion, then beneficial effect is only insignificant.On the other hand, if content surpasses 2.5 weight portions, then excessive spherical organic fine grained can cause that PCR pollutes, drum pollutes and the reduction of transfer efficiency.
The spherical organic fine grained has polymer architecture and can be prepared by following monomer, as: phenylethylene, as styrene, methyl styrene, dimethyl styrene, ethyl styrene, styryl phenyl, chlorostyrene, hexyl benzene ethene, octyl group styrene and nonyl benzene ethene; Vinyl halide is as vinyl chloride and vinyl fluoride; Vinyl esters is as vinyl acetate and vinyl benzoate; Methacrylate is as methyl methacrylate, Jia Jibingxisuanyizhi, propyl methacrylate, n-BMA, isobutyl methacrylate, methacrylic acid 2-ethylhexyl and phenyl acrylate; Acrylic acid derivative is as vinyl cyanide and methacrylonitrile; Acrylate is as methyl acrylate, ethyl acrylate, butyl acrylate, phenyl acrylate; Tetrafluoroethene; And vinylidene fluoride, they can separately or be used in combination.Monomer can be used in the potpourri of styrene resin, epoxy resin, vibrin or urethane resin.
Hydrophobic silica has 20～80m 2/ g, preferred 30～50m 2The specific surface area of/g.Hydrophobic silica prevents that toner from blocking blade.If silicon dioxide has less than 20m 2The specific surface area of/g, then toner can block blade and the pattern of being stripped from may appear in the image of printing.In addition, the specific surface area of silicon dioxide surpasses 80m 2/ g, then hydrophobic silica can embed in the surface of toner-particle, thereby causes that the toner at the blade place blocks and the weakening permanance.Only when hydrophobic silica used with the spherical organic fine grained, hydrophobic silica had just stoped the toner at the blade place to block.
Here, the specific surface area of hydrophobic silica is meant the value of measuring according to the BET method.For example, specific surface area can use the commercially available High Precision Automatic gas absorption instrument that gets to measure.Inert gas, particularly nitrogen are used as absorption gas and form the needed gas absorption amount of unimolecular layer to be determined at the hydrophobic silica surface.BET specific surface area (S, m 2/ g) determine by measuring.
Preferably, based on the female particle of the toner of per 100 weight portions, hydrophobic silica is attached on the toner-particle with 0.5～1.5 weight portion.If the adhesion amount of silicon dioxide is lower than 0.5 weight portion, then the flowability of toner diminishes, and this can cause PCR pollution, uneven image and the toner obstruction at the blade place.On the other hand, if the adhesion amount of silicon dioxide surpasses 1.5 weight portions, then excessive silicon dioxide reduces pre-arcing characterisitics.
The silicon dioxide coupling agent, the silicone wet goods can be administered to or be attached to silica dioxide granule and make, its hydrophobization.
For silane coupling agent, dimethyldichlorosilane, trimethyl chlorosilane, methyl trichlorosilane, aryl phenyl dichlorosilane, benzyl dimethyl chlorosilane, bromomethyl dimethylchlorosilane, p-chlorophenyl trichlorosilane, 3-chlorophenyl trimethoxy silane, vinyltriethoxysilane, vinyltriacetoxy silane, divinyl chlorosilane, cyclohexane disilazane can be used.
For silicone oil, at 25 ℃ of silicone oils, can be used as the PE modified silicone oil of silicone oil, ammonia modified silicone oil, the silicone oil of epoxy radicals modification, the epoxy of dimethyl silicone oil, methylphenylsilicone oil, methyl hydrogen silicone oil, alkyl-modified silicone oil, the silicone oil of fluorine modification, pure modification, phenol-modified silicone oil, carboxy-modified silicone oil and sulfhydryl modified silicone oil with viscosity of 50～10000cps (centipoise).
Use the hydrophobicity processing of silicone oil not limited especially, as long as silicone oil is attached on the inorganic particle.For example, silicon dioxide is mixed when stirring in mixing channel, be added into, heat by the silicone oil that sprays with solvent dilution, and drying.
Hydrophobic silica uses as the stirrer of Scroll-type stirrer, Henschel mixer (Henschelmixer) or super stirrer or use surface modification equipment (" Nara blendes together system (NaraHybridization System) ", the mechanical company limited of Nara) and be attached to toner-particle.But the hydrophobic silica loosely is attached to toner-particle or its part can be embedded in the surface of toner-particle.
Metal oxide fine particles has the particle mean size of 50～500nm, preferred 60～300nm.If the particle mean size of metal oxide fine particles is less than 50nm or greater than 500nm, improvement then mobile and that PCR pollutes is not enough.Only when metal oxide fine particles was used with spherical organic fine grained and hydrophobic silica, metal oxide fine particles improved liquidity and PCR pollutes.
For metal oxide fine particles, titania, aluminium oxide, zinc paste, magnesium oxide, ceria, iron oxide, cupric oxide, tin oxide etc. can be used.Consider modification and availability, preferred titania.
Based on the female particle of the toner of per 100 weight portions, with 0.3～2.5 weight portion, more preferably the metal oxide fine particles of 0.5～2 weight portion is attached on the female particle of toner.If adhesion amount is lower than 0.3 weight portion, then PCR pollutes and is not enhanced.On the other hand, if adhesion amount surpasses 2.5 weight portions, then pre-arcing characterisitics variation.
For separant, it has the separant of small-molecular weight, as Tissuemat E, polypropylene wax, olefin resin with small-molecular weight can be used.In addition, fatty acid metal salts can be used.For the olefin resin with small-molecular weight, the multipolymer of polypropylene, tygon, propylene-ethylene etc. can be used.For fatty acid, the natural acid or the synthetic fatty acid that have the saturated or undersaturated of 4～40 carbon atoms and can have hydroxyl, aldehyde radical or an epoxy radicals can be used.For example, caproic acid, sad, capric acid, lauric acid, myristic acid, palmitic acid, palmitoleic acid, stearic acid, oleic acid, linoleic acid, arachidic acid, mountain Yu's acid (behenic acid), erucic acid (erucic acid), montanic acid (montanic acid), isostearic acid, 9,10-epoxystearic acid etc. can be used.The separant that preferably contains 0.05～5 weight portion based on the adhesive resin of per 100 weight portions.Especially, optimization polypropylene.
Hereinafter, will be explained in more detail the present invention by embodiment.But the following examples only are used to understand the present invention, and unrestricted the present invention.
Embodiment
Embodiment 1
1) preparation of the female particle of toner
Use Henschel mixer to mix the component of listing in the following table 1.Potpourri uses two extruders to be melted and to mediate under 155 ℃, uses the jet grinding comminutor to be pulverized, and uses air classifier by sub-sieve, thereby acquisition has the female particle of toner of volume-particle mean size of 8.9 μ m.
Table 1
Kind Component Blending ratio (weight portion)
Adhesive resin Vibrin 100
Colorant Carbon black 10
Charge adjusting agent The containing metal diazo salt 3
Separant Polypropylene with molecular weight 3
2) non-magnetic monocomponent toner preparation of compositions
Based on the female particle of the toner of the preparation of per 100 weight portions, use the have 60m of Henschel mixer with the organic fine grain polystyrene of the conduct-methacrylic acid n-butyl ester (PS/BMA) of the particle mean size with 250,000 weight average molecular weight (Mw) and 50nm of 0.1 weight portion, 0.5 weight portion 2The titania as the particle mean size with 100nm of the hydrophobic silica of hydrophobic silica and 1.0 weight portions of the specific surface area of/g as metal oxide fine particles mixes with the female particle of toner and and stirred 5 minutes, thereby the acquisition non-magnetic monocomponent toner.
Embodiment 2～96 and comparative example 1～16
Except polystyrene-organic fine grained of methacrylic acid n-butyl ester, the fine grain consumption of hydrophobic silica and oxidized metal change into the amount shown in the following table 2～4, prepare non-magnetic monocomponent toner with the method identical with embodiment 1.
Table 2
Kind Weight-mean molecular weight (Mw, 10000) Particle mean size (nm)
PS/BMA A 25 50
PS/BMA B 25 200
PS/BMA C 25 500
PS/BMA D 80 50
PS/BMA E 80 200
PS/BMA F 80 500
PS/BMA G 160 50
PS/BMA H 160 200
PS/BMA I 160 500
PS/BMA J 15 200
PS/BMA K 200 200
PS/BMA L 80 40
PS/BMA M 80 600
Table 3
Kind Organic fine grained (weight portion) Hydrophobic silica (weight portion) Titania (weight portion)
2 PS/BMAA，0.05 0.5 1.0
3 PS/BMAA，1.5 0.5 1.0
4 PS/BMAA，2.5 0.5 1.0
5 PS/BMAA，0.05 1.0 1.0
6 PS/BMAA，1.5 1.0 1.0
7 PS/BMAA，2.5 1.0 1.0
8 PS/BMAA，0.05 1.5 1.0
9 PS/BMAA，1.5 1.5 1.0
10 PS/BMAA，2.5 1.5 1.0
11 PS/BMAB，0.05 0.5 1.0
12 PS/BMAB，1.5 0.5 1.0
13 PS/BMAB，2.5 0.5 1.0
14 PS/BMAB，0.05 1.0 1.0
15 PS/BMAB，1.5 1.0 1.0
16 PS/BMAB，2.5 1.0 1.0
17 PS/BMAB，0.05 1.5 1.0
18 PS/BMAB，1.5 1.5 1.0
19 PS/BMAB，2.5 1.5 1.0
20 PS/BMAC，0.05 0.5 1.0
21 PS/BMAC，1.5 0.5 1.0
22 PS/BMAC，2.5 0.5 1.0
23 PS/BMAC，0.05 1.0 1.0
24 PS/BMAC，1.5 1.0 1.0
25 PS/BMAC，2.5 1.0 1.0
26 PS/BMAC，0.05 1.5 1.0
27 PS/BMAC，1.5 1.5 1.0
28 PS/BMAC，2.5 1.5 1.0
29 PS/BMAD，0.05 0.5 1.0
30 PS/BMAD，1.5 0.5 1.0
31 PS/BMAD，2.5 0.5 1.0
32 PS/BMAD，0.05 1.0 1.0
33 PS/BMAD，1.5 1.0 1.0
34 PS/BMAD，2.5 1.0 1.0
35 PS/BMAD，0.05 1.5 1.0
36 PS/BMAD，1.5 1.5 1.0
37 PS/BMAD，2.5 1.5 1.0
38 PS/BMAE，0.05 0.5 1.0
39 PS/BMAE，1.5 0.5 1.0
40 PS/BMAE，2.5 0.5 1.0
41 PS/BMAE，0.05 1.0 1.0
42 PS/BMAE，1.5 1.0 1.0
43 PS/BMAE，2.5 1.0 1.0
44 PS/BMAE，0.05 1.5 1.0
45 PS/BMAE，1.5 1.5 1.0
46 PS/BMAE，2.5 1.5 1.0
47 PS/BMAF，0.05 0.5 1.0
48 PS/BMAF，1.5 0.5 1.0
49 PS/BMAF，2.5 0.5 1.0
50 PS/BMAF，0.05 1.0 1.0
51 PS/BMAF，1.5 1.0 1.0
52 PS/BMAF，2.5 1.0 1.0
53 PS/BMAF，0.05 1.5 1.0
54 PS/BMA F，1.5 1.5 1.0
55 PS/BMA F，2.5 1.5 1.0
56 PS/BMA G，0.05 0.5 1.0
57 PS/BMA G，1.5 0.5 1.0
58 PS/BMA G，2.5 0.5 1.0
59 PS/BMA G，0.05 1.0 1.0
60 PS/BMA G，1.5 1.0 1.0
61 PS/BMA G，2.5 1.0 1.0
62 PS/BMA G，0.05 1.5 1.0
63 PS/BMA G，1.5 1.5 1.0
64 PS/BMA G，2.5 1.5 1.0
65 PS/BMA H，0.05 0.5 1.0
66 PS/BMA H，1.5 0.5 1.0
67 PS/BMA H，2.5 0.5 1.0
68 PS/BMA H，0.05 1.0 1.0
69 PS/BMA H，1.5 1.0 1.0
70 PS/BMA H，2.5 1.0 1.0
71 PS/BMA H，0.05 1.5 1.0
72 PS/BMA H，1.5 1.5 1.0
73 PS/BMA H，2.5 1.5 1.0
74 PS/BMA I，0.05 0.5 1.0
75 PS/BMA I，1.5 0.5 1.0
76 PS/BMA I，2.5 0.5 1.0
77 PS/BMA I，0.05 1.0 1.0
78 PS/BMA I，1.5 1.0 1.0
79 PS/BMA I，2.5 1.0 1.0
80 PS/BMA I，0.05 1.5 1.0
81 PS/BMA I，1.5 1.5 1.0
82 PS/BMA I，2.5 1.5 1.0
83 PS/BMA E，1.5 0.5 0.3
84 PS/BMA E，1.5 0.5 2.5
85 PS/BMA E，1.5 1.0 0.3
86 PS/BMA E，1.5 1.0 2.5
87 PS/BMA E，1.5 1.5 0.3
88 PS/BMA E，1.5 1.5 2.5
Table 4
Kind Organic fine grained (weight portion) Hydrophobic silica (weight portion) Titania (weight portion)
1 PS/BMA E，1.5 1.0 0.2
2 PS/BMA E，1.5 1.0 2.6
3 PS/BMA E，1.5 0.4 1.0
4 PS/BMA E，1.5 1.6 1.0
5 - 1.0 1.0
6 - 1.0 1.0
7 PS/BMA E，1.5 - 1.0
8 PS/BMA E，1.5 - -
9 PS/BMA E，1.5 1.0 -
10 PS/BMA E，1.5 1.0 1.0
11 PS/BMA E，0.03 0.5 1.0
12 PS/BMA E，3.0 0.5 1.0
13 PS/BMA E，0.03 1.0 1.0
14 PS/BMA E，3.0 1.0 1.0
15 PS/BMA E，0.03 1.5 1.0
16 PS/BMA E，3.0 1.5 1.0
17 PS/BMA J 1.5 0.5 1.0
18 PS/BMA K 1.5 0.5 1.0
19 PS/BMA L 1.5 0.5 1.0
20 PS/BMA M 1.5 0.5 1.0
Embodiment 89
Except having 1 with 1.5 weight portions, 000, (the organic fine grained of methyl methacrylate (PMMA powder) replaces outside the PS/BMA, prepares non-magnetic monocomponent toner with the method identical with embodiment 1 for the particle mean size of 000 weight average molecular weight (Mw) and 0.1 μ m poly-.
The comparative example 21
Except having 600 with 1.5 weight portions, non-spherical (R=0.54) organic fine grained (St/BA/MMA powder) that comprises styrene-propene acid butyl ester-methacrylate of the particle mean size of 000 weight average molecular weight (Mw) and 0.15 μ m replaces outside the spherical PS/BMA, prepares non-magnetic monocomponent toner with the method identical with embodiment 89.
＜test implementation example 1 〉
Under the relative humidity of 5 ℃ of temperature and 20%, the non-magnetic monocomponent toner composition of embodiment 1～89 and comparative example's 1～21 preparation is applied to contact-type non-magnetic mono-component development printer (ML5300, Samsung Electronics), to print 5000 paper.Be printed on standard temperature and humidity (20 ℃ are carried out under 55%RH).The characteristic test of toner is as follows.
1, low temperature slur picture
Low temperature and humidity (5 ℃, 20%RH) under behind print pattern on the standard paper of predetermined number, observe whether any print image is arranged with bore hole in non-image areas.
The unparalleled picture of low temperature (good): be printed at the non-image areas pattern-free.
Low temperature has slur picture (poor): be printed at the non-image areas pattern.
2, toner blocks
Behind the paper of printing predetermined number, print complete (solid) black.Observe whether any pattern of being stripped from of being caused at the obstruction at development blade place by toner is arranged on print image.
The obstruction of no toner (good): the pattern of not being stripped from.
The obstruction of toner (poor): the pattern of on solid image, observing of being stripped from.
3, pre-arcing characterisitics
Behind the paper of printing predetermined number, print image observes whether printing identical pattern owing to incomplete fusing in non-image areas.
Not fusing incomplete (good): do not print at nonprinting region.
Fusing is (poor) not exclusively: print at nonprinting region.
Non-magnetic monocomponent toner composition by embodiment 1～89 preparation does not demonstrate low temperature slur picture, toner blocks or the fusing problem.
Comparative example 1～21 test result is as shown in table 5 below.
Kind Low temperature slur picture Toner blocks Fusing not exclusively
The comparative example 1 No Observe No
The comparative example 2 No No Difference
The comparative example 3 Observe No Difference
The comparative example 4 Observe Observe No
The comparative example 5 No Observe No
The comparative example 6 Observe Observe No
The comparative example 7 No Observe No
The comparative example 8 No No Difference
The comparative example 9 Observe No No
The comparative example 10 No Observe No
The comparative example 11 Observe No Difference
The comparative example 12 No Observe No
The comparative example 13 Observe No Difference
The comparative example 14 Observe No No
The comparative example 15 No Observe Difference
The comparative example 16 Observe Observe No
The comparative example 17 Observe Observe No
The comparative example 18 No No Difference
The comparative example 19 Observe Observe No
The comparative example 20 No No Difference
The comparative example 21 Observe Observe No
Therefore, confirm that non-magnetic monocomponent toner composition of the present invention (embodiment 1～89) is being good than comparative example 1～21 non-magnetic monocomponent toner composition aspect low temperature slur picture, toner obstruction and the pre-arcing characterisitics.In comparative example 21, be different from and use the fine grain situation of spherical organic, the toner that identifies blade blocks.And identify the increase that PCR pollutes.
By above description obviously as can be known, non-magnetic monocomponent toner composition of the present invention is guaranteed the smooth supply of the toner in the non-magnetic mono-component developing process of the contact of developer roll therein photoreceptor owing to good flowability, and has reduced PCR pollution and deterioration of image, makes and form uniform toner layer on developer roll, stop at the obstruction at the blade place of developer roll and solved the problem of the low temperature slur picture of non-image areas at low temperatures.Therefore, it can be used for adopting the wherein image printing device of the non-magnetic mono-component toning system of developer roll contact photoreceptor.

Claims (13)

1, a kind of non-magnetic monocomponent toner composition comprises:
A) the female particle of the toner of 100 weight portions, the female particle of described toner comprises the adhesive resin of 100 weight portions, the colorant of 3～20 weight portions and the charge adjusting agent of 0.5～5 weight portion;
B) 0.05～2.5 weight portion has 1,000,000～1, the spherical organic fine grained of 600,000 weight average molecular weight Mw and the particle mean size of 50～500nm;
C) 0.5～1.5 weight portion has 20～80m 2The hydrophobic silica of the specific surface area of/g; With
D) metal oxide fine particles with 50～500nm particle mean size of 0.3～2.5 weight portion,
Wherein, spherical organic fine grained b) have and be at least 0.92 the circularity mean value R that equation is calculated that passes through:
R＝L 0/L 1
Wherein, L 1For being the girth of organic fine grain projection image of unit with nm, and L 0For with nm being the girth with organic fine grain projected area circle of the same area of having of unit.
2, non-magnetic monocomponent toner composition according to claim 1, wherein the female particle of toner a) further contains the separant of 0.05～5 weight portion.
3, non-magnetic monocomponent toner composition according to claim 1, wherein spherical organic fine grained b) polymkeric substance of serving as reasons and being selected from the monomer of the group that comprises following material and preparing: styrene, methyl styrene, dimethyl styrene, ethyl styrene, styryl phenyl, chlorostyrene, hexyl benzene ethene, octyl group styrene and nonyl benzene ethene; Be selected from the vinyl halide in vinyl chloride and the vinyl fluoride; Be selected from the vinyl esters in vinyl acetate and the vinyl benzoate; Be selected from the methacrylate in methyl methacrylate, Jia Jibingxisuanyizhi, propyl methacrylate, n-BMA, isobutyl methacrylate, methacrylic acid 2-ethylhexyl and the phenyl acrylate; Be selected from the acrylic acid derivative in vinyl cyanide and the methacrylonitrile; Be selected from the acrylate in methyl acrylate, ethyl acrylate, butyl acrylate and the phenyl acrylate; Tetrafluoroethene; Vinylidene fluoride; And composition thereof.
4, non-magnetic monocomponent toner composition according to claim 1, wherein hydrophobic silica c) by silane coupling agent or silicone oil hydrophobization.
5, non-magnetic monocomponent toner composition according to claim 4, wherein silicone oil has 50～10 under 25 ℃, the viscosity of 000cps.
6, non-magnetic monocomponent toner composition according to claim 1, wherein metal oxide fine particles d) be at least a metal oxide that is selected from the group that comprises titania, aluminium oxide, zinc paste, magnesium oxide, ceria, iron oxide, cupric oxide and tin oxide.
7, a kind of method for preparing non-magnetic monocomponent toner comprises step:
Step 1: the charge adjusting agent that mixes, mediates, pulverizes and sieve the colorant of adhesive resin, 3～20 weight portions of 100 weight portions and 0.5～5 weight portion is with the female particle of preparation toner; With
Step 2: use stirrer with female particle of the toner of 100 weight portions and i) 0.05～2.5 weight portion has 1,000, the spherical organic fine grained of 000～1,600,000 weight average molecular weight Mw and the particle mean size of 50～500nm, ii) 0.5～1.5 weight portion has 20～80m 2The hydrophobic silica of the specific surface area of/g and the iii) metal oxide fine particles mixing of the particle mean size with 50～500nm of 0.3～2.5 weight portion:
Wherein, spherical organic fine grained i) have and be at least 0.92 the circularity mean value R that equation is calculated that passes through:
R＝L 0/L 1
Wherein, L 1For being the girth of organic fine grain projection image of unit with nm, and L 0For with nm being the girth with organic fine grain projected area circle of the same area of having of unit.
8, method according to claim 7 wherein, uses Henschel mixer to mix in step 1, uses two extruders to mediate, and uses the jet grinding comminutor to pulverize, and uses air classifier to carry out sub-sieve.
9, method according to claim 7, wherein, the separant of 0.05～5 weight portion is further joined in the female particle of toner in step 1.
10, method according to claim 7, wherein, the polymkeric substance of serving as reasons and being selected from the monomer of the group that comprises following material and the preparing spherical organic fine grained b of step 2): styrene, methyl styrene, dimethyl styrene, ethyl styrene, styryl phenyl, chlorostyrene, hexyl benzene ethene, octyl group styrene and nonyl benzene ethene; Be selected from the vinyl halide in vinyl chloride and the vinyl fluoride; Be selected from the vinyl esters in vinyl acetate, the vinyl benzoate; Be selected from the methacrylate in methyl methacrylate, Jia Jibingxisuanyizhi, propyl methacrylate, n-BMA, isobutyl methacrylate, methacrylic acid 2-ethylhexyl and the phenyl acrylate; Be selected from the acrylic acid derivative in vinyl cyanide and the methacrylonitrile; Be selected from the acrylate in methyl acrylate, ethyl acrylate, butyl acrylate and the phenyl acrylate; Tetrafluoroethene; Vinylidene fluoride; And composition thereof.
11, method according to claim 7, wherein the hydrophobic silica of step 2 is by silane coupling agent or silicone oil hydrophobization.
12, method according to claim 11, wherein silicone oil has 50～10 under 25 ℃, the viscosity of 000cps.
13, method according to claim 7, wherein the metal oxide fine particles of step 2 is at least a metal oxide that is selected from the group that comprises titania, aluminium oxide, zinc paste, magnesium oxide, ceria, iron oxide, cupric oxide and tin oxide.
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CN1405637A (en) * 2001-09-19 2003-03-26 株式会社理光 Dry toner and electrostatic photographic developing device using same
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US5185229A (en) * 1990-01-19 1993-02-09 Nippon Paint Co., Limited Dry toner for high speed electrophotography
JPH06266152A (en) * 1993-03-12 1994-09-22 Konica Corp Color toner
CN1131284A (en) * 1994-12-05 1996-09-18 佳能株式会社 Toner for electrostatic image development
EP0860746A2 (en) * 1997-02-20 1998-08-26 Sharp Kabushiki Kaisha Electrophotographic toner and method of manufacturing same
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