JP3010331B2 - Method for producing polymerized toner for developing electrostatic images - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for efficiently producing a polymerized toner by a suspension polymerization method.

[0002]

2. Description of the Prior Art Electrophotography is disclosed in U.S. Pat. No. 2,297,6.
As described in, for example, US Pat. No. 91/91, a number of methods are known. Generally, a photoconductive substance is used to form an electric latent image on a photoreceptor by various means, and then the latent image is formed. The image is developed using toner, and if necessary, the toner image is transferred to a transfer member such as paper, and then fixed by heating, pressure, or solvent vapor to obtain a copy. Further, as a method of developing using a toner or a method of fixing a toner image,
Conventionally, various methods have been proposed, and a method suitable for each image forming process has been adopted.

Conventionally, toners used for these purposes are generally prepared by melt-mixing a coloring agent composed of a dye and a pigment in a thermoplastic resin, uniformly dispersing the same, and then using a pulverizer or a classifier to obtain a toner having a desired particle size. Has been manufactured.

[0004] Although this method can produce fairly good toners, it does have certain limitations, namely the choice of toner materials. For example, the resin colorant dispersion is brittle enough,
It must be able to be comminuted in an economically feasible production equipment. However, when the resin colorant dispersion is made brittle to satisfy these requirements, the particle size range of the particles formed when actually pulverized at a high speed tends to be widened, and in particular, a relatively large proportion of the fine particles The problem of inclusion occurs. Further, such a highly brittle material is liable to be further pulverized or powdered when used for development in a copying machine or the like. Further, in this method, it is difficult to completely and uniformly disperse solid fine particles such as a colorant in a resin, and depending on the degree of the dispersion, an increase in fog, a decrease in image density, and color mixing / transparency are difficult. Attention must be paid to dispersion, as it will cause defects. Further, exposure of the coloring agent to the fracture surface may cause fluctuations in development characteristics.

On the other hand, in order to overcome the problems of the toner caused by these pulverization methods, Japanese Patent Publication Nos.
Nos. 10799 and 51-14895 propose a method for producing a toner by a suspension polymerization method. In the suspension polymerization method, a polymerizable monomer, a colorant, a polymerization initiator, and, if necessary, a crosslinking agent, a charge control agent, and other additives are uniformly dissolved or dispersed to form a monomer composition. A continuous phase containing the monomer composition containing a dispersion stabilizer,
For example, the toner particles are dispersed in an aqueous phase using a suitable stirrer, and simultaneously undergo a polymerization reaction to obtain toner particles having a desired particle size.

[0006] Since this method does not include any pulverizing step, the toner does not need to be brittle and a soft material can be used. In addition, the colorant is not exposed to the particle surface, and uniform friction can be obtained. There is an advantage of having a charging property.

However, in obtaining the above-mentioned polymerizable monomer composition by a conventional suspension polymerization method, it takes a long time to disperse a toner property imparting agent such as a coloring agent and a charge controlling agent, Insufficient dispersion of a toner property imparting agent such as a charge control agent tends to cause a decrease in image density or a decrease in granulation of a monomer composition in a continuous phase containing a dispersion stabilizer. There is a point.

[0008]

SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing a toner for developing an electrostatic image by a suspension polymerization method, in which a dispersion of a colorant and the like is more uniform and the image density is good. It is in.

Another object of the present invention is to provide a method for producing a toner having a uniform and sharp particle size distribution in producing a toner by a suspension polymerization method.

Another object of the present invention is to provide a method for producing a toner in which a dispersion prepared in a dispersion step can be easily stored in the production of a toner by a suspension polymerization method.

[0011]

The object of the present invention is attained by the following constitutions.

That is, the present invention provides a dispersion step of dispersing a colorant in a monomer system containing at least a polymerizable monomer, and dispersing the monomer system in an aqueous medium to form suspended particles. And a method for producing a polymerized toner for developing an electrostatic image, comprising the step of polymerizing the obtained suspended particles, wherein in the dispersion step, a media, a rotating rotor and a stator are used. The rotor is rotated so that the peripheral speed at the foremost end in the rotation direction of the above ranges from 3 m / s to 20 m / s, and the initial viscosity of the monomer system is 1 mPa · s (1 cP) to 100 mPa.
S (100 cP), and a method for producing a polymerized toner for electrostatic image development, characterized in that the viscosity of the prepared liquid after dispersion is controlled in the range of 10 to 1000 times the initial viscosity.

Further, the present invention provides a dispersing step of dispersing a colorant in a wax system containing at least a polyalkylene wax, and dissolving and mixing the wax system with a monomer system containing at least a polymerizable monomer. A step of dispersing the dissolved mixed solution in an aqueous medium, granulating suspended particles, and a method of producing a polymerized toner for electrostatic image development, comprising a step of polymerizing the obtained suspended particles. In the dispersing step, using a media type dispersing machine having a media, a rotating rotor and a stator, the rotor is rotated so that the peripheral speed of the foremost part in the rotating direction of the rotor is in the range of 3 m / s to 20 m / s. Then, the initial viscosity of the wax system is set to 1 mPa · s (1 cP) to 100 mPa · s.
(100 cP), and a method for producing a polymerized toner for electrostatic charge image development, characterized in that the viscosity of the prepared liquid after dispersion is controlled within a range of 10 to 1000 times the initial viscosity.

Hereinafter, the present invention will be described in detail.

The present inventors have conducted intensive studies and found that when a colorant is dispersed in a monomer system using a media type disperser, the colorant can be uniformly dispersed in the monomer system in a short time. I found Further, when the colorant is dispersed in a wax system containing at least a polyalkylene wax, the colorant can be uniformly dispersed in the wax system in a short time, and they are cooled, solidified and stored. be able to.

As the media type disperser used in the dispersing step, dispersers as shown in FIGS. 1 to 4 are used. Hereinafter, the configuration of FIGS. 1 to 4 will be described. A media-type dispersing machine 1 as shown in FIG. 1 includes a rotating rotor 3 and a stator 4 and a separation valve 6 for separating the dispersion liquid from the medium 5, and a raw material input port 1 is provided above the stator 4. The outlet 2 is provided below the disperser via a separation valve 6. Such a media-type dispersing machine 1 supplies a raw material slurry from a raw material inlet 1 on an upper portion of a stator, and disperses the raw material slurry by a rotating rotor 3, a stator 4 and a medium 5. At this time, the pressure inside the disperser is set by adjusting the separation valve 6, and the disperser is operated at a constant pressure. The dispersion liquid is discharged from the discharge port 2 at the lower part of the disperser through the separation valve 6.

Media type dispersing machine 2 as shown in FIG.
Are rotating rotor 3, stator 4 and media 5
(Or screen) to separate the liquid and the dispersion
6, a raw material inlet 1 is provided at the upper part of the side of the disperser, and the outlet 2 is provided at the upper part of the side of the disperser opposite to the side at which the raw material inlet 1 is provided via a gap (or screen) 6. Is provided. Such a media-type dispersing machine 2 supplies a raw material slurry from a raw material inlet 1 on an upper side of the dispersing machine, and disperses the raw material slurry by a rotating rotor 3, a stator 4 and a media 5. The dispersion liquid is discharged through the gap (or screen) 6 from the discharge port 2 at the upper part of the side of the disperser opposite to the side where the raw material input port 1 is provided.

Media type dispersing machine 3 as shown in FIG.
Are rotating rotor 3, stator 4 and media 5
(Or screen) to separate the liquid and the dispersion
The material inlet 1 is provided at the lower part of the stator 4 and the outlet is provided at the upper part of the stator 4 via a slit (or screen) 6. Such a media-type dispersing machine 3 supplies a raw material slurry from a raw material inlet 1 at a lower portion of a side surface of a stator, and disperses the raw material slurry by a rotating rotor 3, a stator 4 and a media 5. The dispersion liquid is discharged from a discharge port 2 provided at an upper portion of the stator through a slit (or a screen) 6.

A media type dispersing machine 4 as shown in FIG.
Is composed of a stator 4 having a cross section of an inverted triangle like the rotor 3 having a cross section of an inverted triangle, and gaps 6 and 7 for separating the dispersion liquid from the medium 5. Provided with stator 4
The discharge port 2 is provided in the upper part via a gap. Such a media-type dispersing machine 4 supplies a raw material slurry from a raw material input port 1 at a lower portion of a stator 4, and the raw material slurry is introduced into the dispersing machine through a gap 7, and the rotating cross section is the same as the rotor 3 having an inverted triangular shape. The raw material slurry is dispersed by the stator 4 and the mediar 5 each having an inverted triangular cross section. The dispersion liquid is discharged from the discharge port 2 provided on the upper part of the stator through the gap 6.

As described above, the initial viscosity of the monomer system was adjusted to 1 mPa · s using a media type disperser as shown in FIGS.
(1 cP) to 100 mPa · s (100 cP), and controlling the viscosity of the prepared liquid after dispersion within a range of 10 times or more and 1000 times or less of the initial viscosity can reduce aggregation of a colorant or the like. It is preferable in that the fluid shear stress, the compression of the media, and the shear stress of the grinding work more efficiently.

In the dispersing machine as shown in FIGS. 1 to 4, it is preferable to use a media having a diameter of 0.1 mm to 5 mm from the viewpoint of dispersibility of the colorant and the like.
Furthermore, it is more preferable to use in the range of 0.3 mm to 2 mm.

In the present invention, the media-type dispersing machine has a peripheral speed of 3 m / m at the tip of the rotor, that is, the tip in the rotating direction, in terms of dispersibility of the colorant and the like and wear of the media and the stator. s to 20 m / s by rotating the rotor in the range of 5 to 20 m / s.
It is preferable to use the rotor by rotating the rotor in the range of m / s to 15 m / s.

In the dispersing machine as shown in FIGS. 1 to 4, in order to control the dispersion temperature, the structure of the stator portion is made hollow so that a heat medium or a refrigerant can pass therethrough so that the temperature can be controlled. It is more preferable that the rotor portion has a hollow structure so that the heat medium or the refrigerant can pass therethrough so that the temperature can be controlled.

In the dispersing machine as shown in FIGS. 1 to 4, it is preferable to use a wear-resistant material such as zirconia as a material for the stator portion and the rotor portion from the viewpoint of wear resistance.

In the media type dispersing machine as shown in FIGS. 1 to 4, the raw material is supplied from the upper portion of the stator as shown in FIG. 1, dispersed while pressurizing the inside of the mill, and discharged from the lower portion of the stator. The use of a media type disperser which is capable of dispersing the colorant is preferable because the dispersing efficiency of the colorant is good and a short path can be prevented.

As the media material used in the media type disperser, for example, glass, steel, chromium alloy,
Alumina, zirconia, zircon, titania and the like can be mentioned.

Among the above media materials, zirconia and titania are more preferable from the viewpoint of abrasion resistance.

The polymerizable monomer constituting the polymerizable monomer system and the toner property imparting agent such as a colorant used in the present invention include the following.

Examples of the polymerizable monomer include styrene monomers such as styrene, o-methylstyrene, m-methylstyrene, p-methylstyrene, p-methoxystyrene, and p-ethylstyrene; methyl acrylate; Ethyl acrylate, n-butyl acrylate, isobutyl acrylate, n-propyl acrylate, n-octyl acrylate, dodecyl acrylate, 2-ethylhexyl acrylate, stearyl acrylate, 2-chloroethyl acrylate, phenyl acrylate and the like Acrylic esters, methyl methacrylate, ethyl methacrylate, n-propyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, n-octyl methacrylate, dodecyl methacrylate, 2-ethylhexyl methacrylate, stearyl methacrylate, methacryl Phenyl, dimethylaminoethyl methacrylate, methacrylic acid esters other acrylonitrile such as ethyl methacrylate aminoethyl, methacrylonitrile, and the like monomers acrylamide.

These monomers can be used alone or as a mixture. Among the above-mentioned monomers, it is preferable to use styrene or a styrene derivative alone or in a mixture with another monomer, from the viewpoint of the developing characteristics and durability of the toner.

In the present invention, polymerization may be carried out by adding a resin having a polar group to the monomer system. The polar resins that can be used in the present invention are exemplified below. (1) Examples of the cationic polymer include a polymer of a nitrogen-containing monomer such as dimethylaminoethyl methacrylate and diethylaminoethyl methacrylate, and a copolymer with styrene, an unsaturated carboxylic acid ester, and the like. (2) Examples of the anionic polymer include nitrile monomers such as acrylonitrile, halogen-containing monomers such as vinyl chloride, unsaturated carboxylic acids such as acrylic acid and methacrylic acid,
Other examples include unsaturated dibasic acids / unsaturated dibasic acid anhydrides, polymers such as nitro monomers, and copolymers with styrene monomers. These polar resins are localized near the surface of the toner, thereby improving the blocking resistance of the toner.

As the coloring agent used in the present invention, known coloring agents can be used. For example, carbon black, iron black, C.I. I. Direct Red 1, C.I. I. Direct Red 4, C.I. I. Acid Red 1, C.I. I. Basic Red 1, C.I. I. Modant Red 30, C.I.
I. Direct Blue 1, C.I. I. Direct Blue 2, C.I. I. Acid Blue 9, C.I. I. Acid Blue 15, C.I. I. Basic Blue 3, C.I. I. Basic Blue 5, C.I. I. Modant Blue 7, C.I. I.
Direct Green 6, C.I. I. Basic Green 4, C.I. I. Dyes such as Basic Green 6, graphite, cadmium yellow, mineral fast yellow, navel yellow, naphthol yellow S, Hanza yellow G, permanent yellow NCG, tartrazine lake, molybdenum orange, permanent orange GT
R, benzidine orange G, cadmium red, permanent red 4R, watching red calcium salt,
Brilliant Carmine 3B, Fast Violet B,
Pigments such as methyl violet lake, navy blue, cobalt blue, alkali blue lake, Victoria blue lake, quinacridone, rhodamine lake, phthalocyanine blue, fast sky blue, pigment green B, malachite green lake, final yellow green G and the like. In the present invention, in order to obtain a toner using a polymerization method, it is necessary to pay attention to the polymerization inhibitory and aqueous phase migration properties of the colorant, preferably, surface modification, for example,
It is better to perform a hydrophobic treatment with a substance that does not inhibit polymerization. In particular, attention must be paid to the use of dyes and carbon black since many of them have polymerization inhibitory properties. As a preferable method for surface-treating the dye system, there is a method in which a polymerizable monomer is polymerized in the presence of these dyes in advance, and the obtained colored polymer is added to the monomer system. In addition, regarding carbon black, in addition to the same treatment as the above-described dye, a graft treatment with a substance that reacts with the surface functional group of carbon black, for example, polyorganosiloxane or the like may be performed.

In the present invention, a magnetic substance may be added.
This is also preferably used after performing a surface treatment.

In the present invention, a polyalkylene-based wax may be added as an essential constituent component. In addition, a releasing agent described below is used in combination for the purpose of improving the offset property in hot roll fixing. It is also possible. For example, paraffin / polyolefin-based waxes and modified products thereof, for example, oxides and graft-treated products, higher fatty acids, metal salts thereof, amide waxes and the like can be mentioned. These waxes are used in the ring and ball method (JIS K
2531) has a softening point of 40 to 130 ° C, preferably 50 to 120 ° C.
When the temperature is lower than 130 ° C., the blocking resistance and shape retention of the toner are insufficient, and when the temperature is higher than 130 ° C., the effect of the releasability is insufficient. Generally, it is preferable to use 1.0 to 100 parts by weight of the release agent per 100 parts by weight of the polymerizable monomer.

In the present invention, it is desirable to add a charge control agent to the toner material in order to control the chargeability of the toner. As these charge control agents, those having little polymerization inhibition and water phase transfer among known ones are used. For example, as positive charge control agents, nigrosine dyes, triphenylmethane dyes, quaternary ammonium salts, amines And polyamine compounds. Examples of the negative charge control agent include metal-containing salicylic acid compounds, metal-containing monoazo dye compounds, styrene-acrylic acid copolymers, and styrene-methacrylic acid copolymers.

As the polymerization initiator, any suitable polymerization initiator, for example, 2,2′-azobis- (2,4-dimethylvaleronitrile), 2,2′-azobisisobutyronitrile, 1'-azobis (cyclohexane-1-
Azo or diazo polymerization initiators such as carbonitrile), 2,2′-azobis-4-methoxy-2,4-dimethylvaleronitrile, azobisisobutyronitrile, benzoyl peroxide, methyl ethyl ketone peroxide,
Peroxide-based polymerization initiators such as diisopropyl peroxycarbonate, cumene hydroperoxide, 2,4-dichlorobenzoyl peroxide, and lauroyl peroxide are exemplified. These polymerization initiators are preferably added in an amount of 0.5 to 20% by weight of the polymerizable monomer.

In the present invention, a crosslinking agent may be added, and a preferable addition amount is 0.001 to 15% by weight.

The additives used in the present invention for imparting various properties are selected from the viewpoint of durability when added to the toner.
The particle diameter is preferably 1/10 or less of the weight average diameter of the toner particles. The particle size of the additive means an average particle size obtained by observing the surface of the toner particles with an electron microscope. As additives for the purpose of imparting these properties, for example, the following are used.

1) Fluidity imparting agents: metal oxides (such as silicon oxide, aluminum oxide, and titanium oxide), carbon black, and carbon fluoride. Those subjected to a hydrophobic treatment are more preferable.

2) Abrasives: metal oxides (strontium titanate, cerium oxide, aluminum oxide, magnesium oxide, chromium oxide, etc.), nitrides (silicon nitride, etc.), carbides (silicon carbide, etc.), metal salts (calcium sulfate, etc.) , Barium sulfate, calcium carbonate, etc.).

3) Lubricants: fluororesin powder (vinylidene fluoride, polytetrafluoroethylene, etc.), fatty acid metal salt (zinc stearate, calcium stearate, etc.).

4) Charge controllable particles: metal oxides (such as tin oxide, titanium oxide, zinc oxide, silicon oxide, and aluminum oxide) and carbon black.

These additives are used in an amount of 0.1 to 10 parts by weight based on 100 parts by weight of the toner particles.
0.1 to 5 parts by weight are used. These additives may be used alone or in combination of two or more.

The aqueous medium used in the present invention includes:
Eventually a suitable stabilizer is added. For example, as an inorganic compound, calcium phosphate, magnesium phosphate, aluminum phosphate, zinc phosphate, calcium carbonate, magnesium carbonate, calcium hydroxide, magnesium hydroxide,
Examples include aluminum hydroxide, calcium metasilicate, calcium sulfate, barium sulfate, bentonite, silica, and alumina. As an organic compound, polyvinyl alcohol, gelatin, methylcellulose, methylhydroxypropylcellulose, ethylcellulose, sodium salt of carboxymethylcellulose, polyacrylic acid and salts thereof, starch and the like can be used by dispersing them in an aqueous phase. This stabilizer is used in an amount of 0.2 parts based on 100 parts of the polymerizable monomer.
It is preferred to use ２０20 parts by weight.

In order to finely disperse these stabilizers, 0.001 to 0.1 parts by weight of a surfactant may be used. This is to promote the intended action of the dispersion stabilizer, and specific examples thereof include sodium dodecylbenzene sulfate, sodium tetradecyl sulfate, sodium pentadecyl sulfate, sodium octyl sulfate,
Examples include sodium oleate, sodium laurate, potassium stearate, calcium oleate and the like.

When an inorganic compound is used among these dispersion stabilizers, a commercially available one may be used as it is, but in order to obtain finer particles, the inorganic compound may be formed in an aqueous medium.

For example, in the case of calcium phosphate, an aqueous solution of sodium phosphate and an aqueous solution of calcium chloride may be mixed under high stirring.

The polymerized toner used in the present invention is obtained by the following method. That is, a releasing agent, a coloring agent, a charge control agent and other additives are added to the polymerizable monomer, and the initial viscosity is set to 1 mPa · s by the above-mentioned media type dispersing machine.
(1 cP) to 100 mPa · s (100 cP).
The polymer was uniformly dissolved or dispersed while controlling so as to be within the range of 2 times or less, a polymerization initiator was added to the dispersion, and the monomer system uniformly dissolved or dispersed by a stirrer, a homogenizer, an ultrasonic disperser or the like was used. Prepare.

When a polyalkylene wax is used, a coloring agent, a release agent, a charge control agent, and other additives are added to the wax while controlling the viscosity to a predetermined value using the media type disperser described above. The polymer is uniformly dissolved or dispersed, and a polymerizable monomer and a polymerization initiator are added to the dispersion to prepare a monomer system which is uniformly dissolved or dispersed by a stirrer, a homogenizer, an ultrasonic disperser or the like.

These monomer systems are dispersed in an aqueous medium containing a dispersion stabilizer using a conventional stirrer or a homomixer / homogenizer. Preferably, the granulation is performed by adjusting the stirring speed and time so that the monomer droplets have a desired toner particle size, generally a particle size of 30 μm or less. After that, by the action of the dispersion stabilizer, stirring may be performed to such an extent that the particle state is maintained and the particles are prevented from settling or floating. After completion of the reaction, while adding an aqueous medium to the suspension, the aqueous medium is distilled off to remove the dispersion stabilizer, and the generated toner particles are collected by washing and filtration, and dried. In the suspension polymerization method, usually, 30 parts of water is added to 100 parts by weight of the monomer system.
It is preferable to use 0 to 3000 parts by weight as a dispersion medium.

In the above step, the polymerization is carried out at a polymerization temperature of 40 ° C. or higher, generally 50 to 90 ° C. Further, the temperature may be raised in the latter half of the polymerization reaction.

The particle size distribution measurement in the present invention will be described.

As a measuring device, Coulter Counter T
A-II type (manufactured by Coulter), number average distribution,
Interface to output volume average distribution (made by Nikkaki)
And CX-1 personal computer (manufactured by Canon)
And the electrolyte is 1% Na using primary grade sodium chloride.
Prepare a Cl aqueous solution.

The measuring method is as follows.
In 50 ml, 0.1 to 5 ml of a surfactant, preferably an alkylbenzene sulfonate, is added as a dispersant, and 0.5 to 50 mg of a measurement sample is further added.

The electrolytic solution in which the sample was suspended was subjected to a dispersion treatment for about 1 to 3 minutes using an ultrasonic disperser, and the particle size distribution of particles of 2 to 40 μm was measured using the Coulter Counter TA-II using an aperture of 100 μm. Is measured to obtain a volume average distribution and a number average distribution. A weight average particle diameter is obtained from the obtained volume average distribution and number average distribution.

The endothermic peak top temperature in the present invention is D
Heating rate 1 using SC-7 (manufactured by PerkinElmer)
The measurement was performed at 0 ° C./min, and was determined from the peak showing the maximum endotherm in the DSC curve at the time of the first temperature rise.

The viscosity measurement in the present invention will be described.

As a measuring device, a rotary viscometer VS-1 was used.
Using a mold (manufactured by Shibaura System Co., Ltd.), the viscosity was measured by rotating the rotor for 1 minute for the sample adjusted to a predetermined temperature by a constant temperature water bath.

[0059]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be specifically described below based on embodiments.

Example 1 451 g of a 0.1 M Na ₃ PO ₄ aqueous solution was added to 709 g of ion-exchanged water, heated to 60 ° C., and then heated to 12,000 rpm using a TK homomixer (manufactured by Tokushu Kika Kogyo). And stirred. A 1.0 M CaCl ₂ aqueous solution was added to the mixture.
7 g was gradually added to obtain an aqueous medium containing Ca ₃ (PO ₄ ) ₂ .

Styrene 1700 g 2-ethylhexyl acrylate 300 g C.I. I. Pigment Blue 15: 3 100 g Paraffin wax (mp 70 ° C.) 600 g Di-tert-butylsalicylate metal compound 50 g The above polymerizable monomer mixture (initial viscosity at 60 ° C. 3
2cP) was heated to 60 ° C. and provided with a zirconia rotor and a stator having a hollow structure, and had a diameter of 1.0 m.
The zirconia beads of 0.8 m were filled into a media-type disperser having a mill volume of 1 liter as shown in FIG. 1 at a supply rate of 12 kg / h by a pump, and the rotor was rotated at 2500 rpm (rotor rotation). 7.9 m / s of peripheral speed at the forefront in the direction, and mill internal pressure 1 kg /
cm ^2, the mill in a temperature 60 ° C., 30 minutes, and dispersed in a circular fashion, to prepare a dispersion liquid in the at 60 ° C.] viscosity 460mPa · s (460cP).

A polymerization initiator, 2,
2'-azobis (2,4-dimethylvaleronitrile) 1
0 g and 1 g of dimethyl 2,2′-azobisisobutyrate were uniformly dissolved at 60 ° C. to prepare a polymerizable monomer system.

The above-mentioned polymerizable monomer system is charged into the above-mentioned aqueous medium, and the mixture is stirred at 60 ° C. under a N ₂ atmosphere at 10,000 rpm for 20 minutes using a TK homomixer to granulate the polymerizable monomer system. did. Thereafter, the mixture was reacted at 60 ° C. for 3 hours while stirring with a paddle stirring blade.
The reaction was performed for 0 hours.

After cooling, hydrochloric acid was added, and Ca ₃ (P
O ₄ ) ₂ was dissolved, filtered, washed with water and dried to obtain a polymerized toner. The particle diameter of the obtained toner is 8.5 μm in weight average diameter.
m and had a sharp particle size distribution. The endothermic peak top temperature measured by DSC was 70 ° C.

With respect to 100 parts by weight of the obtained toner, B
0.7 parts by weight of a hydrophobic silica having a specific surface area of 200 m ² / g by the ET method was externally added. 93 parts by weight of an acryl-coated ferrite carrier was mixed with 7 parts by weight of this toner to prepare a developer.

Using this developer and an externally added toner, an image was formed with a Canon full color copying machine CLC-500. Table 1 shows the results.

Regarding the dispersibility of the dispersion, one or two drops of the dispersion were applied on a slide glass and colored at 200 times magnification using an optical microscope BH2-UMA (Olympus Optical). It was examined by observing the state of the dispersed particles of the agent. Table 1 shows the results. Furthermore,
Regarding the granulation property in the granulation step, one or two drops of the granulation liquid were dropped on a slide glass, and a cover glass was placed on the slide liquid, and the magnification was measured using an optical microscope BH2-UMA (manufactured by Olympus Optical Co., Ltd.). It was investigated by observing the size and distribution of the granulated particles at 200x. Table 1 shows the results. In addition, after the dispersion step was completed, the dispersion was recovered from the disperser, but the recoverability of the dispersion was also good.
A visual inspection was performed on the media after dispersion was completed.
No abnormalities were found in the media.

Example 2 451 g of a 0.1 M Na ₃ PO ₄ aqueous solution was added to 709 g of ion-exchanged water, heated to 60 ° C., and then heated to 12,000 rpm using a TK homomixer (manufactured by Tokushu Kika Kogyo Co., Ltd.). And stirred. A 1.0 M CaCl ₂ aqueous solution was added to the mixture.
7 g was gradually added to obtain an aqueous medium containing Ca ₃ (PO ₄ ) ₂ .

Styrene 1700 g 2-ethylhexyl acrylate 300 g C.I. I. Pigment Blue 15: 3 100 g Di-tert-butylsalicylic acid metal compound 50 g The above polymerizable monomer mixture (initial viscosity at 30 ° C. 1
8 mPa · s [cP]) at 30 ° C. equipped with a rotor made of zirconia and a stator having a hollow structure, and filled with 0.9 liter of zirconia beads having a diameter of 1.0 mm. Is supplied at a supply rate of 7.2 kg / h by a pump to a media-type dispersing machine as shown in (1), the rotor rotational speed is 2200 rpm (the peripheral speed at the foremost portion in the rotational direction of the rotor is 6.9 m / s), and the internal pressure of the mill is increased. 1.0 kg / cm ² , dispersed in one pass at a temperature of 30 ° C. in the mill, and a viscosity of 880 mPa · s (880 cP) [30 ° C.
In this example, a dispersion was prepared.

To 215 g of the above dispersion, 60 g of paraffin wax (mp 70 ° C.) and a polymerization initiator, 2,2′-
Azobis (2,4-dimethylvaleronitrile) 10 g,
And 1 g of dimethyl 2,2′-azobisisobutyrate were uniformly dissolved at 60 ° C. to prepare a polymerizable monomer system.

The above-mentioned polymerizable monomer system was charged into the above-mentioned aqueous medium, and the mixture was stirred at 10,000 rpm for 20 minutes with a TK homomixer at 60 ° C. in an N ₂ atmosphere to granulate the polymerizable monomer system. did. Thereafter, the mixture was reacted at 60 ° C. for 3 hours while stirring with a paddle stirring blade, and then the liquid temperature was set to 80 ° C.
The reaction was performed for 10 hours. Thereafter, the mixture was cooled and hydrochloric acid was added.
a ₃ (PO ₄ ) ₂ was dissolved, filtered, washed with water and dried to obtain a polymerized toner. The obtained toner had a weight average particle size of 8.4 μm and a sharp particle size distribution. Also,
The endothermic peak top temperature measured by DSC was 70 ° C.

With respect to 100 parts by weight of the obtained toner, B
0.7 parts by weight of a hydrophobic silica having a specific surface area of 200 m ² / g by the ET method was externally added. 93 parts by weight of an acryl-coated ferrite carrier was mixed with 7 parts by weight of this toner to prepare a developer.

Using this developer and externally added toner, an image was formed with a Canon full color copying machine CLC-500. Table 1 shows the results.

Regarding the dispersibility of the dispersion, one or two drops of the dispersion were applied on a slide glass, and the colorant was examined at 200 times magnification using an optical microscope BH2-UMA (manufactured by Olympus Optical Co., Ltd.). Was examined by observing the state of dispersed particles. Table 1 shows the results. Furthermore,
Regarding the granulation property in the granulation step, one or two drops of the granulation liquid were dropped on a slide glass, and a cover glass was placed on the slide liquid, and the magnification was measured using an optical microscope BH2-UMA (manufactured by Olympus Optical Co., Ltd.). It was investigated by observing the size and distribution of the granulated particles at 200x. Table 1 shows the results. After the dispersion step, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good, and the media after the dispersion was visually inspected. I couldn't.

Example 3 A polymerized toner was obtained in the same manner as in Example 1, except that the diameter of the media used was 2 mm and the viscosity of the dispersion was 420 mPa · s (420 cP).

The obtained toner had a weight average diameter of 8.7 μm and a sharp particle size distribution.

In the same manner as in Example 1, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 1 shows the results.

After the completion of the dispersion step, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good, and the media after the completion of the dispersion was visually inspected. No abnormalities were observed.

Example 4 In Example 1, the diameter of the media used was 0.3 m.
m, and the dispersion viscosity is 480 mPa · s (480 cP).
A polymerized toner was obtained in the same manner as described above.

The obtained toner had a weight average diameter of 8.3 μm and a sharp particle size distribution.

In the same manner as in Example 1, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 1 shows the results.

After the dispersion step was completed, the dispersion was recovered from the disperser. The recoverability of the dispersion was good, and the media was visually inspected after the completion of the dispersion. No abnormalities were observed.

Example 5 In Example 1, the rotor speed of the media-type dispersing machine was 1600 rpm (the peripheral speed at the foremost part in the rotation direction of the rotor was 5 m / s), and the viscosity of the dispersion was 415 mPa · s.
A polymerized toner was obtained by performing the same operation except that s (415 cp) was used.

The obtained toner had a weight average diameter of 8.7 μm and a sharp particle size distribution.

In the same manner as in Example 1, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 1 shows the results.

After the dispersion step was completed, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good, and the media after the dispersion was visually inspected. No abnormalities were observed.

Example 6 In Example 1, the rotational speed of the rotor of the media type disperser was set to 4750 rpm (the peripheral speed at the foremost part in the rotational direction of the rotor was 15 m / s), and the viscosity of the dispersion liquid was 520 mPa.s.
A polymerized toner was obtained by performing the same operation except that s (520 cP) was used.

The obtained toner had a weight average diameter of 8.6 μm and a sharp particle size distribution.

In the same manner as in Example 1, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 1 shows the results.

After the dispersion step was completed, the dispersion was recovered from the disperser. The recoverability of the dispersion was good, and the media after the dispersion was visually inspected. No abnormalities were observed.

Comparative Example 1 An aqueous medium was obtained in the same manner as in Example 1.

A polymerizable monomer mixture having the same composition as in Example 1 (initial viscosity at 60 ° C. 32 mPa · s [32c
P]) was heated to 60 ° C and pumped into a medialess disperser Ebara Milder (manufactured by Ebara Corporation) using a pump.
The rotor is supplied at a supply rate of 80 kg / h and the rotor speed is 5000
rpm (peripheral speed 1 at the tip of the rotor in the rotation direction)
5 m / s) for 60 minutes in a circulation system to prepare a dispersion (viscosity 350 mPa · s [350 cP]). Thereafter, the operation was performed in the same manner as in Example 1 to obtain a polymerized toner.

The weight average particle diameter of the obtained toner is 10.1 μm.
And had a rather broad particle size distribution. In the same manner as in Example 1, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 1 shows the results.

Comparative Example 2 In Example 1, the rotational speed of the rotor of the media type dispersing machine was 7640 rpm (the peripheral speed at the foremost part in the rotational direction of the rotor 24 m / s) and the diameter of the media was 2.0 mm.
Polymerized toner was obtained in the same manner except that the viscosity of the dispersion was changed to 460 mPa · s (460 cP). The obtained toner had a weight average diameter of 8.8 μm and a rather broad particle size distribution. In the same manner as in Example 1, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope.

After the dispersing step was completed, the dispersion was recovered from the disperser, and the recoverability of the dispersion was good.
However, a visual inspection of the media after the completion of the dispersion revealed that the media was cracked (chipped), which is considered to be due to the high peripheral speed.

Comparative Example 3 In Example 1, the rotational speed of the rotor of the media type disperser was 640 rpm (the peripheral speed at the foremost part in the rotational direction of the rotor 2 m / s), the diameter of the media was 2.0 mm, and the viscosity of the dispersion liquid was changed. Was changed to 183 mPa · s (183 cP) to obtain a polymerized toner. The obtained toner had a weight average diameter of 8.9 μm and a rather broad particle size distribution. In the same manner as in Example 1, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 1 shows the results.

After the completion of the dispersion, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good. Further, after the completion of the dispersion, the media was visually inspected. I was not able to admit.

Comparative Example 4 A polymerized toner was obtained in the same manner as in Example 1, except that the diameter of the media was 0.05 mm and the viscosity of the dispersion was 260 mPa · s (260 cP). The obtained toner had a weight average diameter of 9.8 μm and had a rather broad particle size distribution.

In the same manner as in Example 1, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 1 shows the results.

After the dispersion was completed, the dispersion was recovered from the disperser. However, the recoverability of the dispersion was extremely poor due to the small outer diameter of the media. Furthermore, a visual inspection was performed on the media after the dispersion was completed, and no cracks (breaks) in the media were found.

Comparative Example 5 In Example 1, the rotational speed of the rotor of the media type disperser was 1600 rpm (the peripheral speed at the foremost portion in the rotational direction of the rotor 5 m / s) and the diameter of the media was 8 mm.
Polymerized toner was obtained by performing the same operation except that the viscosity of the dispersion was changed to 80 mPa · s (80 cP). The obtained toner had a weight average diameter of 9.8 μm and had a rather broad particle size distribution. The dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope in the same manner as in the examples. Table 1 shows the results.

After the dispersion was completed, the dispersion was recovered from the disperser. The recoverability of the dispersion was good. After the completion of the dispersion, the media was visually inspected. I was not able to admit.

[0103]

[Table 1] After warming the 0.1M-Na ₃ PO ₄ aqueous solution 451g to put to 60 ° C. Example 7 Ion-exchanged water 709 g, and stirred at 12,000rpm using a TK-type homomixer (manufactured by Tokushu Kika Kogyo) . A 1.0 M CaCl ₂ aqueous solution was added to the mixture.
7 g was gradually added to obtain an aqueous medium containing Ca ₃ (PO ₄ ) ₂ .

Paraffin wax (mp 70 ° C.) 1800 g C.I. I. Pigment Blue 15: 3 300 g Di-tert-butylsalicylate metal compound 150 g The above wax-based mixture (initial viscosity at 80 ° C. of 65)
mPa · s [cP]), heated to 80 ° C., equipped with a zirconia rotor and a stator having a hollow structure, and filled with 0.8 liter of zirconia beads having a diameter of 1.0 mm and a mill volume of 1 liter. Is supplied at a supply rate of 12 kg / h by a pump to a media-type dispersing machine as shown in FIG. 1 at a rotor rotation speed of 2500 rpm (a peripheral speed of the foremost part in the rotation direction of the rotor of 7.9 m / s),
Mill internal pressure 1 kg / cm ² , mill internal temperature 80 ° C, dispersed for 30 minutes by circulation method, viscosity 940 mPa · s (940
cP) at 80 ° C. to prepare a dispersion. In 75 g of the dispersion, a polymerizable monomer, 170 g of styrene, 30 g of 2-ethylhexyl acrylate, a polymerization initiator,
2'-azobis (2,4-dimethylvaleronitrile) 1
0 g and 1 g of dimethyl 2,2′-azobisisobutyrate were uniformly dissolved at 60 ° C. to prepare a polymerizable monomer system.

The above-mentioned polymerizable monomer system was charged into the aqueous medium, and the mixture was stirred at 10,000 rpm for 20 minutes with a TK homomixer at 60 ° C. in an N ₂ atmosphere to granulate the polymerizable monomer system. did. Thereafter, the mixture was reacted at 60 ° C. for 3 hours while stirring with a paddle stirring blade.
The reaction was performed for 0 hours.

Thereafter, the mixture was cooled, hydrochloric acid was added, and Ca ₃ (P
O ₄ ) ₂ was dissolved, filtered, washed with water and dried to obtain a polymerized toner. The particle diameter of the obtained toner is 8.4 μm in weight average diameter.
m and had a sharp particle size distribution. The endothermic peak top temperature measured by DSC was 70 ° C.

With respect to 100 parts by weight of the obtained toner, B
0.7 parts by weight of a hydrophobic silica having a specific surface area of 200 m ² / g by the ET method was externally added. 93 parts by weight of an acryl-coated ferrite carrier was mixed with 7 parts by weight of this toner to prepare a developer.

Using this developer and an externally added toner, an image was formed with a Canon full color copying machine CLC-500. Table 2 shows the results.

Regarding the dispersibility of the dispersion liquid, one or two drops of the dispersion liquid were dropped on a slide glass heated to 80 ° C., and a cover glass was placed thereon, and the dispersion was covered with an optical microscope BH2-UMA ( (Olympus Optical Co., Ltd.), and examined by observing the state of the dispersed particles of the colorant at a magnification of 200 times. Table 2 shows the results. Furthermore, regarding the granulation property in the granulation process, one or two drops of a granulation liquid were dropped on a slide glass, and a cover glass was placed on the slide glass, and an optical microscope BH2-UMA (manufactured by Olympus Optical Co., Ltd.) was used. It was examined by observing the size and distribution of the granulated particles at a magnification of 200 times. Table 2 shows the results. After the dispersion step, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good, and the media after the dispersion was visually inspected. Did not.

Example 8 The same wax-based mixture as in Example 7 was equipped at 80 ° C. with a zirconia rotor and a stator having a hollow structure, and filled with 0.9 liter of zirconia beads having a diameter of 1.0 mm. A media type disperser as shown in FIG. 1 having a mill volume of 1 liter was pumped to 7.2 kg / h.
And a rotor rotation speed of 2200 rpm (a peripheral speed of 6.9 m / at the foremost portion in the rotation direction of the rotor).
s), mill internal pressure 1.0 kg / cm ² , mill internal temperature 80 ° C
In one pass and the viscosity is 1200 mPa · s (1200
cP) at 80 ° C. to prepare a dispersion. In 75 g of the dispersion, a polymerizable monomer, 170 g of styrene, 30 g of 2-ethylhexyl acrylate, a polymerization initiator,
2'-azobis (2,4-dimethylvaleronitrile) 1
0 g and 1 g of dimethyl 2,2′-azobisisobutyrate were uniformly dissolved at 60 ° C. to prepare a polymerizable monomer system.

The above-mentioned polymerizable monomer system was charged into the aqueous medium, and the mixture was stirred at 10,000 rpm for 20 minutes with a TK homomixer at 60 ° C. in an N ₂ atmosphere to granulate the polymerizable monomer system. did. Thereafter, the mixture was reacted at 60 ° C. for 3 hours while stirring with a paddle stirring blade.
The reaction was performed for 0 hours.

Thereafter, the mixture was cooled, hydrochloric acid was added, and Ca ₃ (P
O ₄ ) ₂ was dissolved, filtered, washed with water and dried to obtain a polymerized toner. The particle diameter of the obtained toner is 8.5 μm in weight average diameter.
m and had a sharp particle size distribution. The endothermic peak top temperature measured by DSC was 70 ° C.

With respect to 100 parts by weight of the obtained toner, B
0.7 parts by weight of a hydrophobic silica having a specific surface area of 200 m ² / g by the ET method was externally added. 93 parts by weight of an acryl-coated ferrite carrier was mixed with 7 parts by weight of this toner to prepare a developer.

Using this developer and an externally added toner, an image was formed with a Canon full color copying machine CLC-500. Table 2 shows the results.

Regarding the dispersibility of the dispersion liquid, one or two drops of the dispersion liquid were dropped on a slide glass heated to 80 ° C., and a cover glass was placed thereon, and the dispersion was covered with an optical microscope BH2-UMA ( (Olympus Optical Co., Ltd.), and examined by observing the state of the dispersed particles of the colorant at a magnification of 200 times. Table 2 shows the results. Furthermore, regarding the granulation property in the granulation process, one or two drops of a granulation liquid were dropped on a slide glass, and a cover glass was placed on the slide glass, and an optical microscope BH2-UMA (manufactured by Olympus Optical Co., Ltd.) was used. It was examined by observing the size and distribution of the granulated particles at a magnification of 200 times. Table 2 shows the results.

After the completion of the dispersion step, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good, and the media after the completion of the dispersion was visually inspected. No abnormalities were observed.

Example 9 A polymerized toner was obtained in the same manner as in Example 7, except that the diameter of the media used was 2 mm, and the viscosity of the dispersion was 850 mPa · s (850 cP). The weight average diameter of the obtained toner was 8.6 μm and had a sharp particle size distribution.

In the same manner as in Example 7, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 2 shows the results.

After the dispersion step was completed, the dispersion was recovered from the disperser. The recoverability of the dispersion was good, and the media after the dispersion was visually inspected. No abnormalities were observed.

Example 10 In Example 7, the diameter of the media used was 0.3 m.
m, and the viscosity of the dispersion is 790 mPa · s (790 cP)
A polymerized toner was obtained in the same manner as described above.

The obtained toner had a weight average diameter of 8.4 μm and a sharp particle size distribution.

In the same manner as in Example 7, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 2 shows the results.

After the dispersion step was completed, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good, and the media after the dispersion was visually inspected. No abnormalities were observed.

Example 11 In Example 7, the rotation speed of the rotor of the media type dispersion machine was 1600 rpm (the peripheral speed at the foremost portion in the rotation direction of the rotor was 5 m / s), and the viscosity of the dispersion was 980 mPa · s.
Polymerized toner was obtained by performing the same operation except that s (980 cP) was used.

The obtained toner had a weight average diameter of 8.6 μm and a sharp particle size distribution.

In the same manner as in Example 7, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 2 shows the results.

After the dispersion step was completed, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good, and the media after the completion of the dispersion was visually inspected. No abnormalities were observed.

Example 12 In Example 7, the rotor speed of the media-type disperser was 4750 rpm (the peripheral speed at the foremost part in the rotor rotation direction was 15 m / s), and the viscosity of the dispersion was 1060 mP.
A polymerized toner was obtained by performing the same operation except that a · s (1060 cP) was used.

The obtained toner had a weight average diameter of 8.7 μm and a sharp particle size distribution.

In the same manner as in Example 7, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 2 shows the results.

After the completion of the dispersion step, the dispersion was recovered from the disperser. The recoverability of the dispersion was good, and the media after the completion of the dispersion was visually inspected. No abnormalities were observed.

Comparative Example 6 An aqueous medium was obtained in the same manner as in Example 7.

A polymerizable monomer mixture having the same composition as in Example 7 (initial viscosity at 80 ° C. 65 mPa · s [65c
P]) was heated to 80 ° C and pumped into a medialess disperser Ebara Milder (manufactured by Ebara Corporation) using a pump.
The rotor is supplied at a supply rate of 80 kg / h and the rotor speed is 5000
rpm (peripheral speed 1 at the tip of the rotor in the rotation direction)
5 m / s) for 60 minutes in a circulation system to prepare a dispersion (viscosity: 710 mPa · s [710 cP]). Thereafter, the operation was performed in the same manner as in Example 7 to obtain a polymerized toner.

The obtained toner has a weight average diameter of 10.3 μm.
And had a rather broad particle size distribution. In the same manner as in Example 7, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 2 shows the results.

Comparative Example 7 In Example 7, the rotor speed of the media-type dispersing machine was 7640 rpm (the peripheral speed at the foremost part in the rotation direction of the rotor 24 m / s) and the diameter of the media was 2.0 mm.
Polymerized toner was obtained by performing the same operation except that the dispersion liquid viscosity was changed to 950 mPa · s (950 cP). The obtained toner had a weight average diameter of 8.8 μm and a rather broad particle size distribution. In the same manner as in Example 7, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope.

After the dispersing step was completed, the dispersion was recovered from the disperser, and the recoverability of the dispersion was good.
However, when a visual inspection was performed on the media after the completion of dispersion, cracks (breaks) of the media, which are considered to be caused by the high peripheral speed, occurred.

Comparative Example 8 In Example 7, the rotational speed of the rotor of the media type disperser was 640 rpm (the peripheral speed at the foremost part in the rotational direction of the rotor 2 m / s), the diameter of the media was 2.0 mm, and the viscosity of the dispersion liquid was changed. Was changed to 372 mPa · s (372 cP) to obtain a polymerized toner. The obtained toner had a weight average diameter of 8.9 μm and a rather broad particle size distribution. In the same manner as in Example 7, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 2 shows the results.

After the dispersion was completed, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good. Further, after the dispersion was completed, the media was visually inspected. I was not able to admit.

Comparative Example 9 A polymerized toner was obtained in the same manner as in Example 7, except that the diameter of the media was 0.05 mm and the viscosity of the dispersion was 165 mPa · s (165 cP). The obtained toner had a weight average diameter of 9.2 μm and had a broad particle size distribution.

In the same manner as in Example 7, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope. Table 2 shows the results.

After the dispersion was completed, the dispersion was recovered from the disperser. However, the recoverability of the dispersion was extremely poor due to the small outer diameter of the media. Furthermore, a visual inspection was performed on the media after the dispersion was completed, and no cracks (breaks) in the media were found.

Comparative Example 10 In Example 7, the rotational speed of the rotor of the media type dispersing machine was 1600 rpm (the peripheral speed at the foremost portion in the rotational direction of the rotor 5 m / s) and the diameter of the media was 8 mm.
Polymerized toner was obtained by performing the same operation except that the dispersion viscosity was changed to 530 mPa · s (530 cP). The obtained toner had a weight average diameter of 9.8 μm and had a rather broad particle size distribution. In the same manner as in Example 7, the dispersibility of the dispersion and the granulation in the granulation step were examined with an optical microscope.

After the completion of the dispersion, the dispersion was recovered from the dispersing machine. The recoverability of the dispersion was good. Further, after the completion of the dispersion, the media was visually inspected. I was not able to admit.

[0144]

[Table 2]

[0145]

According to the present invention, by controlling the viscosity of the dispersion in the dispersion step, the dispersibility of the colorant is excellent,
In addition, since the dispersion time is shortened, the polymerized toner can be manufactured efficiently.

Further, when dispersed in a wax containing a polyalkylene-based wax, storage of the dispersion can be facilitated.

[Brief description of the drawings]

FIG. 1 is an explanatory view schematically showing a media type dispersing machine.

FIG. 2 is an explanatory view schematically showing another media-type dispersing machine.

FIG. 3 is an explanatory view schematically showing another media-type dispersing machine.

FIG. 4 is an explanatory view schematically showing another media type dispersing machine.

──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Tatehiko Chiba 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon Inc. (72) Inventor Makoto Shinbayashi 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon Inside (72) Inventor Koji Inaba 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon Inc. (72) Inventor Kasugani valuable Within 3-30-2 Shimomaruko, Ota-ku, Tokyo Canon Inc. (56) References JP-A-3-249761 (JP, A) JP-A-62-203167 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) G03G 9/08

Claims (6)

(57) [Claims] 1. A dispersing step of dispersing a colorant in a monomer system containing at least a polymerizable monomer, a step of dispersing the monomer system in an aqueous medium and granulating suspended particles, in the production method of polymerized toner for electrostatic image development comprising the step of polymerizing the resulting suspended particles in the dispersion step, Mediya rotor rotates and
Using Mediya type dispersing machine having a stator, the rotor
-The peripheral speed at the forefront in the direction of rotation is 3 m / s to 2
By rotating the rotor so as to be in the range of 0 m / s,
The initial viscosity of said monomer system 1mPa · s (1cP) to 1
Was prepared in a range of 00mPa · s (100cP), for developing an electrostatic image, wherein the Turkey controls the 10 to 1000 times the <br/> range of initial viscosity viscosity after dispersion of preparation liquid A method for producing a polymerized toner. Wherein said diameter of said Mediya of Mediya type dispersing machine, a manufacturing method of the polymerized toner according to claim 1 in the range of 0.1mm to 5 mm. 3. The rotation of the rotor of the media type disperser.
The peripheral speed of the outermost tip 5 in the rolling direction m / s to 15 m /
claim to be in the range of s Ru rotate the rotor 1
Or the method for producing a polymerized toner for developing an electrostatic image according to item 2. 4. A dispersing step of dispersing a colorant in a wax system containing at least a polyalkylene-based wax; a step of dissolving and mixing the wax system with a monomer system containing at least a polymerizable monomer; Dispersing the dissolution mixture in an aqueous medium, granulating suspended particles , and a method for producing a polymerized toner for electrostatic image development including a step of polymerizing the obtained suspended particles, in the dispersion step , Media, rotating rotor and
Using Mediya type dispersing machine having a stator, the rotor
-The peripheral speed at the forefront in the direction of rotation is 3 m / s to 2
By rotating the rotor so as to be in the range of 0 m / s,
The initial viscosity of the wax was prepared in a range of 1mPa · s (1cP) to 100mPa · s (100cP), 10 to 1000 times the initial viscosity viscosity after dispersion preparation liquid
Method for producing a polymerized toner for developing an electrostatic image Turkey be controlled in the range of the said. 5. The diameter of Mediya the Mediya type dispersing machine, a manufacturing method of the polymerized toner according to claim 4 in the range of 0.1mm to 5 mm. 6. The rotation of the rotor of the media type disperser.
The peripheral speed of the outermost tip 5 in the rolling direction m / s to 15 m /
The rotor is rotated so as to fall within the range of s.
Or the method for producing a polymerized toner for developing an electrostatic image according to item 5.