JP7414534B2 - Mechanical crusher for toner manufacturing, toner manufacturing method, and toner manufacturing system - Google Patents

Description

The present disclosure relates to a mechanical pulverizer for producing toner used in electrophotography, electrostatic recording, electrostatic printing, and toner jet methods, a method for producing toner, and a toner production system.

In recent years, electrophotographic full-color copying machines have become widespread and are beginning to be applied to the printing market. In the printing market, there is a growing demand for high speed, high image quality, and high productivity while supporting a wide range of media (paper types). In toner, in addition to stabilizing chargeability, developability, and transferability, high image quality can be achieved by further reducing the particle size.
A melt-kneading pulverization method is known as a general method for producing toner particles. Specifically, this is a method in which toner constituent materials such as a binder resin, a colorant, and a release agent are melt-kneaded, cooled and solidified, and then the kneaded material is pulverized by a crushing means to obtain toner particles. Thereafter, if necessary, the particles are classified into a desired particle size distribution or a fluidizing agent is added.
Various types of pulverizers are used as means for pulverizing the kneaded material, and the material to be pulverized is conveyed with high-pressure gas, injected from the outlet of the accelerating tube, and the collision surface of a collision member provided opposite the opening surface of the outlet of the accelerating tube. A collision-type air flow crusher (Patent Document 1) is known that crushes objects to be crushed by the impact force of the collision.
In addition, a rotor supported by a central rotating shaft and having a plurality of convex portions and concave portions on an outer circumferential surface is disposed within a casing having an input port and a discharge port for the material to be crushed; A stator is disposed with a predetermined gap between the outer circumferential surface of A mechanical crushing device (Patent Document 2) is known, which crushes the object by colliding with a convex part or a recess of a rotor or a stator when the object passes through a processing section where the rotor and the stator face each other. ing.

JP2006-051496A JP2011-237816A

In pulverizing the toner melt-kneaded material using the mechanical pulverizer as described above, by increasing the circumferential speed of the rotor of the mechanical pulverizer, the collision energy between the rotor and stator and the object to be pulverized is increased. It becomes possible to reduce the particle size of toner particles.
Furthermore, it is known that the particle size becomes smaller as the gap between the rotor and the stator through which the object to be crushed is narrowed.
In the case of such a mechanical pulverizer, when the object to be pulverized passes through the gap between the rotor and the stator, coarse particles are gradually pulverized and pulverized from upstream to downstream of the rotor and stator. At the same time, collision energy is accumulated in the object to be crushed, causing its temperature to rise.

For example, the temperature increase of the material to be crushed may occur when the rotation speed of the rotor is increased to grind toner particles into smaller particle sizes, or when the amount of material to be crushed per unit time is increased to improve productivity. It becomes more noticeable when increased.
For example, if the temperature of the object to be crushed becomes significant, the surface of the object to be crushed will partially melt, the objects to be crushed will bond together, and the particle size may become unstable. Furthermore, the objects to be crushed may adhere to the inside of the crusher (hereinafter, this phenomenon will be referred to as "fusion"), and stable crushing may not be possible.
The above-mentioned production stability and fusion are issues in toner production using the melt-kneading and pulverization method, particularly in the production of small particle size toner.
The present disclosure provides a mechanical pulverizer for toner production, a toner production method, and a toner production system that achieve reduction in the particle size of toner particles and improvement in productivity in a melt-kneading pulverization method.

One aspect of the present disclosure is
A mechanical crusher for toner production,
The crusher is
Inside the casing, which has an input port and a discharge port for the material to be crushed,
a cylindrical rotor supported by a central rotating shaft and having a plurality of convex portions and concave portions on an outer peripheral surface;
a stator disposed outside the rotor with a predetermined gap from the outer circumferential surface of the rotor, and having a plurality of convex portions and concave portions on the inner circumferential surface thereof;
The pulverizer passes the object to be pulverized through a gap formed between the inner circumferential surface of the stator and the outer circumferential surface of the rotor, and pulverizes the object.
Mechanical pulverization for toner production in which the gap distance when the tip of the convex portion of the rotor and the tip of the convex portion of the stator face each other is wider on the downstream side than on the upstream side in the passing direction of the object to be crushed. Regarding machines.
Further, other aspects of the present disclosure include:
A toner manufacturing method comprising a pulverizing step of pulverizing toner raw materials, the method comprising:
The present invention relates to a toner manufacturing method, wherein the pulverizer used in the pulverizing step is the above-mentioned mechanical pulverizer for toner manufacturing.
Further, other aspects of the present disclosure include:
A toner manufacturing system comprising: a first pulverizer that pulverizes a toner raw material to obtain a first pulverized product; and a second pulverizer that further pulverizes the first pulverized product.
The present invention relates to a toner manufacturing system in which at least the first pulverizer is the above-described mechanical pulverizer for manufacturing toner.

According to the present disclosure, it is possible to simultaneously improve productivity and reduce the particle size of toner particles in a melt-kneading and pulverizing method.

Schematic diagram of the mechanical crusher used in the examples Schematic diagram of the rotor and stator of the mechanical crusher used in the example Schematic diagram of a conventional mechanical crusher

Unless otherwise specified, the expression "XX to YY" or "XX to YY" indicating a numerical range means a numerical range including the lower limit and upper limit, which are the endpoints.
When numerical ranges are described in stages, the upper and lower limits of each numerical range can be arbitrarily combined.

The following are assumed to be the factors contributing to the above effects.
In a conventional mechanical crusher in which the gap between the rotor and the stator is constant, the particle size of the pulverized material is determined by the rotational speed of the rotor and the distance between the gap between the rotor and the stator.
As mentioned above, the higher the rotation speed of the rotor, the smaller the particle size of the object to be crushed, and the smaller the gap between the rotor and the stator, the smaller the particle size of the object to be crushed.
However, the smaller the particle size is, the more remarkable the temperature rise inside the pulverizer becomes, and when pulverizing toner raw materials, the above-mentioned problems of a decrease in stability of the particle size and a decrease in productivity occur as the temperature increases.

On the other hand, the mechanical crusher for producing toner has a configuration in which the distance between the rotor and the stator is wider on the downstream side than on the upstream side in the passing direction of the object to be crushed.
If the gap between the rotor and the stator is widened, the particle size of the material to be crushed will increase. However, in the mechanical crusher with the above configuration, even if the particle size is increased by increasing the rotation speed of the rotor, the temperature inside the machine and the rotation speed will be lower compared to the conventional mechanical crusher. The present inventors have experimentally confirmed that the load current required to drive the child can be suppressed.
Specifically, when toner raw material with a weight average particle size of about 100 μm is crushed to a particle size of 6.0 μm using a conventional crusher with a gap between the rotor and stator of 1.0 mm in the entire area, and when the gap on the upstream side is A comparison was made between pulverization to a particle size of 6.0 μm using a mechanical pulverizer with a gap of 1.0 mm and a gap of 1.4 mm in the downstream region up to 30% from the downstream end of the gap. By using the above-mentioned mechanical crusher, a decrease in the internal temperature of the machine and the load current required to drive the rotor was observed.

The mechanism by which such an effect is obtained is speculated as follows.
In the step of pulverizing using the mechanical pulverizer, toner raw material having a particle size called medium pulverized particles of approximately several tens of micrometers to several hundred micrometers is pulverized from finely pulverized particles to ultrafine pulverized particles of several micrometers.
During the process in which toner raw materials pass through the pulverizer while being pulverized, volumetric pulverization is mainly performed in the upstream part of the machine where medium pulverized particles are pulverized into finely pulverized particles. It is assumed that surface crushing is mainly performed in the downstream area where crushing occurs.
The energy required for pulverization is larger in volumetric pulverization than in surface pulverization, and the generated thermal energy is also greater.
In conventional crushers, the thermal energy generated upstream of the volumetric crushing is stored in the material to be crushed. Since surface pulverization is continued on the downstream side, it is thought that the temperature may exceed the temperature that softens the surface of the object to be pulverized.
Furthermore, it is speculated that energy exceeding the threshold value of energy required for surface pulverization is applied, accelerating the temperature rise of the material to be pulverized.

On the other hand, in the case of the above-mentioned mechanical crusher, the gap between the rotor and stator is set wide in the downstream area where surface crushing is mainly performed, so unnecessary surface crushing energy is applied to the material to be crushed. It is assumed that surface crushing will occur with a moderate amount of energy. From this, it is presumed that the energy accumulated in the object to be crushed on the upstream side causes surface crushing to be performed in the downstream region without adversely affecting the object to be crushed.
Furthermore, we believe that the wide gap between the rotor and stator in the downstream region increases the amount of gas air inside the machine during crushing, which lowers the temperature of the crushed material.
As a result, when using the above-mentioned mechanical crusher, compared to conventional crushers, it is possible to lower the internal temperature of the machine, stabilize the crushed particle size, suppress fusion, and achieve high productivity and small particles. We believe that it is possible to achieve both reductions in diameter.

First, the outline of the pulverization method using the mechanical pulverizer described above will be explained using FIG. 1.
Although FIG. 1 shows a schematic cross-sectional view of a horizontal mechanical crusher, a vertical mechanical crusher may also be used. A surface that rotates at high speed (outer surface ) A cylindrical rotor 103 is provided with a plurality of convex portions and concave portions, and a rotor 103 is arranged on the outside of the rotor 103 with a predetermined gap, and has a plurality of convex portions and concave portions on the surface (inner peripheral surface). It has a stator 104 provided, a raw material inlet 101 for introducing the material to be crushed, and a raw material outlet 106 for discharging the powder after processing.

In the mechanical pulverizer configured as described above, a predetermined amount of powder raw material is fed from the quantitative feeder to the raw material input port 101 of the mechanical pulverizer. The raw material passes through the front chamber 1021 in the mechanical crusher, passes through the crushing section created by the gap between the outer peripheral surface of the cylindrical rotor 103 and the inner peripheral surface of the stator 104, passes through the rear chamber 105, and then passes through the rear chamber 105. It is discharged from an outlet 106 communicating with the chamber 105.
The object to be crushed is crushed by collision with the convex or concave surface of the rotor rotating at high speed within the crushing processing section, or with the convex or concave surface of the stator. The to-be-pulverized material and the toner particles after being crushed are discharged out of the apparatus system along with the flow of air drawn by a suction blower (not shown).

Such a mechanical crusher can be obtained by appropriately modifying a conventional mechanical crusher. Conventional mechanical crushers include, for example, Inomizer (manufactured by Hosokawa Micron), Kryptolin (manufactured by Kawasaki Heavy Industries), Super Rotor (manufactured by Nisshin Engineering), Turbo Mill (manufactured by Turbo Kogyo), and Tornado Mill (manufactured by Nikkiso). (manufactured by).

The gap distance between the stator and rotor of the conventional mechanical crusher shown in FIG. 3 is constant. In the present disclosure, as illustrated in FIGS. 1 and 2, the tips of the protrusions of the stator and the tips of the protrusions of the rotor are opposed to each other on the upstream and downstream sides in the passing direction of the object to be crushed. The distance between the gaps is different. Furthermore, the distance between the gaps on the downstream side is wider than the distance between the gaps on the upstream side.
As a result, as mentioned above, the thermal energy accumulated upstream in the crusher is efficiently dissipated in the area where the gap between the rotor and stator is widened on the downstream side, causing a cooling effect on the material to be crushed. thinking.

In FIGS. 1 and 2, the distance between the gaps on the upstream side is constant, and the distance between the gaps on the downstream side is also constant, but the shapes of the rotor and stator are not limited to such shapes. The cross-sectional shape of the rotor in the direction of the central rotation axis may be inclined. For example, the cross-sectional shape of the rotor in the direction of the central rotation axis may be trapezoidal, or at least a portion of the cross-sectional shape of the rotor in the direction of the central rotation axis may have a tapered shape. On the other hand, similarly, the cross-sectional shape of the stator in the direction of the central rotation axis may be inclined.
Preferably, the distance of the gap on the upstream side is constant. Further, it is preferable that the distance of the gap on the downstream side is constant. The gap distance preferably changes in at least two steps (for example, two to four steps), and more preferably in two steps. As shown in FIGS. 1 and 2, it is preferable that the gap distance on the upstream side and the gap distance on the downstream side change stepwise. The stepped portion may be vertical or sloped. It is preferable that the stepwise change in the distance of the gap is performed by providing a step on the stator side.

In addition, the region where the gap distance on the downstream side is wider than that on the upstream side is determined based on the distance in the central rotation axis direction of the gap formed by the inner peripheral surface of the stator and the outer peripheral surface of the rotor. It is preferable that the range is 15% or more and 55% or less in the upstream direction of the central rotating shaft starting from the downstream end of the central rotating shaft. More preferably, the range is from 20% to 50% from the downstream end of the gap to the upstream direction of the central rotating shaft, and even more preferably from 25% to 40%.
When the area is 15% or more from the downstream end of the gap, the effect of lowering the temperature of the material to be crushed can be more easily obtained.
When the above region is 55% or less from the downstream end of the gap, the rotation speed of the rotor can be maintained within a suitable range to obtain the target particle size.

The distance of the gap on the downstream side is preferably 1.1 times or more and less than 2.1 times the distance of the gap on the upstream side. More preferably, it is 1.2 times or more and 2.0 times or less, and even more preferably 1.3 times or more and 1.8 times or less.
When the distance ratio of the gaps is 1.1 times or more, the effect of lowering the temperature of the material to be crushed can be easily obtained.
When the gap ratio is 2.1 times or less, the rotation speed of the rotor can be maintained within a suitable range to obtain the target particle size.

The distance of the upstream gap is preferably 0.5 mm to 2.0 mm, more preferably 0.7 mm to 1.5 mm.
The distance of the downstream gap is preferably 0.8 mm to 3.0 mm, more preferably 1.2 mm to 2.5 mm.
The distance in the direction of the central rotation axis of the gap formed between the inner circumferential surface of the stator and the outer circumferential surface of the rotor is preferably about 150 mm to 1000 mm, more preferably about 200 mm to 600 mm.

The shapes of the convex portions and concave portions on the inner circumferential surface of the stator are preferably such that linear grooves are formed along the direction of the central rotation axis. Moreover, it is preferable that the shape of the convex part and the concave part of the outer peripheral surface of the rotor is such that a linear groove is formed along the direction of the central rotation axis.
The distance from the tip of the convex part to the deepest part of the concave part is preferably about 1.0 mm to 5.0 mm, more preferably about 2.0 mm to 3.0 mm.
The distance between the protrusions is preferably about 1.0 mm to 8.0 mm, more preferably about 2.0 mm to 5.0 mm.
The diameter of the cross section perpendicular to the central rotational axis direction of the rotor is arbitrarily determined depending on the manufacturing scale and is not particularly limited, but is preferably about 100 mm to 900 mm, more preferably about 250 mm to 800 mm.

In the toner manufacturing method using the pulverization method, a coarse pulverization step to obtain a particle size of about 2 mm and a fine pulverization step to obtain a desired particle size may be employed. A medium pulverization step may be inserted between the coarse pulverization step and the fine pulverization step. The mechanical crusher described above can be used in either step. It is preferable to use the mechanical pulverizer described above in the medium pulverization step and/or the fine pulverization step. Further, the above-mentioned mechanical crushers may be connected in series or in parallel in two or more stages to perform crushing.
In the process of pulverizing small particle size toner having a weight average particle size of 4.0 μm, it is also effective to connect the mechanical pulverizers in series and perform pulverization in two stages.

For example, the following toner manufacturing system is preferable.
The toner manufacturing system includes a first pulverizer that pulverizes toner raw materials to obtain a first pulverized product, and a second pulverizer that further pulverizes the first pulverized product,
It is preferable that at least the first pulverizer is the above-described mechanical pulverizer for producing toner. More preferably, the first pulverizer and the second pulverizer are the above-described mechanical pulverizers for producing toner.

Further, the toner manufacturing method includes a pulverizing step of pulverizing toner raw materials,
The pulverizer used in the pulverizing step is preferably the above-described mechanical pulverizer for producing toner.
Further, the toner manufacturing method includes a pulverizing step of pulverizing toner raw materials,
The grinding step is
a first pulverizing step of pulverizing the toner raw material to obtain a first pulverized product; and a second pulverizing step of further pulverizing the first pulverized product;
It is preferable that the pulverizer used in at least the first pulverizing step is the above-mentioned mechanical pulverizer for producing toner. More preferably, the pulverizer used in the first pulverizing step and the second pulverizing step is the above-described mechanical pulverizer for producing toner.

The configuration for widening the gap is not limited to two-step change upstream and downstream. For example, it is effective to extend the flow toward the downstream in several stages, such as three or four stages.
Furthermore, it is also an effective means to continuously widen the gap toward the downstream side.

In the toner pulverization process, it is preferable that the rotational peripheral speed of the rotor is set to 180 m/sec or more and 230 m/sec or less. More preferably, the speed is 190 m/sec or more and 220 m/sec or less.
When the circumferential speed is 180 m/sec or more, the energy given to the object to be crushed increases when it collides with the stator and rotor in the crusher.
Therefore, the growth of cracks necessary for pulverizing the toner occurs appropriately near the toner surface, and as a result, surface pulverization occurs appropriately. When surface pulverization occurs appropriately in this manner, it is possible to suppress excessive generation of fine powder products that should be removed as a product toner.

When the circumferential speed is 230 m/sec or less, the energy given to the object to be crushed is appropriate. Therefore, it is possible to prevent excessive energy from acting not only on the pulverization of the object to be pulverized, but also as a force that deforms the toner, such as compression or shearing. As a result, flat or irregularly shaped toner is less likely to occur, and desired circularity can be imparted to the product.
Further, by operating the pulverizer within the above peripheral speed range, the particle size distribution of the obtained toner can be made sharp. When the pulverizing process is divided into a coarse pulverizing process and a fine pulverizing process, the process of operating the mechanical pulverizer in the above circumferential speed range is the process of determining the particle size distribution of the toner finally obtained. It is more preferable to apply it to the pulverization process.
Of course, it is also effective to apply the above process in pulverization processes other than the final step.

(Toner manufacturing procedure)
Next, a procedure for manufacturing toner particles using a mechanical crusher will be described.
First, in the raw material mixing step, predetermined amounts of a binder resin, a colorant, and the like are weighed, blended, and mixed. If necessary, a release agent that suppresses the occurrence of hot offset during heat fixing of the toner, a dispersant that disperses the release agent, a charge control agent, and the like may be mixed. Examples of mixing devices include a double con mixer, a V-type mixer, a drum-type mixer, a super mixer, a Henschel mixer, a Nauta mixer, and the like.

Further, the toner raw materials blended and mixed as described above are melt-kneaded to melt the resins and disperse the coloring agent and the like therein. In the melt-kneading step, for example, a batch-type kneader such as a pressure kneader or a Banbury mixer, or a continuous-type kneader can be used. In recent years, single-screw or twin-screw extruders have become mainstream due to their superiority in continuous production, such as the KTK-type twin-screw extruder manufactured by Kobe Steel, and the TEM-type twin-screw extruder manufactured by Toshiba Machinery Co., Ltd. , a twin-screw extruder manufactured by K.C.K., a co-kneader manufactured by Buss, etc. are generally used.
Further, the colored resin composition obtained by melt-kneading the toner raw materials is rolled after melt-kneading with two rolls or the like, and is cooled through a cooling step of cooling with water or the like.

The cooled colored resin composition obtained above is then pulverized to a desired particle size in a pulverization step. In the pulverization process, first, the material is coarsely pulverized using a crusher, hammer mill, feather mill, etc. Furthermore, it is finely pulverized using a mechanical pulverizer such as Inomizer (manufactured by Hosokawa Micron), Kryptron (manufactured by Kawasaki Heavy Industries, Ltd.), Super Rotor (manufactured by Nissin Engineering), or Turbo Mill (manufactured by Turbo Kogyo). In the pulverization step, the toner is pulverized in stages to a predetermined particle size. In the pulverizing step, it is preferable to use the mechanical pulverizer described above.

Next, toner will be explained.
<Binder resin>
The toner contains a binder resin. As the binder resin, common resins can be used, such as the following. Examples include polyester resin, styrene-acrylic acid copolymer, polyolefin resin, vinyl resin, fluororesin, phenol resin, silicone resin, and epoxy resin.
Among these, amorphous polyester resins are preferred from the viewpoint of improving low-temperature fixability. From the viewpoint of achieving both low-temperature fixability and hot offset resistance, it is preferable to use a low-molecular-weight polyester and a high-molecular-weight polyester together. Further, from the viewpoint of further improving low-temperature fixing properties and blocking resistance during storage, crystalline polyester may be used as a plasticizer.

<Colorant>
The toner contains a colorant. As the coloring agent, the following may be mentioned.
Examples of the coloring agent include known organic pigments, oil dyes, carbon black, and magnetic materials.
Examples of the cyan colorant include copper phthalocyanine compounds and derivatives thereof, anthraquinone compounds, and basic dye lake compounds.
Examples of magenta colorants include condensed azo compounds, diketopyrrolopyrrole compounds, anthraquinone compounds, quinacridone compounds, basic dye lake compounds, naphthol compounds, benzimidazolone compounds, thioindigo compounds, perylene compounds, and the like.
Examples of the yellow colorant include condensed azo compounds, isoindolinone compounds, anthraquinone compounds, azo metal complexes, methine compounds, and allylamide compounds.
Examples of the black colorant include carbon black, a magnetic material, and those toned to black using the yellow colorant, magenta colorant, and cyan colorant described above.
These colorants can be used alone or in combination of two or more.

<Release agent>
If necessary, a release agent may be used in the toner to suppress the occurrence of hot offset during heat fixing of the toner. Common examples of the mold release agent include low molecular weight polyolefins, silicone waxes, fatty acid amides, ester waxes, carnauba wax, and hydrocarbon waxes.

Next, a method for measuring the weight average particle diameter (D4) of toner particles will be explained.
<Method for measuring weight average particle diameter (D4) of toner particles>
The weight average particle diameter (D4) of the toner particles was measured using a precise particle size distribution measuring device "Coulter Counter Multisizer 3" (registered trademark, manufactured by Beckman Coulter) equipped with a 50 μm aperture tube using the pore electrical resistance method. The attached special software “Beckman Coulter Multisizer 3” is used to set conditions and analyze measurement data.
Version 3.51 (manufactured by Beckman Coulter) with an effective measurement channel count of 25,000 channels, and the measurement data is analyzed and calculated.
The electrolytic aqueous solution used in the measurement can be one in which special grade sodium chloride is dissolved in ion-exchanged water to have a concentration of about 1% by mass, such as "ISOTON II" (manufactured by Beckman Coulter).
Note that before performing measurement and analysis, the dedicated software is set as follows.
In the "Change standard measurement method (SOM) screen" of the dedicated software, set the total count in control mode to 50,000 particles, set the number of measurements to 1, and set the Kd value to "standard particle 10.0 μm" (Beckman Coulter). Set the value obtained using By pressing the threshold/noise level measurement button, the threshold and noise level are automatically set. Also, set the current to 1600 μA, the gain to 2, the electrolyte to ISOTON II, and check the aperture tube flush after measurement.
On the "Pulse to particle size conversion setting screen" of the dedicated software, set the bin interval to logarithmic particle size, the particle size bin to 256 particle size bins, and the particle size range to 1 μm or more and 30 μm or less.

The specific measurement method is as follows.
(1) Approximately 200 ml of the above electrolyte aqueous solution is placed in a 250 ml round-bottom glass beaker exclusively for Multisizer 3, set on a sample stand, and stirred with a stirrer rod counterclockwise at 24 revolutions/second. Then, use the dedicated software's ``Aperture Tube Flush'' function to remove dirt and air bubbles from inside the aperture tube.
(2) Pour about 30 ml of the above electrolytic aqueous solution into a 100 ml glass flat-bottomed beaker, and add "Contaminon N" as a dispersant (precision measurement of pH 7 consisting of nonionic surfactant, anionic surfactant, and organic builder). Approximately 0.3 ml of a diluted solution prepared by diluting a 10% by mass aqueous solution of a neutral detergent for cleaning utensils (manufactured by Wako Pure Chemical Industries, Ltd.) by 3 times by mass with ion-exchanged water is added.
(3) Two oscillators with an oscillation frequency of 50 kHz are built in with their phases shifted by 180 degrees, and are placed in the water tank of an ultrasonic dispersion device "Ultrasonic Dispersion System Tetora 150" (manufactured by Nikkaki Bios Co., Ltd.) with an electrical output of 120 W. A predetermined amount of ion-exchanged water is poured into the water tank, and approximately 2 ml of the contaminon N is added to the water tank.
(4) Set the beaker of (2) above in the beaker fixing hole of the ultrasonic disperser, and operate the ultrasonic disperser. Then, the height position of the beaker is adjusted so that the resonance state of the liquid level of the electrolytic aqueous solution in the beaker is maximized.
(5) While the electrolytic aqueous solution in the beaker of (4) is irradiated with ultrasonic waves, about 10 mg of toner is added little by little to the electrolytic aqueous solution and dispersed. Then, the ultrasonic dispersion treatment is continued for another 60 seconds. In addition, in the ultrasonic dispersion, the water temperature in the water tank is appropriately adjusted to be 10° C. or more and 40° C. or less.
(6) Using a pipette, drop the electrolytic aqueous solution of (5) in which toner is dispersed into the round-bottomed beaker of (1) placed in the sample stand, and adjust the measured concentration to approximately 5%. . Then, the measurement is continued until the number of particles to be measured reaches 50,000.
(7) Analyze the measurement data using the dedicated software attached to the device and calculate the weight average particle diameter (D4). Note that when the dedicated software is set to graph/volume %, the "average diameter" on the analysis/volume statistics (arithmetic mean) screen is the weight average particle diameter (D4).

<Method for measuring number average particle diameter (D1) of toner particles>
In step (7) of the method for measuring the number average particle diameter (D4) of toner particles, when the graph/number % is set in the dedicated software, the "average diameter" on the analysis/number statistics (arithmetic mean) screen is It is the number average particle diameter (D1).

<Method of measuring average circularity>
The average circularity of toner particles is measured using a flow type particle image analyzer "FPIA-3000" (manufactured by Sysmex Corporation) under measurement and analysis conditions during calibration work.
The specific measurement method is as follows. First, approximately 20 ml of ion-exchanged water from which impure solid matter has been removed is placed in a glass container. Contaminon N is used as a dispersant (a 10% by mass aqueous solution of a neutral detergent for cleaning precision measuring instruments with a pH of 7 consisting of a nonionic surfactant, an anionic surfactant, and an organic builder, manufactured by Wako Pure Chemical Industries, Ltd.) ) is diluted to about 3 times the mass with ion-exchanged water, and then add about 0.2 ml of the diluted solution.
Furthermore, approximately 0.02 g of the measurement sample is added, and a dispersion process is performed for 2 minutes using an ultrasonic disperser to obtain a dispersion liquid for measurement. At that time, the temperature of the dispersion liquid is appropriately cooled to a temperature of 10° C. or higher and 40° C. or lower. As the ultrasonic disperser, a table-top ultrasonic cleaner disperser ("VS-150" (manufactured by Vervo Crea)) with an oscillation frequency of 50 kHz and an electrical output of 150 W was used, and a predetermined amount of ions were placed in the water tank. Replacement water is poured into the tank, and approximately 2 ml of the contaminon N is added to the tank.

For the measurement, the flow-type particle image analyzer equipped with a standard objective lens (10x magnification) was used, and a particle sheath "PSE-900A" (manufactured by Sysmex Corporation) was used as the sheath liquid. The dispersion liquid prepared according to the above procedure is introduced into the flow type particle image analyzer, and 3000 toner particles are measured in the HPF measurement mode and the total count mode. Then, the binarization threshold at the time of particle analysis is set to 85%, the analyzed particle diameter is limited to an equivalent circle diameter of 1.985 μm or more and less than 39.69 μm, and the average circularity of the toner particles is determined.
In the measurement, automatic focus adjustment is performed using standard latex particles ("RESEARCH AND TEST PARTICLES Latex Microsphere Suspensions 5200A" manufactured by Duke Scientific, diluted with ion-exchanged water) before starting the measurement. Thereafter, it is preferable to perform focus adjustment every two hours from the start of the measurement.
In this example, a flow-type particle image analyzer was used, which was calibrated by Sysmex and had a calibration certificate issued by Sysmex. The measurement was carried out under the measurement and analysis conditions under which the calibration certificate was received, except that the particle diameter for analysis was limited to an equivalent circle diameter of 1.985 μm or more and less than 39.69 μm.

EXAMPLES Hereinafter, the present invention will be explained in more detail using Examples and Comparative Examples, but these are not intended to limit the present invention in any way. In addition, in the following prescriptions, parts are based on mass unless otherwise specified.

<Production example of amorphous polyester resin L>
・Polyoxypropylene (2.2)-2,2-bis(4-hydroxyphenyl)propane: 72.0 parts (0.20 mol; 100.0 mol% based on the total number of moles of polyhydric alcohol)
·Terephthalic acid:
28.0 parts (0.17 mol; 96.0 mol% based on the total number of moles of polycarboxylic acids)
- Tin 2-ethylhexanoate (esterification catalyst): 0.5 part The above materials were weighed into a reaction tank equipped with a cooling tube, a stirrer, a nitrogen introduction tube, and a thermocouple. Next, after purging the inside of the flask with nitrogen gas, the temperature was gradually raised while stirring, and reaction was carried out for 4 hours while stirring at a temperature of 200°C.
Furthermore, the pressure inside the reaction tank was lowered to 8.3 kPa and maintained for 1 hour, then cooled to 180° C. and returned to atmospheric pressure.
・Trimellitic anhydride:
1.3 parts (0.01 mol; 4.0 mol% based on the total number of moles of polycarboxylic acids)
・Tert-butylcatechol (polymerization inhibitor): 0.1 part After that, the above materials were added, the pressure inside the reaction tank was lowered to 8.3 kPa, and the reaction was carried out for 1 hour while maintaining the temperature at 180°C, and ASTM D36- After confirming that the softening point measured according to No. 86 reached 90° C., the temperature was lowered to stop the reaction, and amorphous polyester resin L was obtained.

<Production example of amorphous polyester resin H>
・Polyoxypropylene (2.2)-2,2-bis(4-hydroxyphenyl)propane: 72.3 parts (0.20 mol; 100.0 mol% based on the total number of moles of polyhydric alcohol)
·Terephthalic acid:
18.3 parts (0.11 mol; 65.0 mol% based on the total number of moles of polycarboxylic acids)
・Fumaric acid:
2.9 parts (0.03 mol; 15.0 mol% based on the total number of moles of polycarboxylic acids)
- Tin 2-ethylhexanoate (esterification catalyst): 0.5 part The above materials were weighed into a reaction tank equipped with a cooling tube, a stirrer, a nitrogen introduction tube, and a thermocouple. Next, after purging the inside of the flask with nitrogen gas, the temperature was gradually raised while stirring, and the mixture was reacted for 2 hours while stirring at a temperature of 200°C.
Furthermore, the pressure inside the reaction tank was lowered to 8.3 kPa and maintained for 1 hour, then cooled to 180°C and returned to atmospheric pressure.
・Trimellitic anhydride:
6.5 parts (0.03 mol; 20.0 mol% based on the total number of moles of polyhydric carboxylic acid)
・Tert-butylcatechol (polymerization inhibitor): 0.1 part After that, the above materials were added, the pressure inside the reaction tank was lowered to 8.3 kPa, and the reaction was carried out for 15 hours while maintaining the temperature at 160°C, and ASTM D36- After confirming that the softening point measured according to No. 86 reached 137° C., the temperature was lowered to stop the reaction, and an amorphous polyester resin H was obtained.

<Crystalline polyester resin>
・1,6-hexanediol:
34.5 parts (0.29 mol; 100.0 mol% based on the total number of moles of polyhydric alcohol)
・Dodecanedioic acid:
65.5 parts (0.28 mol; 100.0 mol% based on the total number of moles of polycarboxylic acids)
- Tin 2-ethylhexanoate: 0.5 part The above materials were weighed into a reaction tank equipped with a cooling tube, a stirrer, a nitrogen introduction tube, and a thermocouple. After purging the inside of the flask with nitrogen gas, the temperature was gradually raised while stirring, and the reaction was carried out at a temperature of 140° C. for 3 hours while stirring.
Next, the above materials were added, the pressure inside the reaction tank was lowered to 8.3 kPa, and the reaction was carried out for 4 hours while maintaining the temperature at 200° C. to obtain a crystalline polyester resin.

<Toner manufacturing example>
- Amorphous polyester resin L 70 parts - Amorphous polyester resin H 30 parts - Crystalline polyester resin 5 parts - Fischer-Tropsch wax (hydrocarbon wax, maximum endothermic peak temperature 90°C) 8 parts - C.I. I. Pigment Blue 15:3 7 parts The above materials were mixed using a Henschel mixer (model FM-75, manufactured by Mitsui Mining Co., Ltd.) at a rotation speed of 20 s ^-1 and a rotation time of 5 min, and then mixed with a twin-screw kneader (PCM- 30 model, manufactured by Ikegai Co., Ltd.). The barrel temperature during kneading was set so that the outlet temperature of the kneaded product was 120°C. The outlet temperature of the kneaded material was directly measured using a handy type thermometer HA-200E manufactured by Anritsu Keiki Co., Ltd. The obtained kneaded product was cooled and coarsely pulverized using a pin mill to a volume average particle size of 100 μm or less to obtain toner raw material 1.

Specific examples and comparative examples will be described below.
The weight average particle size of the finely pulverized products obtained in the following Examples and Comparative Examples was measured according to the method for measuring the weight average particle size (D4) of toner particles described above.
(Example 1)
In this example, the crusher shown in FIG. 1 is used.
The configuration of the pulverizer shown in FIG. 1 is a modified mechanical pulverizer (turbo mill T250-CRS-rotor shape RS type manufactured by Turbo Kogyo Co., Ltd.).
FIG. 2 is a diagram schematically showing the configuration of a rotor and a stator.
In FIG. 2, 103 represents a rotor, and 104 represents a stator. D1 and D2 represent the distance of the gap when the tip of the convex portion of the stator and the tip of the convex portion of the rotor face each other.
L1 indicates the area of the gap D1 (the area where the gap distance is D1 from the upstream end of the gap), and L2 indicates the area of the gap D2 (the area where the gap distance is D2 from the downstream end of the gap). It shows.
A pulverized product was produced using the above-mentioned mechanical pulverizer using Toner Raw Material 1 under the conditions shown below.

<Condition 1> Feed=30Kg/h
Using the pulverizer shown in FIG. 1, toner raw material 1 was supplied from the supply port at a rate of 30 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and pulverization was performed at a cold air temperature of -10°C.
In addition, the configuration of the crusher under these conditions is as shown in FIG. 2, D1 = 1.0 mm, D2 = 1.5 mm, L1 = 224 mm, L2 = 96 mm (L2 is the area up to 30% from the downstream end of the gap).
Under condition 1, first, the peripheral speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 6.0 μm to 6.2 μm, and then production was continued for 10 hours under the same conditions to produce a pulverized product of approximately 300 kg. I got it.

<Condition 2> Feed=40Kg/h
In this condition, with the same pulverizer configuration as in Condition 1, toner raw material 1 is supplied from the supply port at a rate of 40 kg/h, cold air is flowed in at a flow rate of 4 m ³ /min, and pulverization is performed at a cold air temperature of -10°C. went.
In Condition 2, the peripheral speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 6.0 μm to 6.2 μm, and then production was continued for 10 hours under the same conditions to produce a pulverized product of approximately 400 kg. I got it.

(Comparative example 1)
In this comparative example, the crusher shown in FIG. 3 is used.
The pulverizer shown in Fig. 3 is a mechanical pulverizer (turbo mill T250-CRS-rotor shape RS type manufactured by Turbo Kogyo Co., Ltd.), and the gap between the rotor and stator is in all areas where the rotor and stator face each other. Uniform. The gap distance was 1.0 mm.
In this comparative example, toner raw material 1 was used, and in the same manner as in Example 1, the supply amount from the supply port was 30 kg/h under condition 1 and 40 kg/h under condition 2, and cold air was introduced at an air volume of 4 m ³ /min. Grinding was carried out at a temperature of -10°C.
In this comparative example as well, the circumferential speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 6.0 μm to 6.2 μm under each condition, and then production was continued for 10 hours under the same conditions. Approximately 300 kg of pulverized products were obtained under condition 1 and approximately 400 kg under condition 2.

In the present examples and comparative examples, the manufactured finely pulverized products were sampled every hour, the weight average particle diameter (D4) was measured, and the particle size stability of the finely pulverized products was evaluated.
For evaluation, the difference between the maximum and minimum sampled particle sizes was calculated, and the results were ranked as follows.
A: Less than 0.2 μm, very good.
B...0.2 μm or more and less than 0.4 μm, which is good.
C...0.4 μm or more.

Further, after 10 continuous hours of production, the apparatus was stopped and the degree of toner adhesion (staining) on the rotor and stator was visually confirmed.
The evaluation ranks are as follows.
A: Very good, almost no adhesion.
B... Some adhesion is observed, but it is good.
C: Adhesion is observed.

Table 1 shows the evaluation results under each condition in Example 1 and Comparative Example 1.
As shown in Table 1, the pulverized products produced by the pulverizer of the example have excellent particle size stability.
Furthermore, there is almost no toner adhesion inside the machine after long periods of production, resulting in excellent productivity.
Moreover, compared to the comparative example, when the processing amount was increased and the conditions were made more severe, the effect was more pronounced.

(Example 2)
Using the crusher shown in FIG. 1, pulverized products were manufactured by changing L1 and L2, which indicate regions in which the distance between the rotor 103 and the stator 104 differs, as shown in FIG.
Specifically, L1 and L2 were changed under each condition shown in Table 2, and the ratio of L2 from the downstream end of the gap was changed from 10% to 60%.
In addition, other configurations of the pulverizer were set as D1=1.0 mm and D2=1.5 mm in FIG. 2.
Toner raw material 1 was supplied from the supply port at a rate of 40 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and toner raw material 1 was pulverized at a cold air temperature of -10°C.
In this example, the circumferential speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 5.0 μm to 5.2 μm, and then production was continued for 10 hours under the same conditions to produce a product of approximately 400 kg. A crushed product was obtained.

(Comparative example 2)
Production was continued for 10 hours using the same pulverizer configuration and conditions as Comparative Example 1, except that the peripheral speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 5.0 μm to 5.2 μm. Approximately 400 kg of crushed product will be obtained.
In this Example and Comparative Example, the same evaluation as in Example 1 and Comparative Example 1 was performed. The results are shown in Table 2.
In this example, under the condition that the ratio of the region L2 from the downstream end where the gap is enlarged is 60%, the set particle size is not reached even at the upper limit of the rotation speed of the crusher, and the toner raw material from the supply port is A pulverized product was produced by lowering the feed rate of No. 1 to 30 kg/h.

The throughput was ranked as follows, and a comprehensive evaluation was performed for each item.
Evaluation of throughput A: A throughput of 40 kg/h or more was obtained for the set particle size.
B: A throughput of 30 kg/h was obtained for the set particle size, but a throughput of 40 kg/h was not obtained.
C: A throughput of 20 kg/h was obtained for the set particle size, but a throughput of 30 kg/h was not obtained.

Overall rating: A: All evaluation items were ranked A.
B: In each evaluation item, at least one item had a B rank as the lowest rank.
C...In each evaluation item, there was even one item with C rank as the lowest rank.

As shown in Table 2, good results were obtained in the Examples. In particular, good results were obtained in all items when the ratio of the area where the distance between the downstream rotor and stator gap was increased was 20% to 50%.

表中、「Ｌ２の割合」は、隙間の距離が上流側よりも広くなっている下流側の領域の割合である。

In the table, "Ratio of L2" is the ratio of the region on the downstream side where the gap distance is wider than on the upstream side.

(Example 3)
In this example as well, the crusher shown in FIG. 1 is used.
In this example, pulverized products were manufactured by varying the distances D1 and D2 of the gap between the rotor 103 and the stator 104 shown in FIG.
Specifically, D1 and D2 are set to the values shown in Table 3 under each condition, and the ratio of the distance D2 of the gap between the rotor and stator on the downstream side to the distance D1 of the gap between the rotor and stator on the upstream side (D2 /D1) was varied in the range of 1.1 to 2.1.
In addition, in FIG. 2, the region where the distance of the gap on the downstream side in this example is widened is L1=224 mm and L2=96 mm (region up to 30% from the downstream end of the gap).
The manufacturing conditions for the pulverized product were as follows: 40 kg/h of toner raw material 1 was flowed through the supply port at a flow rate of 4 m ³ /min of cold air, and the toner raw material 1 was pulverized under the condition that the temperature of the cold air was -10°C.
In this example, the circumferential speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 5.0 μm to 5.2 μm, and then production was continued for 10 hours under the same conditions to produce a product of approximately 400 kg. A crushed product shall be obtained.

In this example as well, the same evaluation as in Example 2 was carried out, and the results are shown in Table 3.
In this example, under the condition that D2/D1 is 2.1, even the upper limit of the rotation speed of the crusher does not reach the set particle size, and the amount of toner raw material 1 supplied from the supply port is reduced to 30 kg/ A pulverized product was prepared by lowering the temperature to h.
As shown in Table 3, good results were obtained in the Examples. In particular, good results were obtained in all items when D2/D1 was in the range of 1.2 to 2.0.

(Example 4)
In this example, a pulverizer with the configuration used in Example 1 was used in the first pulverization process, and a conventional pulverizer with the configuration used in Comparative Example 1 was used in the second pulverization process to produce pulverized products. Created.
First, in order to obtain a pulverized product with a weight average particle size of 4.2 μm to 4.4 μm, the particle size set in the first pulverization step was set to a weight average particle size of 5.0 μm to 5.2 μm. The manufacturing conditions for the pulverized product were as follows: Toner raw material 1 was supplied from the supply port at a rate of 40 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and toner raw material 1 was pulverized at a cold air temperature of -10°C.
The peripheral speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 5.0 μm to 5.2 μm, and then production was continued for 10 hours under the same conditions to obtain a pulverized product weighing approximately 400 kg. .
Next, the pulverized product obtained in the first pulverization step was subjected to a second pulverization step. The peripheral speed of the rotor is set so that the weight average particle diameter of the pulverized product is in the range of 4.2 μm to 4.4 μm, and then production is continued for 10 hours under the same conditions to obtain a pulverized product weighing approximately 400 kg. .

(Example 5)
In this example, a pulverized product was produced using the pulverizer having the configuration used in Example 1 in both the first pulverization step and the second pulverization step.
In this example, as in Example 4, in order to obtain a pulverized product with a weight average particle size of 4.2 μm to 4.4 μm, the particle size set in the first pulverization step was set to 5.0 μm to 5.0 μm. It was set to 2 μm. The manufacturing conditions for the pulverized product were as follows: Toner raw material 1 was supplied from the supply port at a rate of 40 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and toner raw material 1 was pulverized at a cold air temperature of -10°C.
The peripheral speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 5.0 μm to 5.2 μm, and then production was continued for 10 hours under the same conditions to obtain a pulverized product weighing approximately 400 kg. .
Next, the pulverized product obtained in the first pulverization step was subjected to a second pulverization step. The peripheral speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 4.2 μm to 4.4 μm, and then production was continued for 10 hours under the same conditions to obtain a pulverized product weighing about 400 kg.

(Comparative example 3)
In this comparative example, a pulverized product was produced using the pulverizer having the configuration used in comparative example 1 in both the first pulverizing step and the second pulverizing step.
In this comparative example, as in Example 4, in order to obtain a pulverized product with a weight average particle size of 4.2 μm to 4.4 μm, the particle size set in the first pulverization step was changed to a weight average particle size of 5.0 μm to 5.0 μm. 2 μm, and the manufacturing conditions for the pulverized product were as follows: Toner raw material 1 was supplied from the supply port at 40 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and toner raw material 1 was pulverized at a cold air temperature of -10°C. .
In this comparative example as well, the circumferential speed of the rotor was set so that the weight average particle size of the pulverized product was in the range of 5.0 μm to 5.2 μm, and then production was continued for 10 hours under the same conditions to produce a product weighing approximately 400 kg. A crushed product was obtained.
Next, the pulverized product obtained in the first pulverization step was subjected to a second pulverization step. The peripheral speed of the rotor is set so that the weight average particle diameter of the pulverized product is in the range of 4.2 μm to 4.4 μm, and then production is continued for 10 hours under the same conditions to obtain a pulverized product weighing approximately 400 kg. .

In Examples 4 and 5 and Comparative Example 3, the same evaluation as in Example 3 was performed. The results are shown in Table 4.
In the second pulverization process of Example 4 and Comparative Example 3, the rotor motor load current reached the upper limit and did not reach the set particle size, so the amount of toner supplied from the supply port was reduced to 30 kg/h. A pulverized product was prepared by lowering the powder.

As shown in Table 4, in a pulverization system that uses a first pulverization step and a second pulverization step to pulverize toner raw materials to a weight average particle size of about 4 μm, at least the first pulverization step is performed using the pulverizer of the embodiment. Good results were obtained using .
Furthermore, by using the pulverizer of the example in both the first pulverizing step and the second pulverizing step, even better results were obtained that were excellent in all items.

(Example 6)
In this example as well, the crusher shown in FIG. 1 is used.
In this example, the peripheral speed of rotation of the rotor 103 shown in FIG. 2 was changed.
In addition, other configurations of the crusher in this example were D1=1.0 mm and D2=1.5 mm in FIG. 2.
The manufacturing conditions for the pulverized product were as follows: Toner raw material 1 was supplied from the supply port at a rate of 40 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and toner raw material 1 was pulverized at a cold air temperature of -10°C.
In this example, L1 and L2 were set so that the weight average particle size of the pulverized product was in the range of 5.0 μm to 5.2 μm, and then production was continued for 10 hours under the same conditions to produce a pulverized product weighing approximately 400 kg. I got it.

Evaluation of average circularity A: 0.955 or more B: 0.950 or more and less than 0.955

Evaluation of D4/D1 (evaluation of particle size distribution)
A...Less than 1.30 B...1.30 or more and less than 1.40

Overall rating: A: All evaluation items were ranked A.
B: In each evaluation item, at least one item had a B rank as the lowest rank.

As shown in Table 5, good results were obtained in the Examples. In particular, good results were obtained in all items when the peripheral speed was 200 m/sec.

(Example 7)
In this example as well, the crusher shown in FIG. 1 is used.
In this example as well, the peripheral speed of rotation of the rotor 103 shown in FIG. 2 was changed, and D2/D1 was changed so that the weight average particle size of the pulverized product was in the range of 5.0 μm to 5.2 μm. Ta.
In addition, in FIG. 2, the region where the distance of the gap on the downstream side in this example is widened is L1=224 mm and L2=96 mm (region up to 30% from the downstream end of the gap).
The manufacturing conditions for the pulverized product were as follows: Toner raw material 1 was supplied from the supply port at a rate of 40 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and toner raw material 1 was pulverized at a cold air temperature of -10°C.
In this example, production is continued for 10 hours under the same conditions to obtain a pulverized product weighing about 400 kg.
In this example as well, the same evaluation as in Example 6 was performed. The results are shown in Table 6.
In this example, under the condition that D2/D1 is 2.1, even the upper limit of the rotation speed of the crusher does not reach the set particle size, and the amount of toner raw material 1 supplied from the supply port is reduced to 30 kg/ A pulverized product was prepared by lowering the temperature to h.

As shown in Table 6, good results were obtained in the Examples. In particular, good results were obtained in all items when the peripheral speed was 200 m/sec.

(Example 8)
In this example, in both the first crushing process and the second crushing process, the crusher shown in FIG. 1 was used, and the peripheral speed of rotation of the rotor 103 shown in FIG. 2 was fixed at 160 m/sec. Shredded. In addition, in FIG. 2, the region where the distance of the gap on the downstream side in this example is widened is L1=224 mm and L2=96 mm (region up to 30% from the downstream end of the gap).
First, in order to obtain a pulverized product with a weight average particle size of 4.2 μm to 4.4 μm, the particle size set in the first pulverization step was set to a weight average particle size of 5.0 μm to 5.2 μm. The manufacturing conditions for the pulverized product were as follows: Toner raw material 1 was supplied from the supply port at a rate of 40 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and toner raw material 1 was pulverized at a cold air temperature of -10°C.
Incidentally, D2/D1 was changed so that the weight average particle diameter of the pulverized product was in the range of 5.0 μm to 5.2 μm, and then production was continued for 10 hours under the same conditions to obtain a pulverized product weighing about 400 kg.
Next, the pulverized product obtained in the first pulverization step was subjected to a second pulverization step. D2/D1 was changed so that the weight average particle size of the pulverized product was in the range of 4.2 μm to 4.4 μm, and then production was continued for 10 hours under the same conditions to obtain a pulverized product weighing about 400 kg.

(Example 9)
In this example, the crusher shown in FIG. 1 was used in both the first crushing process and the second crushing process. Pulverization was carried out with the peripheral speed of rotation of the rotor 103 shown in FIG. 2 fixed at 160 m/sec in the first crushing process and 200 m/sec in the second crushing process. In addition, in FIG. 2, the region where the distance of the gap on the downstream side in this example is widened is L1=224 mm and L2=96 mm (region up to 30% from the downstream end of the gap).
First, in order to obtain a pulverized product with a weight average particle size of 4.2 μm to 4.4 μm, the particle size set in the first pulverization step was set to a weight average particle size of 5.0 μm to 5.2 μm. The manufacturing conditions for the pulverized product were as follows: Toner raw material 1 was supplied from the supply port at a rate of 40 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and toner raw material 1 was pulverized at a cold air temperature of -10°C.
Incidentally, D2/D1 was changed so that the weight average particle diameter of the pulverized product was in the range of 5.0 μm to 5.2 μm, and then production was continued for 10 hours under the same conditions to obtain a pulverized product weighing about 400 kg.
Next, the pulverized product obtained in the first pulverization step was subjected to a second pulverization step. D2/D1 was changed so that the weight average particle diameter of the pulverized product was in the range of 4.2 μm to 4.4 μm, and then production was continued for 10 hours under the same conditions to obtain a pulverized product weighing about 400 kg.

(Example 10)
In this example, the crusher shown in FIG. 1 was used in both the first crushing process and the second crushing process. Pulverization was carried out with the peripheral speed of rotation of the rotor 103 shown in FIG. 2 fixed at 200 m/sec. In addition, in FIG. 2, the region where the distance of the gap on the downstream side in this example is widened is L1=224 mm and L2=96 mm (region up to 30% from the downstream end of the gap).
First, in order to obtain a pulverized product with a weight average particle size of 4.2 μm to 4.4 μm, the particle size set in the first pulverization step was set to a weight average particle size of 5.0 μm to 5.2 μm. The manufacturing conditions for the pulverized product were as follows: Toner raw material 1 was supplied from the supply port at a rate of 40 kg/h, cold air was flowed in at a flow rate of 4 m ³ /min, and toner raw material 1 was pulverized at a cold air temperature of -10°C.
Incidentally, D2/D1 was changed so that the weight average particle diameter of the pulverized product was in the range of 5.0 μm to 5.2 μm, and then production was continued for 10 hours under the same conditions to obtain a pulverized product weighing about 400 kg.
Next, the pulverized product obtained in the first pulverization step was subjected to a second pulverization step. D2/D1 was changed so that the weight average particle diameter of the pulverized product was in the range of 4.2 μm to 4.4 μm, and then production was continued for 10 hours under the same conditions to obtain a pulverized product weighing about 400 kg.

In Examples 8, 9, and 10, the same evaluation as in Example 6 was performed. The results are shown in Table 7.
As shown in Table 7, in a pulverization system that uses a first pulverization step and a second pulverization step to pulverize toner raw materials into a weight average particle diameter of 4 μm, the pulverizer of the embodiment is used at least in the second pulverization step. Good results were obtained using .

101: Supply port, 1021: Front chamber, 1022: Front chamber outlet, 103: Rotor, 104: Stator, 105: Rear chamber, 106: Discharge port, 107: Rotating shaft, 108: Cold air generator, 109: Cold water supply port, 110: Cold water discharge port

Claims (8)

A mechanical crusher for toner production,
The crusher is
Inside the casing, which has an input port and a discharge port for the material to be crushed,
a cylindrical rotor supported by a central rotating shaft and having a plurality of convex portions and concave portions on an outer peripheral surface;
a stator disposed outside the rotor with a predetermined gap from the outer circumferential surface of the rotor, and having a plurality of convex portions and concave portions on the inner circumferential surface thereof;
The pulverizer passes the object to be pulverized through a gap formed between the inner circumferential surface of the stator and the outer circumferential surface of the rotor, and pulverizes the object.
When the tip of the convex part of the rotor and the tip of the convex part of the stator face each other, the gap distance is wider on the downstream side than on the upstream side in the passing direction of the object to be crushed,
Even on the downstream side, where the distance between the gaps when the tips of the convex portions of the rotor and the tips of the convex portions of the stator face each other is wide, the outer peripheral surface of the rotor and the stator A mechanical crusher for producing toner, characterized in that the inner peripheral surface has the convex portion and the concave portion . A region on the downstream side where the gap distance is wider than on the upstream side,
The toner production according to claim 1, wherein the distance in the direction of the center rotation axis of the gap is in the range of 15% or more and upstream of the center rotation axis from the downstream end of the gap to 55% or less. mechanical crusher. 3. The mechanical crusher for producing toner according to claim 1, wherein the distance of the downstream gap is 1.1 times or more and 2.1 times or less the distance of the upstream gap. A toner manufacturing method comprising a pulverizing step of pulverizing toner raw materials, the method comprising:
A method for producing toner, characterized in that the pulverizer used in the pulverizing step is the mechanical pulverizer for toner production according to any one of claims 1 to 3. A toner manufacturing method comprising a pulverizing step of pulverizing toner raw materials, the method comprising:
The grinding step is
a first pulverizing step of pulverizing the toner raw material to obtain a first pulverized product; and a second pulverizing step of further pulverizing the first pulverized product;
A method for producing a toner, wherein the pulverizer used in at least the first pulverizing step is the mechanical pulverizer for toner production according to any one of claims 1 to 3. 6. The toner manufacturing method according to claim 4, wherein in the pulverizing step, the peripheral speed of rotation of the rotor in the mechanical pulverizer for toner manufacturing is set to 180 m/sec or more and 230 m/sec or less. A toner manufacturing method comprising a pulverizing step of pulverizing toner raw materials, the method comprising:
The grinding step is
a first pulverizing step of pulverizing the toner raw material to obtain a first pulverized product; and a second pulverizing step of further pulverizing the first pulverized product;
The pulverizer used in the first pulverizing step and the second pulverizing step is a mechanical pulverizer for toner production according to any one of claims 1 to 3,
A toner manufacturing method, wherein in at least the second pulverizing step, the rotation peripheral speed of the rotor in the toner manufacturing mechanical pulverizer is set to 180 m/sec or more and 230 m/sec or less. A toner manufacturing system comprising: a first pulverizer that pulverizes a toner raw material to obtain a first pulverized product; and a second pulverizer that further pulverizes the first pulverized product.
A toner manufacturing system, wherein at least the first pulverizer is a mechanical pulverizer for toner manufacturing according to any one of claims 1 to 3.

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