JP2006007094A - Method of manufacturing toner and surface modification device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method of manufacturing toner, which holds a high conglobation degree of the toner, has a high fine powder classifier efficiency, and does not increase a processing temperature in a device. <P>SOLUTION: The process of treating a surface modification and a classification at the same time is carried out by using a cylindrical batch type surface modification device. The surface modification device has a body casing 30, a loader 37, a grading means 35, a fine powder discharge 45, a surface modification means 32, 33 and a guiding means 36 dividing into a first space 47 and a second space 48, and a discharge 40, the guiding means having at least a cylindrical partition member, and the upper portion of the cylindrical partition member being composed of a plurality of louvers with the tip directed tangentially in an inner circumferential direction of the cylindrical partition member. When the height of the entire length of the cylindrical partition member is L0 and the height of the dispersion louvers is L1, L1/L0 is 0.1-0.5. The surface modification processed particles in which the fine powders of the predetermined particle diameter or less are removed by repeating the surface modification processing using the limited time classification and a mechanical impact force are obtained. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a method and apparatus for producing toner used in an image forming apparatus such as electrophotography, electrostatic recording, and electrostatic printing.

  Generally, the toner production method includes a pulverization method and a polymerization method. The toner produced by the pulverization method has an advantage that the production cost is lower than that of the polymerization method at present, and is widely used in copiers, printers and the like at present. When the toner is manufactured by the pulverization method, a predetermined amount of a binder resin, a colorant and the like are first mixed, melt-kneaded, cooled, pulverized, classified, and then a fluidity improver is added to manufacture the toner. .

  In recent years, copying machines and the like have been demanded to improve image quality, save energy, and cope with the environment. On the other hand, the technical concept of toner has been shifted to the spheroidization in order to achieve high transfer efficiency and to reduce waste toner. In order to achieve such a technical concept by the pulverization method, a method using a mechanical pulverization method (for example, refer to Patent Document 1), a method using hot air (for example, refer to Patent Document 2), and the like can be mentioned. However, sufficient spheroidization cannot be achieved by the mechanical impact force method. Also, when the wax is contained in the toner, the method using hot air causes the wax to start to melt on the toner surface when the wax starts to melt. Exudation occurs and it becomes difficult to control the surface properties of the toner particles, and problems remain from the viewpoint of quality stability. On the other hand, an apparatus capable of high-performance surface treatment and fine powder removal has been proposed (see Patent Document 3). However, as a problem of the present apparatus, particularly when the degree of spheroidization is maintained, the fine powder removal efficiency, so-called classification yield, tends to decrease. Further, due to the demand for further spheroidization, the spheroidizing member of the apparatus is used at high speed rotation. In such a case, the temperature inside the apparatus (hereinafter referred to as exhaust temperature) affects the toner quality. From the viewpoint of stable productivity and quality stability, the improvement is desired because the temperature rises to a temperature range (50 ° C. or higher).

Japanese Patent Laid-Open No. 9-85741 JP 2000-29241 A JP 2002-233787 A

  An object of the present invention is to provide a method and an apparatus for producing a toner that maintains a high sphericity of toner particles and has a high classification yield.

  The objective of this invention is providing the manufacturing method and apparatus which can reduce the exhaust temperature of a surface modification apparatus.

  SUMMARY OF THE INVENTION An object of the present invention is to provide a method and an apparatus for efficiently producing a toner that hardly causes image fogging.

The present invention includes a step of obtaining a finely pulverized product by melt-kneading a composition containing at least a binder resin, a wax and a colorant, cooling and solidifying the obtained kneaded product, and finely pulverizing the cooled solidified product. In the method for producing a toner, the method includes a step of obtaining toner particles obtained by simultaneously treating the surface modification and classification of the finely pulverized product.
The step of simultaneously performing the surface modification and classification is performed using a cylindrical batch type surface modification apparatus,
The surface reforming apparatus includes a cylindrical main body casing, a charging unit for charging the finely pulverized material into the main body casing, and continuously supplying fine powder having a predetermined particle size or less from the finely pulverized material charged into the main body casing to the outside of the device. Classification means for automatically discharging and removing, a fine powder discharging section for discharging fine powder removed by the classification means to the outside of the main body casing, and for treating the treated particles from which the fine powder has been removed using a mechanical impact force The surface modification means that rotates in the same direction as the rotation direction of the classification means, and the space between the classification means and the surface treatment means, the first space before being introduced into the classification means, and the fine powder by the classification means Guide means for partitioning the classified particles into a second space for introducing the particles into the surface treatment means, fine powder having a predetermined particle size or less is removed by the classification means, and surface modification treatment is performed by the surface modification means. Where Has a discharge portion for discharging outside the main casing of physical particles as the surface modified particles,
The guide means has at least a cylindrical partition member, and the upper portion of the cylindrical partition member is composed of a plurality of louvers whose tips are directed in the tangential direction of the inner circumferential circle of the cylindrical partition member, When the overall height of the partition member is L0 and the height of the dispersion louver portion is L1, L1 / L0 is 0.1 to 0.5, and the finely pulverized product is introduced into the first space. The classifying means passes through a plurality of louvers provided at the upper part of the guide means with the tips directed in the tangential direction of the inner circumferential circle of the main body casing while the finely pulverized product is swirled by a swirling flow. The fine particles having a predetermined particle size or less are continuously discharged out of the apparatus and removed by the classifying means, and introduced into the surface treatment means using mechanical impact force through the second space. By carrying out reforming treatment and circulating it again to the first space , By repeating the surface modification treatment using a fixed time classification and a mechanical impact force, fine powder under predetermined particle diameter or less have been removed, a process for producing a toner, characterized in that to obtain a surface modification treatment particles.

  Furthermore, as the present invention to be achieved more suitably, the surface modification device has an upper lid casing for holding the classification means and the discharge portion, and an upper end portion of the guide means is in close contact with the lower surface of the upper lid casing. The present invention relates to a method for producing a toner.

Further, the present invention is a batch-type surface reforming apparatus that is used in the production of toner and that simultaneously performs particle classification and spheronization treatment,
Cylindrical main body casing, input portion for supplying the finely pulverized material into the main body casing, and classifying means for continuously discharging and removing fine powder having a predetermined particle diameter or less from the finely pulverized material input into the main body casing to the outside of the apparatus. A fine powder discharger for discharging the fine powder removed by the classification means to the outside of the main body casing; and a rotation direction of the classification means for surface-treating the treated particles from which the fine powder has been removed using a mechanical impact force. Surface modification means rotating in the direction, first and second spaces provided between the classification means and the surface treatment means, the first space for introducing the particles to be treated into the classification means And a second space for introducing the particles to be treated into the surface modifying means, a guide means for partitioning the first space and the second space, and fine powder having a predetermined particle size or less by the classifying means. Removed and Has a discharge portion for discharging outside the main casing to be treated particles surface modification treatment by serial surface modification means is performed as a surface-modified particles,
The guide means has at least a cylindrical partition member, and an upper portion of the cylindrical partition member is composed of a plurality of louvers whose front ends are directed in a tangential direction of the inner circumferential direction of the cylindrical partition member, The present invention relates to a surface modification apparatus characterized in that L1 / L0 is 0.1 to 0.5, where L0 is the total length of the cylindrical partition member and L1 is the height of the dispersion louver portion.

  Furthermore, as the present invention to be achieved more preferably, the surface modification device has an upper lid casing for holding the classification means and the discharge portion, and an upper end portion of the guide means is in close contact with the lower surface of the upper lid casing. The present invention relates to a surface modification device characterized by the following.

  According to the present invention, the upper part of the guide ring is configured as a louver, so that it is possible to ensure a good classification yield by achieving a reduction in dust concentration and uniformity in the apparatus, and further in the tank. The temperature can be lowered, leading to the realization of a higher sphere by increasing the rotation speed of the dispersion rotor. Furthermore, according to the electrophotographic characteristics, it is possible to obtain a good image with little fogging.

  First, an overview of the surface modification apparatus used in the production method of the present invention will be given.

  The surface modification device of the present invention is a batch-type device that performs classification and surface modification treatment at the same time, and has a cylindrical main body casing, a charging unit for charging the finely pulverized material into the main body casing, and the main body casing. A classifying means that rotates in a predetermined direction for continuously removing fine powder having a predetermined particle size or less from the finely pulverized product to the outside of the apparatus to obtain treated particles, and the fine powder removed by the classifying means is removed from the main body casing. A fine powder discharge section for discharging the particles, a surface modification means for rotating the treated particles from which the fine powder has been removed using a mechanical impact force in the same direction as the rotation direction of the classification means, First and second spaces provided between the classification means and the surface treatment means, the first space for introducing the particles to be treated into the classification means and the surface treatment particles. To introduce to quality means Fine powder having a predetermined particle size or less was removed by the second space, the guide means for partitioning the first space and the second space, and the classification means, and the surface modification treatment was performed by the surface modification means. A discharge section for discharging the particles to be processed out of the main casing as surface-modified particles;

  FIG. 1 is a schematic cross-sectional view showing a preferred example of a surface modifying apparatus used in the present invention. 2 is an external view of the guide means in the present invention, FIG. 3 is a side view of the guide means in the present invention, and FIG. 4 is a horizontal sectional view of the louver portion of the guide means in the present invention.

  The batch type surface reforming apparatus shown in FIG. 1 includes a cylindrical main body casing 30; a top plate 43 installed so as to be openable and closable at an upper portion of the main body casing; a fine powder discharge casing 44 which is a fine powder discharge portion; Cooling jacket 31 capable of passing water; a plurality of rectangular disks 33 on the upper surface, which are attached to the central rotating shaft in the main body casing 30 as surface modification means (even number is considered in consideration of rotational balance) A dispersion rotor 32, which is a disk-like rotating body that rotates at a high speed in a predetermined direction (usually counterclockwise as viewed from the top surface of the apparatus); The liner 34 as a fixed body having a number of grooves on the surface (there is no need to have grooves on the liner surface); the surface-modified raw material particles are classified into a predetermined particle size. , A classification rotor 35 as a classifying means that rotates in the same direction as the rotation direction of the dispersion rotor 32 for continuously removing fine powder having a predetermined particle diameter or less; fine powder removed by the classification rotor 35 is outside the apparatus (that is, the main body casing). 30), a fine powder discharge port 45 as a fine powder discharge portion formed on the side surface of the main body casing 30; a cold air inlet 46 for introducing cold air into the main body casing 30; For this purpose, the raw material inlet 37 and the raw material inlet 39 serving as input portions formed on the side surface of the main casing 30; for discharging the surface-modified powder (that is, surface-modified particles) out of the main casing 30. A product discharge port 40 and a product extraction port 42 as a discharge portion of the material; and further, between the raw material input port 37 and the raw material supply port 39 so that the surface modification time can be freely adjusted. Having a product discharge valve 41 installed between the open material feed valve 38 is location and product discharge port 40 and the product extracting hole 42,.

  The surface modification apparatus further includes a guide ring 36 as a cylindrical guide means having an axis perpendicular to the top plate 43 in the main body casing 30. The upper end of the guide ring 36 is usually provided at a predetermined distance from the top plate (usually about 20 to 50 mm), and at least a part of the classification rotor 36 is installed in a state where it is covered with the cylinder. . Further, the lower end of the guide ring 36 is provided at a predetermined distance from the disk portion of the dispersion rotor 32 or the square disk 33. By this guide ring 36, the space between the classification rotor 35 and the dispersion rotor 32-liner 34 in the apparatus is divided into a first space 47 outside the cylinder and a second space 48 inside the cylinder. . Here, the first space 47 is a space for introducing the particles to be processed into the classification rotor 35, and the second space 48 is a space for introducing the particles to be processed into the dispersion rotor. Further, a gap between the plurality of rectangular disks 33 installed on the dispersion rotor 32 and the liner 34 is the surface modification zone 49, and the classification rotor 35 and the peripheral portion of the rotor are the classification zone 50.

  The finely pulverized product supplied into the apparatus from the raw material supply port 39 is outside the guide ring by the swirl flow formed by the suction air volume by the blower (not shown), the rotation of the dispersion rotor 32, and the rotation of the classification rotor 35. , While passing through the space (that is, the first space 47), the classification process is performed by reaching the classification zone 50 in the vicinity of the classification rotor 35 through the space between the upper end of the guide ring and the top plate. Here, since the direction of the swirl flow formed in the apparatus is the same as the rotation direction of the dispersion rotor 32 and the classification rotor 35, in this embodiment, it is counterclockwise as viewed from the upper surface of the apparatus.

  The fine powder to be removed by the classification means is sucked through a slit (not shown) of the classification rotor 35 and removed through the fine powder discharge port 45. The particles to be treated after the fine powder removal reaches the surface modification zone 49 in the vicinity of the dispersion rotor 32 via the second space 48, and the surface is modified by the hammer provided in the dispersion rotor 32 and the liner 34 provided in the main body casing. Quality processing is performed. The particles to be treated that have undergone surface modification reach the classification rotor 35 again while turning along the guide ring 36 described above, and the same processing is repeated. After performing the treatment for a predetermined time, the discharge valve 41 is opened, and the surface-modified particles from which fine powder having a predetermined particle diameter or less is removed can be obtained.

  As a result of intensive studies, the present inventors have found that an improvement in classification yield and a reduction in the exhaust temperature of the apparatus can be achieved by configuring the upper part of the partition member (FIG. 2) constituting the guide ring as a louver.

  That is, the guide means has at least a cylindrical partition member, and the upper portion of the cylindrical partition member is composed of a plurality of louvers whose front ends are directed in the tangential direction of the inner circumferential circle of the cylindrical partition member, This is a case where L1 / L0 is 0.1 to 0.5, where L0 is the overall height of the cylindrical partition member and L1 is the height of the dispersion louver portion.

  Here, the effects of the present invention will be described below.

  The finely pulverized product introduced into the first space of the surface modifying apparatus according to the present invention is an estimate when it reaches the vicinity of the classification rotor, but is not in a finely dispersed state in which the aggregation of powders is sufficiently solved, In the lump state, it reaches the vicinity of the classification rotor, classification is performed, and the classified one is sent to the dispersion rotor and subjected to surface modification, and a certain process is repeated. That is, it is considered that the dust density density in each part of the first space and the second space in the surface modification device is in a non-uniform state. Since it is difficult to perform regular classification and surface treatment due to such a state, the temperature inside the tank is caused by heat generation caused by a decrease in classification accuracy and a temporary load increase in the dispersion treatment. We believe that an increase will occur. On the other hand, by making the upper part of the guide ring according to the present invention into a louver structure, fine dispersion of the powder is promoted when the powder passes through the louver part, and each part of the first space and the second space in the apparatus is promoted. It is considered that the dust density density of the water becomes uniform, regular classification and surface treatment are possible, and improvement in classification yield and reduction in temperature in the tank are achieved. The range in which the louver portion according to the present invention occupies the upper part of the cylindrical partition member is such that L1 / L0 is 0.1 when the overall height of the cylindrical partition member is L0 and the height of the dispersion louver portion is L1. To 0.5. If it is less than 0.1, a sufficient dispersion effect cannot be obtained, and if it is more than 0.5, powder that cannot reach the classification rotor from the first space may be generated. It is not possible to do this.

In a more preferred aspect, the upper end portion of the guiding means is in close contact with the inner surface of the top plate. In this case, all the powder that reaches the classification rotor will reach the louver, so that fine dispersion and uniform dispersion of the powder inside the apparatus can be achieved more effectively, and the object of the present invention can be achieved more suitably. Become.

  The specification of the guide ring is that the upper louver part and the lower guide ring part can be divided so that the upper part can be configured as a louver. The structure of the upper louver part (the gap width between each louver and the number of louvers) , The louver angle, the height of the louver portion, etc.) are appropriately selected to find the optimum conditions. Usually, the gap width between individual louvers is preferably set at equal intervals, and the gap width between the individual louvers is preferably set in the range of 5 mm to 40 mm, more preferably in the range of 7 mm to 25 mm. . When the gap width between the individual louvers is narrower than 5 mm, it may be difficult for the powder to pass smoothly between the louvers. When the gap width between the individual louvers is larger than 40 mm, a sufficient dispersion effect is obtained. It may be difficult to obtain. The number of louvers is appropriately determined in relation to the gap width between louvers.

Furthermore, in the production method of the present invention, in the particle size distribution of the finely pulverized product, the weight average particle size D4 is 3.5 to 7.5 μm, 4.0 μm or less is 80% by number or less, and the specific gravity is 1.0 g / It can be suitably used optionally classifying surface treatment things cm ³ ~1.5g / cm ^3. The present invention aims at optimizing the dispersibility in the present apparatus, and is because the effect of the present invention tends to become apparent when a toner having higher cohesion is used.

  Incidentally, since the surface of the toner obtained by the production method of the present invention is modified, the obtained modified particles will be described below.

  As an indicator of the degree of surface modification of the surface modified particles, the average circularity can be used as an index in the present invention.

  The average circularity in the present invention is used as a simple method for quantitatively expressing the shape of particles, and in the present invention, measurement is performed using a flow type particle image analyzer FPIA-1000 manufactured by Toa Medical Electronics, The circularity of the measured particles is obtained by the following formula, and the value obtained by dividing the total circularity of all the measured particles by the total number of particles is defined as the average circularity.

  As a measurement method, about 5 mg of toner is dispersed in 10 ml of water in which about 0.1 mg of a nonionic surfactant is dissolved to prepare a dispersion, and ultrasonic waves (20 kHz, 50 W) are irradiated to the dispersion for 5 minutes. The degree of circularity of the toner is measured with the above apparatus at a dispersion concentration of 5000 to 20000 / μl.

  The “average circularity” in the present invention is an index of the degree of unevenness of the surface-modified particles, and indicates 1.000 when the toner is a perfect sphere, and the average circularity becomes smaller as the toner shape becomes more complicated. Become.

  Moreover, the amount of ultrafine powder was investigated as an evaluation standard of the present invention. This is because there is a correlation with image fogging.

  The amount of ultrafine powder is judged by the number% of 3.0 μm or less from the particle size distribution measured by FPIA-1000. 15% or less is necessary to maintain a good fog level in image evaluation.

  According to the toner production method of the present invention, the average circularity of the particles obtained in the surface modification step is 0.01 to 0.00 mm higher than the average circularity of the finely pulverized product introduced into the surface modification step. 05 can be increased. This is because the surface shape of the toner can be arbitrarily controlled by arbitrarily controlling the surface modification time of the surface modifying apparatus as described above. Usually, by using this apparatus, toner having a circularity of 0.935 to 0.980 can be arbitrarily obtained. From the viewpoint of improving transfer efficiency and hollowing out, it is preferable to maintain a circularity of 0.940 or more.

  The particle size distribution of the toner can be measured by various methods. In the present invention, the following measurement apparatus was used.

  That is, a Coulter Counter TA-II type or Coulter Multisizer II (manufactured by Coulter, Inc.) was used as a measuring device. A 100 μm aperture was used as the aperture, and the volume and number distribution of the toner were measured to calculate the volume distribution and the number distribution. Then, the weight-average weight average particle diameter obtained from the volume distribution according to the present invention was obtained.

  Next, the manufacturing process of the present invention will be outlined. In order to produce the toner particles according to the present invention, for example, a binder resin, a wax, a metal salt or a metal complex, a pigment or dye as a colorant, a magnetic material, a charge control agent if necessary, other additives, etc. Are mixed thoroughly by a mixer such as a Henschel mixer and a ball mill, and then melted and kneaded using a heat kneader such as a heating roll, a kneader, and an extruder so that the resins are compatible with each other. After dispersing or dissolving the dye and magnetic substance, cooling and solidifying, coarsely pulverizing the solidified product, finely pulverizing with a pneumatic impact pulverizer such as I-mill or mechanical impact pulverizer such as turbo mill and kryptron, Toner particles having a desired particle diameter can be obtained by using a batch type surface treatment and classifying apparatus that are preferably used in the present invention.

  Next, the constituent material of toner particles containing the binder resin, wax and colorant according to the present invention will be described. In the present invention, conventionally known various toner particle materials can be used without particular limitation.

  As the binder resin constituting the toner particles, any resin usually used for toner can be used, and examples thereof include the following.

  The binder resin used in the present invention includes, for example, a homopolymer of styrene such as polystyrene, poly-p-chlorostyrene and polyvinyltoluene, and a substituted polymer thereof; styrene-p-chlorostyrene copolymer, styrene. -Vinyltoluene copolymer, styrene-vinylnaphthalene copolymer, styrene-acrylic acid ester copolymer, styrene-methacrylic acid ester copolymer, styrene-α-chloromethyl methacrylate copolymer, styrene-acrylonitrile copolymer Polymer, styrene-vinyl methyl ether copolymer, styrene-vinyl ethyl ether copolymer, styrene-vinyl methyl ketone copolymer, styrene-butadiene copolymer, styrene-isoprene copolymer, styrene-acrylonitrile-indene copolymer Styrenic copolymers such as coalesced; Vinyl chloride, phenolic resin, natural modified phenolic resin, natural resin modified maleic acid resin, acrylic resin, methacrylic resin, polyvinyl acetate, silicone resin, polyester resin, polyurethane, polyamide resin, furan resin, epoxy resin, xylene resin, polyvinyl Butyral, terpene resin, coumarone indene resin and petroleum resin can be used. Cross-linked styrene resins are also preferred binder resins.

  Examples of the comonomer for the styrene monomer of the styrene copolymer include acrylic acid, methyl acrylate, ethyl acrylate, butyl acrylate, dodecyl acrylate, octyl acrylate, 2-ethylhexyl acrylate, phenyl acrylate, methacrylic acid. Monocarboxylic acid having a double bond such as acid, methyl methacrylate, ethyl methacrylate, butyl methacrylate, octyl methacrylate, acrylonitrile, methacrylonitrile, acrylamide or a substituted product thereof; for example, maleic acid, butyl maleate, Dicarboxylic acids having a double bond such as methyl maleate and dimethyl maleate and substituted products thereof; for example, vinyl esters such as vinyl chloride, vinyl acetate and vinyl benzoate; Ethylenic olefins such as alkylene; for example, vinyl methyl ketone, vinyl ketones such as vinyl hexyl ketone; for example, vinyl methyl ether, vinyl ethyl ether, vinyl ethers such as vinyl isobutyl ether; and the like. These vinyl monomers are used alone or in combination.

  Here, as the crosslinking agent, compounds having two or more polymerizable double bonds are mainly used. For example, aromatic divinyl compounds such as divinylbenzene and divinylnaphthalene; for example, ethylene glycol diacrylate and ethylene glycol diacrylate. Carboxylates having two double bonds, such as methacrylate and 1,3-butanediol dimethacrylate; divinyl compounds of divinylaniline, divinyl ether, divinyl sulfide and divinyl sulfone; and compounds having three or more vinyl groups; Can be used alone or as a mixture.

  As a factor attributed to the binder resin, as a preferable physical property of the toner, in the molecular weight distribution measured by GPC of THF-soluble matter, the toner has at least one peak in a molecular weight region of 2,000 to 50,000, and the molecular weight More preferably, 1000 to 30,000 components are present in an amount of 50 to 90%.

  In the present invention, the following waxes are used as the material for the toner particles from the viewpoint of improving releasability from the fixing member at the time of fixing and improving fixability. Examples of the wax include paraffin wax and derivatives thereof, microcrystalline wax and derivatives thereof, Fischer-Tropsch wax and derivatives thereof, polyolefin wax and derivatives thereof, carnauba wax and derivatives thereof, and the derivatives include oxides and vinyl monomers. Block copolymers and graft-modified products. In addition, alcohols, fatty acids, acid amides, esters, ketones, hydrogenated castor oil and derivatives thereof, plant waxes, animal waxes, mineral waxes, petrolactams and the like can also be used.

  In the present invention, a charge control agent is preferably blended (internally added) into toner particles or mixed (externally added) with toner particles as a material for toner particles. The charge control agent makes it possible to control the optimum charge amount according to the development system, and in particular, it is possible to produce a toner with a more stable balance between the particle size distribution and the charge amount.

  As the negative charge control agent for controlling the toner to be negatively charged, for example, organometallic complexes and chelate compounds are effective, and monoazo metal complexes, acetylacetone metal complexes, aromatic hydroxycarboxylic acid metal complexes, and aromatic dicarboxylic acids. There are metal complexes. Others include aromatic hydroxycarboxylic acids, aromatic monocarboxylic acids and aromatic polycarboxylic acids and their metal salts, anhydrides, esters, and phenol derivatives such as bisphenols.

  Examples of the positive charge control agent for controlling the toner to be positively charged include modified products of nigrosine and fatty acid metal salts, etc .; tributylbenzylammonium-1-hydroxy-4-naphthosulfonate, tetrabutylammonium tetrafluoroborate Quaternary ammonium salts such as: onium salts such as phosphonium salts thereof, and lake pigments thereof; triphenylmethane dyes and lake pigments thereof (as rake agents include phosphotungstic acid, phosphomolybdic acid, Phosphotungstic molybdic acid, tannic acid, lauric acid, gallic acid, ferricyanide, ferrocyanide, etc.); metal salts of higher fatty acids; diorganotin oxides such as dibutyltin oxide, dioctyltin oxide, dicyclohexyltin oxide; dibuty Suzuboreto, dioctyl tin borate, such as diorganotin tin borate such dicyclohexyl tin borate; is.

  These charge control agents can be used alone or in combination of two or more.

  The above-described charge control agent is preferably used in the form of fine particles. In this case, the number average particle diameter of these charge control agents is particularly preferably 4 μm or less, and more preferably 3 μm or less. When these charge control agents are internally added to the toner particles, they are preferably added to the toner particles in an amount of 0.1 to 20 parts by mass, particularly 0.2 to 10 parts by mass with respect to 100 parts by mass of the binder resin.

  In the present invention, various conventionally known colorants can be used as the toner particle material. The colorant used in the present invention is adjusted to black by a chromatic colorant such as carbon black or a magnetic material, a yellow colorant, a magenta colorant, and a cyan colorant shown below as a black colorant. A combination or the like is used.

  As the yellow colorant, compounds represented by condensed azo compounds, isoindolinone compounds, anthraquinone compounds, azo metal complexes, methine compounds, and allylamide compounds are used. Specifically, C.I. I. Pigment Yellow 12, 13, 14, 15, 17, 62, 74, 83, 93, 94, 95, 97, 109, 110, 111, 120, 127, 128, 129, 147, 168, 174, 176, 180, 181 and 191 are preferably used.

  As the magenta colorant, condensed azo compounds, diketopyrrolopyrrole compounds, anthraquinones, quinacridone compounds, basic dye lake compounds, naphthol compounds, benzimidazolone compounds, thioindigo compounds, and perylene compounds are used. Specifically, C.I. I. Pigment Red 2, 3, 5, 6, 7, 23, 48: 2, 48: 3, 48: 4, 57: 1, 81: 1, 144, 146, 166, 169, 177, 184, 185, 202, 206, 220, 221, 254 are particularly preferred.

  As the cyan colorant, copper phthalocyanine compounds and derivatives thereof, anthraquinone compounds, and basic dye lake compounds can be used. Specifically, C.I. I. Pigment Blue 1, 7, 15, 15: 1, 15: 2, 15: 3, 15: 4, 60, 62, 66 and the like can be used particularly preferably.

  These colorants can be used alone or mixed and further used in the form of a solid solution. In the present invention, the colorant is selected in consideration of hue angle, saturation, brightness, weather resistance, OHP transparency, and dispersibility in the toner. These chromatic colorants are contained in the toner particles in a total amount of 1 to 20 parts by mass with respect to 100 parts by mass of the binder resin.

  Further, in order to improve fluidity, transferability, etc., a toner can be obtained by externally adding a known external additive such as inorganic fine powder to the toner particles and passing through the sieving step presented in the present invention. .

  Hereinafter, the present invention will be specifically described with specific toner production methods, examples, and comparative examples.

<Example 1>
Unsaturated polyester resin 100 parts by mass Copper phthalocyanine pigment 4 parts by mass (CI Pigment Blue 15: 3)
Paraffin wax 6 parts by mass (maximum endothermic peak 73 ° C)
Charge control agent (salicylic acid metal complex E-88 (manufactured by Orient Chemical Co., Ltd.)) 2 parts by mass After thoroughly mixing the materials of the above prescription with a Henschel mixer (FM-75 type, manufactured by Mitsui Miike Chemical Co., Ltd.) It knead | mixed with the biaxial kneader (PCM-30 type | mold, Ikegai Iron Works Co., Ltd.) set to the temperature of 110 degreeC. The obtained kneaded product was cooled and coarsely pulverized to 1 mm or less with a hammer mill to obtain a coarsely pulverized product for toner production.

The obtained toner raw material coarsely pulverized product was pulverized with an I-DS5 type pulverizer (manufactured by Nippon New Match Cook) using jet air to obtain a finely pulverized product. The particle size of the finely pulverized product was such that D4 was 6.8 μm, and the number of 4.0 μm or less was 55%. The finely pulverized product was subjected to surface modification and classification using a surface modification apparatus equipped with a guide ring (L0 = 330 mm, L1 = 65 mm) shown in FIG. 2 (see FIG. 3). The distance between the top plate inner surface and the guide ring upper end was set to 35 mm. 24 louvers were used (see FIG. 4). As operating conditions, the inlet temperature is -20 ° C., the throughput is 75 kg / hr, the classification rotor rotational speed is 6500 rpm (the outer diameter of the classification rotor is 240 mm, the tip peripheral speed is 81 m / sec), the dispersion rotor is 5300 rpm (the outer diameter of the dispersion rotor is 400 mm). The tip peripheral speed was 111 m / sec), the cycle time was 46 sec (input time: 8 sec, treatment time 30 sec, discharge time 8 sec), and the air flow was 21 m ³ / min for 24 minutes. The temperature of the outflow gas at the fine powder outlet (hereinafter referred to as the exhaust temperature) was monitored as an index indicating the temperature inside the apparatus at 24 minutes. The exhaust temperature was 45 ° C., and toner particles having a particle diameter of 7.6 μm and 4.0 μm or less were 11%. The classification yield was 65%. The classification yield was determined from ((total amount of classified product obtained) ÷ (total amount of finely pulverized product charged)) × 100.

  Toner particles were obtained by externally adding 1.2 parts by weight of hydrophobic silica to 100 parts by weight of toner particles. A developer was prepared by adding 95 parts by mass of an acrylic-coated ferrite carrier to 5 parts by mass of the toner. Using this developer, an image was evaluated in a low-temperature / low-humidity environment (15 ° C, 10%) using a Canon full-color copier CLC1000 remodeled machine (with the oil application mechanism of the fixing unit removed). The fogging level (◯: good level, x: bad level, Δ: acceptable level, ○ Δ: intermediate level between ○ and Δ, Δ ×: intermediate level between Δ and ×) was examined for 10,000 sheets durability. The results are shown in Table 1.

<Example 2>
A toner was prepared in the same manner as in Example 1 except that the L1 value of the guide ring was 100 mm, and image output was evaluated. The results are shown in Table 1.

<Example 3>
A toner was prepared in the same manner as in Example 1 except that the L1 value of the guide ring was 100 mm, the L0 value was 365 mm, and a sealed system was used, and image evaluation was performed. The results are shown in Table 1.

<Example 4>
A toner was prepared in the same manner as in Example 1 except that the L1 value of the guide ring was 100 mm, the L0 value was 365 mm (sealed system), and the rotational speed of the dispersion rotor was 5800 rpm, and the image formation evaluation was performed. It was. The results are shown in Table 1.

<Example 5>
A toner was prepared in the same manner as in Example 3 except that the L1 value of the guide ring was 130 mm, and image output was evaluated. The results are shown in Table 1.

<Reference example>
A toner was prepared in the same manner as in Example except that a guide ring having no louver portion was used, and image output was evaluated. The results are shown in Table 1.

<Comparative Example 1>
A toner was prepared in the same manner as in Comparative Example 1 except that the rotational speed of the dispersion rotor was changed to 5800 rpm, and image output evaluation was performed. The results are shown in Table 1.

It is a schematic sectional drawing of the surface modification apparatus used in the surface modification process of this invention. It is an external view of the partition member which comprises the surface modification apparatus used in the surface modification process of this invention. It is a side view of the partition member which comprises the surface modification apparatus used in the surface modification process of this invention. It is an upper section of the partition member which constitutes the surface modification device used in the surface modification process of the present invention.

Explanation of symbols

30: Main body casing 31: Cooling jacket 32: Dispersion rotor 33: Square disk 34: Liner 35: Classification rotor 36: Guide ring 37: Raw material inlet 38: Raw material supply valve 39: Raw material supply port 40: Product discharge port 41: Product discharge valve 42: Product extraction port 43: Top plate 44: Fine powder discharge casing 45: Fine powder discharge port 46: Cold air inlet 47: First space 48: Second space 49: Surface modification zone 50: Classification zone 51 : Sealing material

Claims (4)

A step of melt-kneading a composition containing at least a binder resin, a wax and a colorant, cooling and solidifying the obtained kneaded product, and finely pulverizing the cooled solidified product to obtain a finely pulverized product, and the obtained finely pulverized product In a method for producing a toner, the method includes a step of obtaining toner particles obtained by simultaneously treating the surface modification and classification.
The step of simultaneously performing the surface modification and classification is performed using a cylindrical batch type surface modification apparatus,
The surface reforming apparatus includes a cylindrical main body casing, a charging unit for charging the finely pulverized material into the main body casing, and continuously supplying fine powder having a predetermined particle diameter or less from the finely pulverized material charged into the main body casing to the outside of the device. Classification means for automatically discharging and removing, a fine powder discharge portion for discharging fine powder removed by the classification means to the outside of the main body casing, and for treating the treated particles from which the fine powder has been removed using a mechanical impact force The surface modification means that rotates in the same direction as the rotation direction of the classification means, and the space between the classification means and the surface treatment means, the first space before being introduced into the classification means, and fine powder by the classification means Guide means for partitioning the classified particles into a second space for introducing the particles into the surface treatment means, fine powder having a predetermined particle size or less is removed by the classification means, and surface modification treatment is performed by the surface modification means. Where Has a discharge portion for discharging outside the main casing of physical particles as the surface modified particles,
The guide means has at least a cylindrical partition member, and the upper portion of the cylindrical partition member is composed of a plurality of louvers whose tips are directed in a tangential direction of the inner circumferential circle of the cylindrical partition member, When the overall height of the partition member is L0 and the height of the dispersion louver portion is L1, L1 / L0 is 0.1 to 0.5, and the finely pulverized product is introduced into the first space. The finely pulverized product is swirled by a swirling flow and is sent to the classification unit through the louvers provided at the upper part of the guide unit. The classification unit removes fine powder having a predetermined particle size or less to the outside of the apparatus. While continuously discharging and removing, it is introduced into the surface treatment means using mechanical impact force through the second space, surface modification treatment is performed, and the mixture is circulated again to the first space, so that it is constant. Repeated surface modification using time classification and mechanical impact force It allows fines under predetermined particle diameter or less have been removed, producing a toner, characterized in that to obtain a surface modification treatment particles.   2. The toner manufacturing method according to claim 1, wherein the surface modifying apparatus has a top plate that can be opened and closed at an upper portion of the main body casing, and an upper end portion of the guide means is in close contact with the inner surface of the top plate. . A batch-type surface modification device used for toner production, in which particle classification and spheroidization are performed simultaneously,
Cylindrical main body casing, input portion for supplying the finely pulverized material into the main body casing, and classifying means for continuously discharging and removing fine powder having a predetermined particle diameter or less from the finely pulverized material input into the main body casing to the outside of the apparatus. A fine powder discharger for discharging the fine powder removed by the classification means to the outside of the main body casing; and a rotation direction of the classification means for surface-treating the treated particles from which the fine powder has been removed using a mechanical impact force. Surface modification means rotating in the direction, first and second spaces provided between the classification means and the surface treatment means, the first space for introducing the particles to be treated into the classification means And a second space for introducing the particles to be treated into the surface modifying means, a guide means for partitioning the first space and the second space, and fine powder having a predetermined particle size or less by the classifying means. Removed and Has a discharge portion for discharging outside the main casing to be treated particles surface modification treatment by serial surface modification means is performed as a surface-modified particles,
The guide means has at least a cylindrical partition member, and the upper portion of the cylindrical partition member is composed of a plurality of louvers whose front ends are directed in the tangential direction of the inner circumferential circle of the cylindrical partition member, A surface reforming apparatus, wherein L1 / L0 is 0.1 to 0.5, where L0 is a total length of the cylindrical partition member and L1 is a height of the dispersion louver portion.   4. The surface modification apparatus according to claim 3, wherein the surface modification apparatus has a top plate that can be opened and closed at an upper portion of the main body casing, and an upper end portion of the guide means is in close contact with an inner surface of the top plate.

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