JP2013178562A - Method for producing toner - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing toner capable of reducing an increase in temperature in a pulverization chamber or a decrease in cooling efficiency caused by high-speed rotation of a rotor even in a large-scale pulverizer having a coolant channel for cooling inside the rotor.SOLUTION: There is provided a method for producing toner having a step of pulverizing a coarsely pulverized product by pulverizing means and classifying the resulting pulverized product with classification means, wherein a pulverizer used for the pulverizing means has a stator and a rotor attached to a central rotary shaft, the stator includes the rotor and is arranged so that the surface of the stator and the surface of the rotor have a gap to form a pulverizing zone, a product to be pulverized is pulverized with the rotation of the rotor in the pulverizing zone, the stator and the rotor have a plurality of concave parts and convex parts, the unevenness is provided in parallel to the central rotary shaft, and the temperature Trin (°C) of the coolant introduced into a coolant channel of the rotor is -20.0≤Trin≤20.0.

Description

  The present invention relates to a method for producing a toner used in an image forming method such as an electrophotographic method, an electrostatic recording method, an electrostatic printing method, or a toner jet recording method.

  In image forming methods such as electrophotography, electrostatic photography, and electrostatic printing, toner for developing an electrostatic charge image is used. One of the methods for producing toner is the following method.

  First, a binder resin for fixing to a transfer material, various colorants for producing a color as a toner, and a charge control agent for imparting electric charge to particles are used as raw materials. Other additives such as a mold and a fluidity-imparting agent are added and dry mixing is performed.

  After that, after melt-kneading with a general-purpose kneading device such as a roll mill or an extruder and cooling and solidifying, the kneaded material is refined with various pulverizing devices, and the obtained coarsely pulverized material is introduced into various wind classifiers for classification. By performing, a classified product having a particle size required for the toner is obtained.

  Further, a fluidizing agent, a lubricant and the like are externally added as necessary, and dry-mixed to obtain a toner for image formation.

  In the case of a toner used in the two-component development method, various magnetic carriers and the above toner are mixed and then used for image formation.

Various pulverizers are used as the pulverizing means. Particularly, in recent years, energy saving of the apparatus has been demanded from the viewpoint of reducing CO ₂ emission, and a pulverizer as shown in FIG. 6 with low power consumption is used. There are many cases.

  In the pulverizer shown in FIG. 6, the material to be pulverized is introduced by introducing a powder raw material into a pulverization zone formed between a rotor 314 rotating at high speed and a stator 310 arranged around the rotor 314. Crush.

  Therefore, according to the pulverizer, a large amount of air is not required for pulverization unlike the jet airflow pulverizer.

  Therefore, power consumption is very small, and it is possible to finely pulverize with much energy saving compared to a jet airflow pulverizer. In addition, since it is less pulverized than a jet airflow type pulverizer, the generation of fine powder is small, and it is possible to improve the classification yield in the subsequent classification process.

  Further, when attention is paid to the shape of the toner fine particles pulverized by these pulverizers, the toner fine particles pulverized in are irregular and angular shapes, and the toner particles pulverized by the pulverizer shown in FIG. It is known that the shape has roundness.

  For this reason, the toner particles pulverized by the pulverizer shown in FIG. 6 have a smaller specific surface area than the toner particles pulverized by the jet airflow pulverizer, so that the fluidity is good and the voids are small. There is an advantage that the filling property is excellent, and the addition amount of the external additive is small.

  That is, according to the pulverizer shown in FIG. 6, it is possible to produce toner of excellent quality with energy saving and high yield.

  However, the pulverizer shown in FIG. 6 is pulverized by introducing a powder raw material into a pulverization zone formed between a rotor 314 rotating at high speed and a stator 310 disposed around the rotor 314. Therefore, most of the factors that determine the toner particle diameter are considered to be determined by the number of rotations of the rotor 314 and the minimum distance between the rotor 314 and the stator 310.

  Therefore, if the pulverizer shown in FIG. 6 is used to obtain toner particles having a small particle diameter of 6 μm or less, the speed of the rotor 314 is increased and the minimum distance between the rotor 314 and the stator 310 is reduced. Necessary.

  However, the number of rotations of the rotor 314 and the minimum distance between the rotor 314 and the stator 310 are naturally limited in the apparatus configuration. Therefore, in the pulverizer shown in FIG. It was very difficult to obtain toner particles.

  Further, when the processing amount per unit time is increased while the rotor 314 is rotated at a high speed, the temperature of the object to be pulverized and the temperature of the air in the pulverization chamber increase due to frictional heat at the time of pulverization. Since in-machine fusion occurs, it is not preferable in terms of toner productivity.

  As a countermeasure, in order to prevent adverse effects on quality due to temperature rise in the crushing chamber and in-machine fusion, it is possible to increase the minimum gap between the rotor 314 and the stator 310, but the processing amount per unit time can be increased, The desired toner particle diameter cannot be maintained.

  As a result, the burden on the next classification step is increased, which is not preferable in terms of toner productivity.

  In order to suppress the above-described increase in the temperature in the pulverization chamber, the pulverizer disclosed in Patent Document 1 includes a pulverizer in which an inner refrigerant circulation path for circulating the refrigerant inside the rotor and cooling the rotor is formed. It has been proposed (see FIGS. 4 and 7).

  In the pulverizer shown in FIG. 4, the rotor 614 itself is a single unit in which a plurality of disks 322 having the same shape are combined.

  Each unit is formed with a refrigerant reservoir 616 constituting the inner refrigerant circulation path and a communication hole that communicates the refrigerant reservoir with each other along the outer periphery.

  Furthermore, a plurality of communication holes that communicate with the refrigerant storage portion 616 are provided along the outer peripheral portion of the unit, and the refrigerant storage portion is disposed inside the refrigerant storage portion 616 of the unit. A refrigerant shielding portion 615 is formed to limit the unit only to the outer peripheral portion.

  According to Patent Document 1, an extremely high cooling effect can be obtained by circulating a refrigerant inside the rotor 614.

  Therefore, at the time of pulverization, the objects to be crushed may be melted and fused to each other, or the rotor 614 and the stator 610 may be fused to be pulverized, or the object to be crushed may be deteriorated by heat. It is supposed to be prevented.

  Furthermore, since it is possible to efficiently pulverize a granular material that is vulnerable to heat, productivity is improved.

  However, when the size of the apparatus is increased with the configuration of the rotor 614 described above, there is a problem in that the main body vibration value in the high-speed rotation region of the rotor 614 is high and the pulverizer is stably operated.

  The reason is considered to be the deviation of the refrigerant in the refrigerant reservoir 616 accompanying the increase in the size of the rotor 614 and the high-speed rotation.

  As described above, if the rotor 614 cannot be stably rotated at a high speed, in order to obtain a desired toner particle diameter, the processing amount per unit time must be reduced, which is satisfactory from the viewpoint of toner productivity. Absent.

  Further, the pulverizer disclosed in Patent Document 1 has a configuration in which at least one of the concave portion of the rotor 614 and the concave portion of the stator 610 is inclined in a direction that hinders the flow of the object to be pulverized (FIG. 5). reference).

  With the configuration shown in FIG. 5, it is possible to increase the time for which the pulverized particles stay in the pulverization chamber, thereby preventing excessive pulverization, reducing the particle diameter, and simultaneously preventing the generation of coarse particles.

  This is because at least one of the concave portion of the rotor 614 and the concave portion of the stator 610 is inclined in a direction that obstructs the flow of the object to be pulverized, so that the object to be pulverized can be smoothly moved in the air flow direction. This is because it is hindered and acts to hinder the flow of the powder object.

  However, when the size of the apparatus is increased by the configuration of the rotor 614 and the stator 610 described above and the processing amount per unit time is increased, the temperature rise in the grinding chamber in the high-speed rotation region of the rotor 614 is quick, and the grinding machine There is a problem in terms of stable operation.

  The reason is considered to be that the time during which the powdered material stays in the grinding chamber becomes excessively long in the high-speed rotation region of the rotor 614 as the apparatus becomes larger.

  The above-described increase in the temperature of the pulverization chamber is directly linked to toner quality problems and in-machine fusion. Therefore, in order to prevent adverse toner quality and in-machine fusion, the amount of processing per unit time must be reduced, which is also not satisfactory from the viewpoint of toner productivity.

JP 2004-42029 A

  An object of the present invention is to solve the problems of the prior art, and even in a large pulverizer equipped with a cooling refrigerant flow path inside the rotor, the temperature rise of the pulverization chamber and the main body accompanying the high-speed rotation of the rotor To provide a toner manufacturing method capable of reducing an increase in vibration value and a decrease in cooling efficiency.

  As a result of investigations to solve the above-described problems of the prior art, the inventors have found the cause of the increase in the main body vibration value in the high-speed rotation range that occurs when the apparatus is enlarged with the configuration of the rotor 614 described above. The present invention is considered to be biased by a change in the weight of the refrigerant itself when the refrigerant flows.

  Further, it is considered that the cause of the temperature rise in the crushing chamber generated when the apparatus is enlarged with the configuration of the rotor 614 and the stator 610 described above is that the residence time in which the powdered material stays in the crushing chamber is exceeded. Invented.

  Further, the present inventors have considered that the cause of the decrease in cooling efficiency is the relationship between the temperature and flow rate of the refrigerant flowing through the rotor and the jacket provided in the pulverizer.

That is, a mixture containing at least a binder resin and a colorant is melt-kneaded, the obtained kneaded product is cooled, the cooled product is coarsely pulverized, and the obtained coarsely pulverized product is pulverized by a pulverizing means. In the method for producing a toner having at least a step of classifying the pulverized product by classification means,
The pulverizer used in the pulverizing means comprises at least a powder inlet for charging a coarsely pulverized product into the pulverizing means, a stator, a rotor attached to a central rotating shaft, and pulverized powder. A powder outlet for discharging from the pulverizing means,
The stator includes the rotor, and the rotor surface and the rotor surface are arranged so that there is a gap between the rotor and the rotor surface to form a grinding zone;
In the pulverization zone, the object to be crushed is pulverized as the rotor rotates, and the stator and the rotor have a plurality of convex portions and concave portions,
The unevenness is provided in parallel to the central rotation axis, and the rotor includes a cooling coolant channel inside.
The temperature Trin (° C.) of the refrigerant introduced into the refrigerant flow path is −20.0 ≦ Trin ≦ 20.0.
The present invention relates to a toner production method.

  According to the present invention, even in a large pulverizer equipped with a cooling refrigerant flow path inside the rotor 314, a decrease in cooling efficiency and in-machine fusion due to high-speed rotation of the rotor 314 can be prevented, and a unit per unit time can be prevented. The throughput can be improved. Furthermore, it is possible to obtain toner particles having a sharp particle size distribution and rounded, efficiently and stably, and with good toner productivity.

It is the schematic of an example rotor and stator used in this invention. It is a schematic sectional drawing of an example rotor used in this invention. It is a schematic sectional drawing of an example rotor used in this invention. It is a schematic sectional drawing of an example rotor used in the conventional crushing process. It is the schematic of an example rotor and stator used in the conventional crushing process. It is a schematic sectional drawing of an example grinder used in the present invention. It is a schematic sectional drawing of the crusher of an example used in a comparative example and a reference example.

  Hereinafter, the present invention will be described in more detail with reference to preferred embodiments.

  As a result of studies to solve the above-described problems of the prior art, the present inventors have found that the cause of the increase in the temperature of the crushing chamber and the increase in the vibration value of the main body caused by the high-speed rotation of the rotor in a large crusher We thought that there was a bias due to changes in the weight of the refrigerant itself during water and a lack of cooling area inside the rotor.

  Furthermore, in the large pulverizer, the cause of the temperature increase in the pulverization chamber caused by the high-speed rotation of the rotor is due to the shortage of the cooling area inside the rotor 614 and the excess of the residence time in which the powdered material stays in the pulverization chamber. I thought it was.

  In other words, if the refrigerant flow path that can eliminate the bias due to the change in the weight of the refrigerant itself and increase the cooling area is configured, the temperature rise in the grinding chamber and the main body vibration value associated with the high-speed rotation of the rotor can be reduced. It was possible to obtain high cooling efficiency.

  Furthermore, if the structure of the plurality of uneven portions on the surface of the stator and the rotor is configured so that the powdered material does not stay excessively in the grinding chamber, the temperature of the grinding chamber accompanying the high-speed rotation of the rotor is reduced. We thought that the temperature rise could be reduced.

  In order to achieve the above-described object in the present invention, a configuration of a preferable apparatus will be described with reference to FIGS.

  FIG. 1 shows an example of a schematic view of a rotor and a stator of a crusher used in the present invention, and FIGS. 2 and 3 show an example of a schematic cross-sectional view of a rotor used in the present invention.

The pulverizer according to the present invention includes a powder inlet 311 for introducing a material to be crushed into the pulverizing means, a stator 310, a rotor 314 attached to at least the central rotating shaft 312 and pulverized powder. And at least a powder discharge port 302 for discharging the powder from the pulverizing means,
(1) The stator 310 includes the rotor 314;
(2) The surface of the stator 310 and the surface of the rotor 314 are arranged such that the rotor 314 has a predetermined gap to form a grinding zone,
(3) In the pulverization zone, the object to be crushed is pulverized as the rotor 314 rotates,
(4) The surface of the stator 310 and the surface of the rotor 314 are both pulverizers having a plurality of convex portions and concave portions,
(5) As shown in FIG. 1, the concavo-convex portion is provided in parallel to the central rotation axis 312.
(6) As shown in FIG. 2, it is preferable that the rotor 314 has a cooling refrigerant flow path N therein.

Furthermore, as shown in FIG.
(1) The rotor 314 has a plurality of recesses on the outer peripheral surface,
(2) The rotor 314 includes a cooling coolant flow path N therein,
(3) A length obtained by connecting a straight line from the center point p of the rotor 314 to the concave bottom surface r of the rotor 314 is defined as Dpr,
(4) When D pq is a length obtained by connecting a straight line from the center point p of the rotor 314 to the outermost shell q of the refrigerant flow path,
(5) It is preferable to provide a cooling refrigerant flow path N so as to satisfy the following expression (1).
Formula (1) 1.0 mm <= Dpr-Dpq <= 25.0mm

Further, the refrigerant flow path inside the rotor 314 of the present invention is as shown in FIG.
(1) Refrigerant flow path L for introducing a refrigerant from one direction on the powder inlet 311 side or the powder outlet 302 side via the central rotating shaft 312,
(2) Refrigerant flow path M for conveying the refrigerant to the outer layer portion in the rotor 314,
(3) Refrigerant flow path N for conveying the refrigerant in the outer layer portion of the rotor 314 in parallel with the central rotation shaft 312;
(4) a refrigerant flow path P for conveying the refrigerant from the outer layer portion of the rotor 314 toward the central rotation shaft 312;
(5) Refrigerant flow path Q for discharging refrigerant in the same direction region or in the opposite direction with respect to the refrigerant introduction direction
It is preferable that it is the structure of these.

  The rotor 314 of the present invention has a configuration in which a plurality of independent disks 322 are connected as shown in FIG.

  That is, the rotor 314 of the present invention is provided with the refrigerant flow path M for conveying the refrigerant to the outer layer portion in each disk 322 independently according to the number of the disks 322.

  Further, the refrigerant can be separately introduced from the refrigerant flow path L into the refrigerant flow path M provided independently according to the number of the disks 322.

  Furthermore, the rotor 314 of the present invention is provided with the refrigerant flow path P for conveying the refrigerant from the outer layer portion of each disk 322 toward the central rotation shaft 312 according to the number of the disks 322.

  Further, the refrigerant can be separately returned to the refrigerant flow path Q from the refrigerant flow path P provided independently according to the number of the disks.

  As a result of the study by the present inventors, the rotor 314 having the above-described configuration enables the pulverization chamber temperature accompanying the high-speed rotation of the rotor 314 even in a large-scale pulverizer having a cooling coolant channel therein. Temperature increase and increase in the body vibration value can be reduced.

  Furthermore, it is possible to prevent adverse effects on quality due to a rise in the temperature in the grinding chamber and in-machine fusion, and further, the throughput per unit time can be improved. Toner particles having a sharp particle size distribution can be efficiently and stably In particular, it can be obtained with good toner productivity.

  In the rotor 314 of the present invention, the refrigerant flow path M for conveying the refrigerant to the outer layer portion in each disk 322 is preferably composed of a plurality of independent disks 322. .

  Further, in the rotor 314 of the present invention, the refrigerant flow path P for conveying the refrigerant from the outer layer portion of each disk 322 toward the central rotating shaft 312 is constituted by a plurality of independent disks 322. It is preferred that

  Furthermore, the rotor 314 of the present invention is configured so that the number of flow paths in the refrigerant flow path M for conveying the refrigerant to the outer layer portion in each disk 322 and the refrigerant from the outer layer portion of each disk 322 toward the central rotating shaft 312. It is preferable that the number of flow paths in the refrigerant flow path P for transporting is the same.

  Further, the sizes of the flow path M and the flow path P are equal to each other in diameter and length, thereby canceling out the resistance caused by the centrifugal force and stable refrigerant without being affected by the rotational speed of the rotor 314. A flow rate can be obtained.

  In addition, the processing of the flow path M and the flow path P is performed by drilling from the surface layer toward the center of the shaft with a drill, inserting a plug to a position where it crosses the cooling hole later, and filling the surface layer back by welding. Apply.

Furthermore, as a result of examination by the inventors, as shown in FIG.
(1) A length obtained by connecting a straight line from the center point p of the rotor 314 to the concave bottom surface r of the rotor 314 is Dpr,
(2) When Dp q is a length obtained by connecting a straight line from the center point p of the rotor 314 to the outermost shell q of the refrigerant flow path,
(3) By providing a cooling coolant flow path so as to satisfy the following formula (1), the vibration value can be reduced and high cooling efficiency can be obtained even at high speed rotation of the rotor 314. I understood that.
Formula (1) 1.0 mm <= Dpr-Dpq <= 25.0mm

  As a result of studies by the present inventors, in the formula (1), when Dpr-Dpq is less than 1.0 mm, the vibration value associated with the high-speed rotation of the rotor 314 increases, and the rotor 314 has a high-speed rotation. It is not satisfactory from the point of stable operation.

  Furthermore, as a result of studies by the present inventors, when Dpr-Dpq exceeds 25.0 mm, a sufficient cooling effect cannot be obtained this time, so the throughput per unit time cannot be improved. Is not satisfactory enough.

  Next, an outline of a pulverization method using a pulverizer used in the toner production method of the present invention will be described with reference to FIG.

  FIG. 6 shows an example of a grinding system incorporating a grinding machine used in the present invention.

  FIG. 6 shows a schematic cross-sectional view of a horizontal general pulverizer. As a result of the study by the present inventors, the horizontal pulverizer is more advantageous in terms of vibration when it is configured to have a cooling refrigerant flow path inside the rotor 314 compared to the vertical pulverizer. I found out.

  As a reason, the rotor 314 includes a cooling coolant channel inside, and if water is passed through the coolant channel, the rotor 314 inevitably increases in weight. In the case of a vertical pulverizer, this increased amount is disadvantageous in terms of vibration because the load is inevitably applied to the lower part of the rotor 314.

  However, in the case of a horizontal pulverizer, even if the weight of the rotor 314 increases, the increase is applied evenly to the left and right of the rotor 314, so it is considered advantageous in terms of vibration.

  The pulverizer in FIG. 6 is provided with a number of grooves on the surface formed of a casing 313, a jacket 316 that allows water to flow through the casing 313, and a rotating body that is attached to the central rotary shaft 312 in the casing 313. And a rotor 314.

  Further, the pulverizer in FIG. 6 includes a stator 310 provided with a large number of grooves on the outer surface of the rotor 314 arranged at regular intervals, and a powder for introducing a raw material to be treated. The body is composed of a body inlet 311 and a powder outlet 302 for discharging the processed powder.

  As described above, the rotor 314 has a configuration in which a plurality of independent disks 322 are connected.

  In the pulverizer configured as described above, when a predetermined amount of the powder raw material is charged into the powder inlet 311 of the mechanical pulverizer from the quantitative feeder 315 shown in FIG. It is introduced into a grinding zone which is a grinding treatment chamber which is a gap between the rotor 314 and the stator 310.

  The impact generated between the rotor 314 provided with a large number of grooves on the surface rotating at a high speed in the grinding chamber and the stator 310 provided with a large number of grooves on the surface, and behind this It is pulverized instantaneously by a large number of ultra-high speed eddy currents.

  Thereafter, the powder is discharged through the powder discharge port 302. The air carrying the particles (air) passes through the pulverization chamber, passes through the collecting cyclone 229, the bag filter 222, and the suction blower 224, and is discharged out of the system.

  In the present invention, since the powder raw material is pulverized in this manner, a desired pulverization treatment can be easily performed without increasing the fine powder and coarse powder.

  In the toner manufacturing method of the present invention, it is preferable that the concavo-convex portion is provided in parallel to the central rotation shaft 312.

  By providing the concavo-convex portion in parallel to the central rotating shaft 312, it is possible to prevent adverse effects on quality and in-machine fusion due to a rise in the temperature in the grinding chamber when the rotor 314 rotates at high speed.

  This is because by providing the concavo-convex portion in parallel to the central rotation shaft 312, it is possible to prevent the powder material from staying in the crushing chamber for an excessively long time.

  In the toner production method of the present invention, the interdental distance formed by the irregularities is preferably 1.0 or more and 6.0 mm or less, and more preferably 2.0 or more and 5.0 mm or less. Further preferred.

  In addition, when the interdental distance formed by the unevenness is less than 1.0 mm, the throughput per unit time cannot be improved. Further, there is a possibility of causing a short pass without being pulverized, which is not satisfactory from the viewpoint of toner productivity.

  In addition, when the interdental distance formed by the unevenness exceeds 6.0 mm, the particle size obtained even when the rotor 314 is rotated at a high speed becomes large, and toner particles having a desired small particle size cannot be obtained. The quality is not satisfactory.

  In the toner production method of the present invention, the minimum distance between the surface of the rotor 314 and the surface of the stator 310 in the pulverizer is preferably 0.5 to 10.0 mm, and preferably 0.5 to 5 mm. More preferably, it is 0.0 mm.

  When the minimum distance between the rotor 314 and the stator 310 in the pulverizer is less than 0.5 mm, the load on the apparatus itself is increased, and at the same time, the pulverization is excessively pulverized and the toner is thermally deteriorated and fused in the machine. This is also not satisfactory from the viewpoint of toner productivity.

  Further, when the minimum distance between the rotor 314 and the stator 310 in the pulverizer exceeds 10.0 mm, a short pass is caused without being pulverized, which is not satisfactory from the viewpoint of toner productivity.

  Furthermore, in the toner manufacturing method of the present invention, the rotational peripheral speed of the rotor 314 is preferably 30 m / sec to 175 m / sec, and more preferably 40 m / sec to 160 m / sec.

  As a result of investigations by the present inventors, if the rotational peripheral speed of the rotor 314 is less than 30 m / sec, in order to obtain a toner having a small particle size, the amount of processing per unit time must be reduced. It is not satisfactory enough.

  Further, if the rotational peripheral speed of the rotor 314 exceeds 175 m / sec, the load on the apparatus itself increases, and at the same time, the material to be pulverized is excessively pulverized during pulverization, and at the same time, surface alteration due to heat and in-machine melting This is also unsatisfactory in terms of toner productivity because it tends to wear.

  Next, a method for producing the toner of the present invention will be described.

  First, in the raw material mixing step, as a toner internal additive, at least a resin and a colorant are weighed and mixed in a predetermined amount and mixed. Examples of the mixing apparatus include a double-con mixer, a V-type mixer, a drum-type mixer, a super mixer, a Henschel mixer, and a Nauter mixer.

  Further, the toner raw materials blended and mixed as described above are melt-kneaded to melt the resins and disperse the colorant and the like therein. In the melt-kneading step, for example, a batch kneader such as a pressure kneader or a Banbury mixer, or a continuous kneader can be used.

  In recent years, single-screw or twin-screw extruders have become mainstream due to the advantage of being capable of continuous production. For example, KTK type twin screw extruder manufactured by Kobe Steel, TEM type twin screw extruder manufactured by Toshiba Machine Co., Ltd. In general, a twin-screw extruder manufactured by Kay Sea Kay, a co-kneader manufactured by Buss, or the like is used.

  Furthermore, the colored resin composition obtained by melt-kneading the toner raw material is rolled by a two-roll roll after melt-kneading, and then cooled through a cooling step of cooling by water cooling or the like.

  The cooled product of the colored resin composition obtained above is pulverized to a desired particle size in the fine pulverization step through the coarse pulverization step.

  In the coarse pulverization step, a crusher such as a crusher, a hammer mill, or a feather mill is usually used. In the toner production method of the present invention, the particle size of the coarsely pulverized product supplied to the fine pulverization step is 50 μm or more and 300 μm. The following is preferable.

  When the particle size of the coarsely pulverized product supplied to the pulverization step exceeds 300 μm, the productivity improvement effect may not be achieved with respect to the fine particles. Further, when the particle size of the coarsely pulverized product is less than 50 μm, the influence on the pulverization step and the subsequent steps is small, but it becomes difficult to control the temperature in the pulverizer used in the coarse pulverization step, which is not preferable in terms of toner production.

  Therefore, in the toner manufacturing method of the present invention, the pulverizer used in the coarse pulverization step is arranged on the same axis via a plurality of rotary impactors (hammers) for primary pulverization and baffle plates for controlling the powder flow. A rotor composed of a rotating body having at least a central rotating shaft for secondary crushing, and unevenness arranged around the rotor (rotor) while maintaining a certain distance from the rotor surface. It is more preferable to use a coarse pulverizer having two or more pulverization zones each having a stator and having a pulverization zone housed in one unit and operated at the same rotational speed by the same power source. preferable.

  Next, in the pulverization step, the pulverization is performed by the pulverizer of the present invention described above.

In the toner production method of the present invention, a mixture containing at least a binder resin and a colorant is melt-kneaded, the obtained kneaded product is cooled, the cooled product is coarsely pulverized, and the obtained coarsely pulverized product is pulverized. In the toner production method comprising at least a step of pulverizing by a means and classifying the obtained pulverized product by a classification means,
The pulverizer used in the pulverizing means is pulverized with at least a powder inlet 311 for charging an object to be pulverized into the pulverizing means, a stator 310, and a rotor 314 attached to the central rotating shaft 312. Powder discharge port 302 for discharging the powder from the crushing means, the stator 310 includes the rotor 314, and the surface of the stator 310 and the surface of the rotor surface 314 are The rotor 314 is arranged to have a predetermined gap to form a pulverization zone. In the pulverization zone, an object to be crushed is pulverized as the rotor 314 rotates, and the stator 310 and The rotor 314 has a plurality of convex portions and concave portions,
The unevenness is provided in parallel to the central rotation axis, and the rotor 314 includes a cooling coolant channel inside.
The temperature Trin (° C.) of the refrigerant flowing through the refrigerant flow path is −20.0 ≦ Trin ≦ 20.0.
It is characterized by being.

  If the temperature Trin (° C.) of the refrigerant flowing through the refrigerant flow path is Trin> 20.0, the temperature of the rotor 314 cannot be lowered, and the temperature rise in the grinding chamber accompanying high-speed rotation cannot be reduced, which is not preferable. .

  Further, if the temperature Trin (° C.) of the refrigerant flowing through the refrigerant flow path is set to Trin <−20.0, a high-spec refrigerant production apparatus is required, which is not preferable from the viewpoint of energy saving of the apparatus.

In the toner manufacturing method of the present invention, the relationship between the refrigerant temperature Trin (° C.) introduced into the refrigerant flow path and the refrigerant temperature Trout (° C.) discharged into the refrigerant flow path is 5.0 ≦ Trout−Trin. ≦ 25.0
It is preferable that

  The relationship between the refrigerant temperature Trin (° C.) introduced into the refrigerant flow path and the refrigerant temperature Trout (° C.) discharged outside the refrigerant flow path was received from the rotor 314 until the introduced refrigerant was discharged. It is considered that the change is due to the amount of heat. That is, if the relationship between the refrigerant temperature Trin (° C.) introduced into the refrigerant channel and the refrigerant temperature Trout (° C.) discharged outside the refrigerant channel is Trout−Trin> 25.0, the rotor 314 This indicates that excessive heat is applied, and the temperature of the rotor 314 itself cannot be lowered, which is not preferable.

  Further, since the rotor 314 rotates at a high speed, the temperature of the crushing chamber rises not a little. Therefore, in order for the relationship between the refrigerant temperature Trin (° C.) introduced into the refrigerant flow path and the refrigerant temperature Trout (° C.) discharged to the outside of the refrigerant flow path to be Trout−Trin <5, the rotor 314 internal It is necessary to flow a large amount of refrigerant into the apparatus or introduce an excessively cooled dehumidified gas into the apparatus, and as described above, a high-spec refrigerant production apparatus and a cold air apparatus are required. It is not preferable from the viewpoint of energy saving.

Further, according to the toner production method of the present invention, the pulverizer includes a cooling jacket 316 on the outer periphery of the stator, and the cooling refrigerant temperature Tjin (° C.) introduced into the jacket 316 is −10. .0 ≦ Tjin ≦ 10
It is preferable that

  If the cooling refrigerant temperature Tjin (° C.) introduced into the jacket 316 is Tjin> 10.0, the refrigerant temperature in the jacket 316 is too high to provide cooling ability, This is not preferable because the temperature rise cannot be prevented. Further, if Tjin <−10.0, the pulverized toner fine particles have an irregular shape and an angular shape, which is not preferable in terms of toner quality.

Furthermore, in the toner manufacturing method of the present invention, the relationship between the refrigerant temperature Tjin (° C.) introduced into the jacket 316 and the refrigerant temperature Tjout (° C.) discharged outside the jacket 316 is 1.0 ≦ Tjout−Tjn ≦ 10. .0
It is preferable that

  The relationship between the refrigerant temperature Tjin (° C.) introduced into the jacket 316 and the refrigerant temperature Tjout (° C.) discharged to the outside of the jacket 316 indicates that the refrigerant introduced into the jacket 316 is the high speed of the rotor 314. It is considered that the amount of heat received from the grinding chamber, the stator 310, or the like whose temperature has increased due to rotation is worthy.

  For this reason, if the relationship between the refrigerant temperature Tjin (° C.) introduced into the jacket 316 and the refrigerant temperature Tjout (° C.) discharged outside the jacket 316 is Tjout−Tjin> 10.0, This indicates that excessive heat is applied to the child 310, and an increase in the temperature of the grinding chamber cannot be prevented, which is not preferable.

  Further, as described above, since the rotor 314 rotates at a high speed, the temperature of the pulverization chamber rises not a little. For this reason, in order to make Tjout−Tjin <1.0, a large amount of refrigerant must flow inside the jacket 316 or a dehumidified gas that has been excessively cooled in the pulverizer must be introduced into the apparatus. As described above, a high-spec refrigerant manufacturing apparatus and a cold air apparatus are required, which is not preferable from the viewpoint of energy saving of the apparatus.

Furthermore, in the toner manufacturing method of the present invention, the flow rate Ar (m ³ / min) of the cooling refrigerant in the rotor 314 is 1.0 ≦ Ar ≦ 15.0.
It is preferable that 2.0 ≦ Ar ≦ 12.0.

When the flow rate Ar (m ³ / min) of the cooling refrigerant in the rotor 314 is Ar> 15.0, the main body vibration value in the high-speed rotation region of the rotor 314 is high, and the pulverizer is stably operated. There is a problem in that point, which is not preferable. Further, if the flow rate Ar (m ³ / min) of the cooling refrigerant in the rotor 314 is Ar <1.0, the temperature of the rotor 314 may not be lowered, and the grinding chamber accompanying high-speed rotation may not be achieved. It is not preferable because the temperature rise cannot be reduced.

Furthermore, in the method for producing a toner of the present invention, a dehumidified gas is introduced into the pulverizer together with the coarsely pulverized product, and a temperature Thin (° C.) of the introduced dehumidified gas is −10.0 ≦ Thin ≦ 40. 0
It is preferable that 10.0 ≦ Thin ≦ 30.0 is more preferable.

  By introducing a dehumidified gas into the pulverizer together with the coarsely pulverized product, dew condensation in the pulverizer is prevented. Further, if the temperature Thin (° C.) of the introduced dehumidifying gas is Thin> 40.0, the temperature of the pulverization chamber is increased, which may cause a decrease in cooling efficiency and in-machine fusion, which is not preferable. Further, if Thin <-10.0, the pulverized toner fine particles have an irregular shape and an angular shape, which is not preferable in terms of toner quality.

Further, in the toner production method of the present invention, the temperature Thout (° C.) of the dehumidified gas discharged to the outside of the pulverizer is 20.0 ≦ Thout <60.0.
It is characterized by being.

  If the temperature Thout (° C.) of the dehumidified gas discharged to the outside of the pulverizer is Thout ≧ 60.0, it indicates that the temperature of the pulverization chamber has risen, thus causing in-machine fusion. This is not preferable. Further, if Thout <20.0, the shape of the pulverized toner particles is indefinite and angular, which is not preferable in terms of toner quality.

  After pulverizing to a predetermined toner particle size in the pulverization step, toner particles are obtained through a classification step. For convenience, a surface modification step may be provided before and after the classification step to modify the surface of the toner particles.

  Further, toner is obtained by externally adding external additives such as inorganic fine particles to the obtained toner particles as necessary.

  The finely pulverized product obtained in the pulverization step is classified into toner particles having a desired particle size in the classification step. Examples of the classifier include a turboplex, a TSP separator, a TTSP separator (manufactured by Hosokawa Micron), and an elbow jet (manufactured by Nippon Steel Mining).

  Furthermore, if necessary, surface modification = spheronization treatment can be performed in the surface modification step to form surface modified particles. Examples of the surface reformer include a hybridization system (manufactured by Nara Machinery Co., Ltd.); Nobilta (manufactured by Hosokawa Micron Corporation) and the like.

  After surface modification, for example, Ultrasonic (manufactured by Sakae Sangyo Co., Ltd.); Resona sieve, gyro shifter (Tokuju Kogakusha Co., Ltd.); Turbo screener (manufactured by Turbo Kogyo Co., Ltd.) ); A sieving machine such as a high volter (manufactured by Toyo Hitec Co., Ltd.) may be used.

  A toner is obtained by externally adding external additives such as inorganic fine particles to the obtained toner particles as necessary.

  As a method of externally adding an external additive to toner particles, a predetermined amount of toner particles and various known external additives are blended, and sheared into a powder such as a Henschel mixer, Mechano Hybrid (Mitsui Mining Co., Ltd.); Stir and mix using a high-speed stirrer that provides force as an external additive.

  Next, a preferable toner configuration for achieving the object in the present invention will be described in detail below.

  Examples of the binder resin used in the present invention include vinyl resins, polyester resins, and epoxy resins. Of these, vinyl resins and polyester resins are more preferable in terms of chargeability and fixability. In particular, when a polyester resin is used, the effect of introducing this apparatus is great.

  In the present invention, vinyl monomer monopolymer or copolymer, polyester, polyurethane, epoxy resin, polyvinyl butyral, rosin, modified rosin, terpene resin, phenol resin, aliphatic or alicyclic hydrocarbon resin, aromatic Petroleum resin or the like can be mixed with the above-described binder resin as necessary.

  When two or more kinds of resins are mixed and used as a binder resin, it is preferable that those having different molecular weights are mixed in an appropriate ratio as a more preferable form.

  The glass transition temperature of the binder resin is preferably 45 to 80 ° C., more preferably 55 to 70 ° C., the number average molecular weight (Mn) is 2,500 to 50,000, and the weight average molecular weight (Mw) is 10,000. It is preferable to be 1,000,000.

  As the binder resin, the following polyester resins are also preferable. In the polyester resin, 45 to 55 mol% of all components is an alcohol component, and 55 to 45 mol% is an acid component.

  The acid value of the polyester resin is preferably 90 mgKOH / g or less, more preferably 50 mgKOH / g or less, and the OH value is preferably 50 mgKOH / g or less, more preferably 30 mgKOH / g or less. This is because as the number of terminal groups of the molecular chain increases, the dependency of the toner on the environment increases in the environment.

  The glass transition temperature of the polyester resin is preferably 50 to 75 ° C, more preferably 55 to 65 ° C. Further, the number average molecular weight (Mn) is preferably 1,500 to 50,000, more preferably 2,000 to 20,000, and the weight average molecular weight (Mw) is preferably 6,000 to 100,000, more preferably. Is preferably 10,000 to 90,000.

  When the toner of the present invention is used as a magnetic toner, the magnetic material contained in the magnetic toner includes iron oxides such as magnetite, maghemite and ferrite, and iron oxides including other metal oxides; Fe, Co, Ni, etc. Metals or alloys of these metals with metals such as Al, Co, Cu, Pb, Mg, Ni, Sn, Zn, Sb, Be, Bi, Cd, Ca, Mn, Se, Ti, W, V , And mixtures thereof.

Specifically, examples of magnetic materials include triiron tetroxide (Fe ₃ O ₄ ), iron sesquioxide (γ-Fe ₂ O ₃ ), iron oxide zinc (ZnFe ₂ O ₄ ), and iron yttrium oxide (Y ₃ Fe). ₅ O ₁₂ ), iron cadmium oxide (CdFe ₂ O ₄ ), iron gadolinium oxide (Gd ₃ Fe ₅ O ₁₂ ), copper iron oxide (CuFe ₂ O ₄ ), lead iron oxide (PbFe ₁₂ O ₁₉ ),
Nickel iron oxide (NiFe ₂ O ₄ ), neodymium iron oxide (NdFe ₂ O ₃ ), barium iron oxide (BaFe ₁₂ O ₁₉ ), magnesium iron oxide (MgFe ₂ O ₄ ), manganese iron oxide (MnFe ₂ O ₄ ), Examples include iron lanthanum oxide (LaFeO ₃ ), iron powder (Fe), cobalt powder (Co), and nickel powder (Ni).

  The magnetic materials described above are used alone or in combination of two or more. A particularly suitable magnetic material is a fine powder of iron tetroxide or γ-iron sesquioxide.

  These may be used in an amount of 20 to 150 parts by mass, preferably 50 to 130 parts by mass, and more preferably 60 to 120 parts by mass with respect to 100 parts by mass of the binder resin.

  Non-magnetic colorants that can be used in the toner of the present invention include any suitable pigment or dye.

  Examples of the pigment include carbon black, aniline black, acetylene black, naphthol yellow, hansa yellow, rhodamine lake, alizarin lake, bengara, phthalocyanine blue, and indanthrene blue.

  These are added in an amount of 0.1 to 20 parts by weight, preferably 1 to 10 parts by weight, based on 100 parts by weight of the binder resin. Similarly, dyes are used, for example, anthraquinone dyes, xanthene dyes, methine dyes, and 0.1 to 20 parts by weight, preferably 0.3 to 10 parts by weight with respect to 100 parts by weight of the binder resin. The addition amount of is good.

  In the toner of the present invention, a charge control agent can be used as necessary in order to further stabilize the chargeability. The charge control agent is preferably used in an amount of 0.5 to 10 parts by mass per 100 parts by mass of the binder resin.

  When the amount is less than 0.5 parts by mass, sufficient charging characteristics may not be obtained, which is not preferable. When the amount exceeds 10 parts by mass, compatibility with other materials is deteriorated or charging is performed under low humidity. It may be excessive, which is not preferable.

  Examples of the charge control agent include the following.

  As a negative charge control agent for controlling the toner to be negative charge, for example, an organometallic complex or a chelate compound is effective. Examples include monoazo metal complexes, aromatic hydroxycarboxylic acid metal complexes, and aromatic dicarboxylic acid metal complexes. Others include aromatic hydroxycarboxylic acids, aromatic mono- and polycarboxylic acids and their metal salts, anhydrides, or esters thereof, or phenol derivatives of bisphenol.

Examples of the positive charge control agent for controlling the toner to be positively charged include modified products such as nigrosine and fatty acid metal salts, tributylbenzylammonium-1-hydroxy-4-naphthosulfonate, tetrabutylammonium tetrafluoroborate and the like. As onium salts such as quaternary ammonium salts and their analogs such as phosphonium salts and their chelating pigments, triphenylmethane dyes and their lake pigments (as rake agents are phosphotungstic acid, phosphomolybdic acid, phosphotungsten) Molybdic acid, tannic acid, lauric acid, gallic acid, ferricyanic acid, ferrocyanic compound, etc.),
Examples of the higher fatty acid metal salt include diorganotin oxides such as dibutyltin oxide, dioctyltin oxide, and dicyclohexyltin oxide, and diorganotin borates such as dibutyltin borate, dioctyltin borate, and dicyclohexyltin borate.

  In the present invention, if necessary, one or more release agents may be contained in the toner particles. Examples of the release agent include the following.

That is, aliphatic hydrocarbon waxes such as low molecular weight polyethylene, low molecular weight polypropylene, microcrystalline wax, and paraffin wax, and oxides of aliphatic hydrocarbon waxes such as oxidized polyethylene wax, or block copolymers thereof. ;
And waxes mainly composed of fatty acid esters such as carnauba wax, sazol wax, and montanic acid ester wax; and those obtained by partially or fully deoxidizing fatty acid esters such as deoxidized carnauba wax.

Furthermore, saturated linear fatty acids such as palmitic acid, stearic acid, and montanic acid; unsaturated fatty acids such as brassic acid, eleostearic acid, and valinal acid;
Saturated alcohols such as stearyl alcohol, aralkyl alcohol, behenyl alcohol, carnauvir alcohol, seryl alcohol, melyl alcohol; long-chain alkyl alcohols; polyhydric alcohols such as sorbitol;
Fatty acid amides such as linoleic acid amide, oleic acid amide, lauric acid amide; saturated fatty acid bisamides such as methylene bisstearic acid amide, ethylene biscapric acid amide, ethylene bislauric acid amide, hexamethylene bisstearic acid amide;
Unsaturated fatty acid amides such as ethylene bisoleic acid amide, hexamethylene bisoleic acid amide, N, N′-dioleyl adipic acid amide, N, N-dioleyl sebacic acid amide; m-xylene bisstearic acid amide, N , N-distearyl isophthalic acid amides and other aromatic bisamides;
Fatty acid metal salts such as calcium stearate, calcium laurate, zinc stearate, magnesium stearate (generally referred to as metal soap), and aliphatic hydrocarbon waxes using vinyl monomers such as styrene and acrylic acid Grafted waxes;
Moreover, the partial esterification thing of fatty acids, such as behenic acid monoglyceride, and a polyhydric alcohol, the methyl ester compound which has a hydroxyl group obtained by hydrogenation etc. of vegetable oils, etc. are mentioned.

  The amount of the release agent is 0.1 to 20 parts by mass, preferably 0.5 to 10 parts by mass, per 100 parts by mass of the binder resin.

  In the present invention, the melting point defined by the maximum endothermic peak temperature at the time of temperature rise measured by a differential scanning calorimeter (DSC) of the release agent is 60 to 130 ° C. (more preferably 80 to 125 ° C. ) Is preferable. When the melting point is less than 60 ° C, the viscosity of the toner is lowered and toner adhesion to the photoreceptor is likely to occur. When the melting point is more than 130 ° C, the low-temperature fixability may be deteriorated, which is not preferable. .

  In the toner of the present invention, a fine powder that can be increased by adding the toner particles externally before and after the addition may be used as a fluidity improver.

  For example, fluorine resin powders such as vinylidene fluoride fine powder and polytetrafluoroethylene fine powder; wet production silica, fine powder silica such as dry production silica, fine powder titanium oxide, fine powder alumina, etc., silane coupling agent, titanium A surface treatment is performed with a coupling agent and silicone oil, and the surface is hydrophobized. Those treated so that the degree of hydrophobicity measured by the methanol titration test shows a value in the range of 30 to 80 are particularly preferred.

A fluidizing agent having a specific surface area by nitrogen adsorption measured by the BET method of 30 m ² / g or more, preferably 50 m ² / g or more gives good results.

  In addition to the polishing effect, the toner of the present invention may contain inorganic fine powders other than those described above as chargeability and fluidity imparting and cleaning aids. By adding the inorganic fine powder externally to the toner particles, the effect can be increased more than before and after the addition.

  Examples of the inorganic fine powder used in the present invention include titanates and / or silicates such as magnesium, zinc, cobalt, manganese, strontium, cerium, calcium, and barium.

  The inorganic fine particles in the present invention are used in an amount of 0.1 to 10 parts by weight, preferably 0.2 to 8 parts by weight, based on 100 parts by weight of the toner.

  Next, a method for measuring various physical property data measured in the following examples will be described below.

<Measurement method of weight average particle diameter (D4)>
The weight average particle diameter (D4) of the toner is determined based on the precise particle size distribution measuring apparatus “Coulter Counter Multisizer 3” (registered trademark, manufactured by Beckman Coulter, Inc.) having a 100 μm aperture tube. Using the attached dedicated software “Beckman Coulter Multisizer 3 Version 3.51” (manufactured by Beckman Coulter, Inc.) for setting and analyzing the measurement data, the measurement data is measured with 25,000 effective channels. Analysis was performed and calculated.

  As the electrolytic aqueous solution used for the measurement, special grade sodium chloride is dissolved in ion-exchanged water so as to have a concentration of about 1% by mass, for example, “ISOTON II” (manufactured by Beckman Coulter, Inc.) can be used.

  Prior to measurement and analysis, dedicated software was set up as follows.

  In the “Standard Measurement Method (SOM) Change Screen” of the dedicated software, set the total count in the control mode to 50000 particles, set the number of measurements once, and set the Kd value to “standard particles 10.0 μm” (Beckman Coulter, Inc.) Set the value obtained using The threshold and noise level are automatically set by pressing the threshold / noise level measurement button. Also, the current is set to 1600 μA, the gain is set to 2, the electrolyte is set to ISOTON II, and the aperture tube flash after measurement is checked.

  In the “pulse to particle size conversion setting screen” of the dedicated software, the bin interval is set to logarithmic particle size, the particle size bin is set to 256 particle size bin, and the particle size range is set to 2 μm to 60 μm.

The specific measurement method is as follows.
(1) About 200 ml of the electrolytic solution is placed in a glass 250 ml round bottom beaker exclusively for Multisizer 3, set on a sample stand, and the stirrer rod is stirred counterclockwise at 24 rpm. Then, dirt and bubbles in the aperture tube are removed by the “aperture flush” function of the analysis software.
(2) About 30 ml of the electrolytic aqueous solution is put in a glass 100 ml flat bottom beaker, and "Contaminone N" (nonionic surfactant, anionic surfactant, organic builder pH 7 precision measurement is used as a dispersant therein. About 0.3 ml of a diluted solution obtained by diluting a 10% by weight aqueous solution of a neutral detergent for washing a vessel (made by Wako Pure Chemical Industries, Ltd.) 3 times with ion exchange water is added.
(3) Two oscillators with an oscillation frequency of 50 kHz are incorporated in a state where the phase is shifted by 180 degrees, and placed in a water tank of an ultrasonic dispersion device “Ultrasonic Dissipation System Tetora 150” (manufactured by Nikki Bios Co., Ltd.) having an electrical output of 120 W. A fixed amount of ion-exchanged water is added, and about 2 ml of the above-mentioned Contaminone N is added to this water tank.
(4) The beaker of (2) is set in the beaker fixing hole of the ultrasonic disperser, and the ultrasonic disperser is operated. And the height position of a beaker is adjusted so that the resonance state of the liquid level of the electrolyte solution in a beaker may become the maximum.
(5) In a state where the electrolytic aqueous solution in the beaker of (4) is irradiated with ultrasonic waves, about 10 mg of toner is added to the electrolytic aqueous solution little by little and dispersed. Then, the ultrasonic dispersion process is continued for another 60 seconds. In the ultrasonic dispersion, the temperature of the water tank is appropriately adjusted so as to be 10 ° C. or higher and 40 ° C. or lower.
(6) To the round bottom beaker of (1) installed in the sample stand, the electrolyte solution of (5) in which the toner is dispersed is dropped using a pipette, and the measurement concentration is adjusted to about 5%. . The measurement is performed until the number of measured particles reaches 50,000.
(7) The measurement data is analyzed with the dedicated software attached to the apparatus, and the weight average particle diameter (D4) is calculated. The “average diameter” on the analysis / volume statistics (arithmetic average) screen when the graph / volume% is set with the dedicated software is the weight average particle diameter (D4).

<Calculation method of fine powder amount>
The number-based fine powder amount (number%) in the toner is calculated as follows.

  For example, the number% of particles having a particle size of 4.0 μm or less in the toner is measured by the above-mentioned Multisizer 3, and (1) graph / number% is set with dedicated software, and the measurement result chart is displayed in number%. (2) Check “<” in the particle size setting portion on the format / particle size / particle size statistics screen, and enter “4” in the particle size input section below. Then, (3) when the analysis / count statistics (arithmetic mean) screen is displayed, the numerical value of the “<4 μm” display portion is the number% of particles of 4.0 μm or less in the toner.

<Measurement of melting point of wax>
Measurement is performed using a differential thermal analysis measuring device (DSC measuring device), DSC-7 (manufactured by Perkin Elmer). The measurement is performed according to ASTM D3418-82. Precisely weigh 2 to 10 mg of the measurement sample and place it in an aluminum pan. Using an empty aluminum pan as a reference, measure it at a temperature rise rate of 10 ° C / min and normal temperature and humidity at a measurement temperature range of 30 to 200 ° C. I do.

  In this temperature raising process, an endothermic peak of a main peak in a temperature range of 30 to 200 ° C. is obtained. The temperature of this endothermic main peak is taken as the melting point of the wax.

<Measurement of glass transition temperature (Tg)>
It measures according to ASTM D3418-82 using a differential scanning calorimeter (DSC measuring device) and DSC-7 (manufactured by Perkin Elmer).

  The sample to be measured is precisely weighed from 5 to 20 mg, preferably 10 mg.

  This is put into an aluminum pan, and an empty aluminum pan is used as a reference, and measurement is performed at a temperature rise rate of 10 ° C./min at a temperature rise rate of 10 ° C./min.

  In this temperature raising process, an endothermic peak of a main peak in a temperature range of 40 to 100 ° C. is obtained.

  At this time, the point of intersection between the base line midpoint before and after the endothermic peak and the differential heat curve is defined as the glass transition temperature Tg in the present invention.

<Measurement of molecular weight distribution of binder resin>
The molecular weight of the chromatogram by GPC is measured under the following conditions.

  The column is stabilized in a heat chamber at 40 ° C., and tetrahydrofuran (THF) as a solvent is allowed to flow through the column at this temperature at a flow rate of 1 ml / min. The sample is dissolved in THF, filtered through a 0.2 μm filter, and the filtrate is used as a sample. Measurement is performed by injecting 50 to 200 μl of a THF sample solution of a resin adjusted to a sample concentration of 0.05 to 0.6 mass%.

  In measuring the molecular weight of a sample, the molecular weight distribution of the sample is calculated from the relationship between the logarithmic value of a calibration curve prepared from several types of monodisperse polystyrene standard samples and the number of counts.

As a standard polystyrene sample for preparing a calibration curve, for example, Pressure Chemical Co. Manufactured by Toyo Soda Kogyo Co., Ltd. and having molecular weights of 6 × 10 ² , 2.1 × 10 ³ , 4 × 10 ³ , 1.75 × 10 ⁴ , 5.1 × 10 ⁴ , 1.1 × 10 ⁵ , 3 .9 × 10 ⁵ , 8.6 × 10 ⁵ , 2 × 10 ⁶ , 4.48 × 10 ⁶ are used, and it is appropriate to use at least about 10 standard polystyrene samples. An RI (refractive index) detector is used as the detector.

As a column, in order to accurately measure a molecular weight region of 10 ^{3 to} 2 × 10 ⁶ , it is preferable to combine a plurality of commercially available polystyrene gel columns. For example, a combination of μ-styragels 500, 10 ³ , 10 ⁴ , and 10 ⁵ manufactured by Waters and a combination of shodex KA-801, 802, 803, 804, 805, 806, and 807 manufactured by Showa Denko are preferable.

<Measurement of acid value of resin>
The “acid value” of the binder resin is determined as follows. Basic operation conforms to JIS-K0070.

  The number of mg of potassium hydroxide required to neutralize free fatty acids, resin acids, etc. contained in 1 g of the sample is called the acid value, and the test is conducted as follows.

(1) Reagent (a) Solvent ethyl ether-ethyl alcohol mixed solution (1 + 1 or 2 + 1) or benzene-ethyl alcohol mixed solution (1 + 1 or 2 + 1), these solutions were subjected to N / 10 hydroxylation using phenolphthalein as an indicator immediately before use. Neutralize with potassium ethyl alcohol solution.
(B) Phenolphthalein solution 1 g of phenolphthalein is dissolved in 100 ml of ethyl alcohol (95 v / v%).
(C) N / 10 potassium hydroxide-ethyl alcohol solution Dissolve 7.0 g of potassium hydroxide in as little water as possible, add ethyl alcohol (95 v / v%) to 1 liter, leave it for 2 to 3 days, and filter. The standardization is performed according to JIS K 8006 (basic matters concerning titration during the reagent content test).

  (2) Operation Weigh correctly 1 to 20 g of sample, add 100 ml of solvent and a few drops of phenolphthalein solution as an indicator, and shake well until the sample is completely dissolved. In the case of a solid sample, dissolve it by heating on a water bath. After cooling, this is titrated with an N / 10 potassium hydroxide ethyl alcohol solution, and the end point of neutralization is defined as the time when the indicator is slightly red for 30 seconds.

  (3) Calculation formula The acid value is calculated by the following formula.

［Ａ：酸価
Ｂ：Ｎ／１０水酸化カリウムエチルアルコール溶液の使用量（ｍｌ）
ｆ：Ｎ／１０水酸化カリウムエチルアルコール溶液のファクター
Ｓ：試料（ｇ）］

[A: acid value B: amount of N / 10 potassium hydroxide ethyl alcohol solution used (ml)
f: Factor of N / 10 potassium hydroxide ethyl alcohol solution S: Sample (g)]

<Measurement of hydroxyl value of binder resin>
The “hydroxyl value” of the binder resin is determined as follows. The basic operation conforms to JIS = K0070.

  When 1 g of a sample is acetylated by a prescribed method, the number of mg of potassium hydroxide required to neutralize acetic acid bonded to a hydroxyl group is referred to as a hydroxyl value, and the test is performed by the following reagents, operations and calculation formulas.

(1) Reagent (a) Acetylation reagent 25 g of acetic anhydride is placed in a 100 ml volumetric flask, pyridine is added to make a total volume of 100 ml, and shaken sufficiently (in some cases, pyridine may be added). The acetylating reagent should be kept away from moisture, carbon dioxide and acid vapors and stored in a brown bottle.
(B) Phenolphthalein solution 1 g of phenolphthalein is dissolved in 100 ml of ethyl alcohol (95 v / v%).
(C) N / 2 potassium hydroxide-ethyl alcohol solution Dissolve 35 g of potassium hydroxide in as little water as possible, add ethyl alcohol (95 v / v%) to 1 liter, leave it for 2 to 3 days, and filter. The orientation is performed according to JIS K 8006.

(2) Operation 0.5 to 2.0 g of a sample is correctly weighed in a round bottom flask, and 5 ml of an acetylating reagent is correctly added thereto. A small funnel is put on the mouth of the flask, and the bottom is immersed in a glycerin bath at 95 to 100 ° C. to heat the bottom. At this time, in order to prevent the temperature of the neck of the flask from rising due to the heat of the bath, a cardboard disc with a round hole in it is put on the base of the neck of the flask.

  After 1 hour, the flask is removed from the bath, and after cooling, 1 ml of water is added from the funnel and shaken to decompose acetic anhydride. In order to further complete the decomposition, the flask was again heated in a glycerin bath for 10 minutes, allowed to cool, and then the funnel and the wall of the flask were washed with 5 ml of ethyl alcohol, and N / 2 potassium hydroxide ethyl alcohol using a phenolphthalein solution as an indicator. Titrate with solution.

  A blank test is performed in parallel with this test. In some cases, a KOH-THF solution may be used as an indicator.

  (3) Calculation formula The hydroxyl value is calculated by the following formula.

［Ａ：水酸基価
Ｂ：空試験のＮ／２水酸化カリウムエチルアルコール溶液の使用量（ｍｌ）
Ｃ：本試験のＮ／２水酸化カリウムエチルアルコール溶液の使用量（ｍｌ）
ｆ：Ｎ／２水酸化カリウムエチルアルコール溶液のファクター
Ｓ：試料（ｇ）
Ｄ：酸価］

[A: Hydroxyl value B: Amount used of N / 2 potassium hydroxide ethyl alcohol solution in blank test (ml)
C: Amount of use of N / 2 potassium hydroxide ethyl alcohol solution in this test (ml)
f: Factor of N / 2 potassium hydroxide ethyl alcohol solution S: Sample (g)
D: Acid value]

<Measurement of specific surface area BET of toner>
The BET specific surface area is measured using a specific surface area measuring device Tristar 3000 (manufactured by Shimadzu Corporation).

  The specific surface area of the toner is calculated by adsorbing nitrogen gas on the sample surface according to the BET method and using the BET multipoint method. Prior to the measurement of the specific surface area, about 2 g of the sample is precisely weighed in a sample tube and evacuated at room temperature for 24 hours. After evacuation, the mass of the entire sample cell is measured, and the exact mass of the sample is calculated from the difference from the empty sample cell.

  An empty sample cell is set in the balance port and analysis port of the BET measuring device. Next, a Dewar bottle containing liquid nitrogen is set at a predetermined position, and P0 is measured by a saturated vapor pressure (P0) measurement command. After the P0 measurement is completed, the prepared sample cell is set in the analysis port, the sample mass and P0 are input, and the measurement is started by the BET measurement command. After that, the BET specific surface area is automatically calculated.

<Measurement of the number of coarse particles in the toner>
In the present invention, the number (j) of coarse particles was measured as follows. By suctioning 0.5 g of toner particles with a vacuum cleaner, the toner particles are passed through a metal mesh (400 mesh) having a diameter of 10 mm. At this time, the toner particles remaining on the mesh are made coarse particles, which are taped, and those pasted on the paper are enlarged with a KEYENCE microscope, and the number of coarse particles (j) is counted.

  EXAMPLES Hereinafter, although an Example demonstrates this invention, this invention is not limited to these Examples.

(Example of toner production)
Binder resin (polyester resin): 100 parts by mass (Tg 60 ° C., acid value 19.5 mgKOH / g, hydroxyl value 24.8 mgKOH / g, molecular weight: Mp7200, Mn2900, Mw56500)
- iron oxide particles: 90 parts by weight (average particle size 0.18 .mu.m, characteristics in 795.8 kA / m magnetic field ^{Hc11.2kA / m, σs83.6Am 2 /kg,σr13.2Am 2} / kg)
・ Azo-based iron complex compound: 2 parts by mass (made by Hodogaya Chemical Co., Ltd., trade name T-77)
Fischer-Tropsch wax: 3 parts by mass (manufactured by Nippon Seiwa Co., Ltd., trade name: FT-100, melting point: 98 ° C.)
The materials having the above formulation were thoroughly mixed with a Henschel mixer and then kneaded with a twin-screw kneader set at a temperature of 130 ° C. The obtained kneaded product was cooled and coarsely pulverized with a coarse pulverizer to obtain a coarsely pulverized product.

  In the present example, the obtained coarsely pulverized product was pulverized using a pulverizer equipped with the rotor 314 shown in FIG. 3 and pulverized under the following conditions.

  As shown in Table 1, the rotor 314 shown in FIG. 3 had an outer diameter of 750 mm and a total length of 440 mm. Note that the number of stages of the disk 322 is two.

  The surface of the rotor 314 and the surface of the stator 310 have a plurality of corrugated convex portions and concave portions, and the interdental distance formed by the concave and convex portions is 3 m. In addition, the distance between the rotor 314 and the stator 310 shown in FIG.

Further, as shown in FIG. 3, the rotor 314 includes a cooling coolant channel N inside, and the coolant channel N has a cooling hole H in its shape. Furthermore, the outer diameter of the cooling hole H was 10 mm, and the cross-sectional area D of the cooling hole was 79 mm ² .

  The number of cooling holes was 75, and the total length of the refrigerant flow path N was 360 mm. Further, the cooling holes were arranged in a line at equal intervals. Further, the number of the refrigerant channels M and P is four, and the number of systems is two systems according to the number of stages of the disk 322.

  Furthermore, Dpr, which is the distance from the rotor 314 center point P shown in FIG. 2 to the bottom surface r of the concave surface of the rotor 314 surface, is 373 mm, and from the rotor 314 center point P, Dpq, which is the distance to the outer shell q, was 357 mm.

  Therefore, Dpr-Dpq in this example was 16 mm.

Further, as the pulverization conditions, the flow rate of the suction blower was set to 25 m ³ / min, and the supply amount of the material to be pulverized from the quantitative supply unit 315 was set to 270 kg / hr.

Further, the refrigerant temperature Tjin (° C.) introduced into the jacket 316 and the refrigerant temperature Tri (° C.) introduced into the refrigerant flow path L are the refrigerant flow rate passing through the jacket 316 and the refrigerant flow rate Ar (m) passing through the refrigerant flow path L. ³ / min), the temperature of the introduced dehumidified gas was changed by the dehumidified gas generating means 319. The dehumidified gas temperature mentioned above indicates the temperature inside the powder inlet 311 shown in FIG. 6, and the discharge temperature of the dehumidified gas is the temperature in the pulverization chamber during pulverization, which is also the powder outlet shown in FIG. The mouth temperature of 302 is shown.

  After the material to be pulverized was pulverized using the pulverizer configuration and pulverization conditions described above, the pulverization state of the pulverizer and the toner quality were evaluated by the following items.

(Evaluation-1: Body vibration value evaluation)
The vibration value (S-0) of the rotor 314 at a rotational peripheral speed of 10 m / sec is measured. Next, each vibration value (S-1) is measured at rotational peripheral speeds of 50 m / sec, 100 m / sec, and 150 m / sec. The vibration difference between S-1 and S-0 at each rotational peripheral speed was confirmed and evaluated according to the following criteria.
A: Less than 25 μm B: 25 μm or more and less than 50 μm C: 50 μm or more and less than 75 μm D: 75 μm or more and less than 100 μm E: 100 μm or more

  The vibration measurement was performed using a porter vibro (model VM-3004SI) manufactured by IMV.

(Evaluation-2: Evaluation for toner particle size)
The desired weight average diameter (D4) of the pulverized product was set to 5.5 ± 0.2 μm, and the number% of particles of 4.0 μm or less in the toner was evaluated according to the following criteria.
A: Less than 55% by number B: 55% to less than 60% C: 60% to less than 65% D: 65% to less than 70% E: 70% or more

(Evaluation-3: Evaluation for coarse particles of toner)
The number (j) of coarse particles of the obtained pulverized product was measured and judged according to the following criteria.
A: 0 ≦ j <50
B: 50 ≦ j <100
C: 100 ≦ j <150
D: 150 ≦ j <200
E: 200 ≦ j

(Evaluation-4: Measurement of specific surface area of toner particles)
The obtained pulverized product is classified by a multi-division classifier using the Coanda effect so that the number% of particles of 4.0 μm or less in the toner is 25% by number or more and less than 32% by number. The BET specific surface area (BET) was measured and evaluated according to the following criteria.
A: BET ≦ 1.05
B: 1.05 <BET ≦ 1.10
C: 1.10 <BET ≦ 1.15
D: 1.15 <BET ≦ 1.20
E: BET> 1.20

<Example 1>
In this embodiment, the temperature of the refrigerant introduced into the rotor 314 is −10 ° C., and the flow rate of the refrigerant is 10 m ³ / min. And the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was adjusted to 15 ° C. Further, the temperature of the refrigerant introduced into the jacket 316 was set to 0 ° C., and the flow rate was adjusted to adjust the difference between the discharged refrigerant temperature and the introduced refrigerant temperature to 5 ° C. Furthermore, the temperature of the dehumidifying gas introduced into the pulverizer was adjusted to 20 ° C., and the discharge temperature was adjusted to 40 ° C. At this time, the main body vibration value evaluation was A.

  When the obtained coarsely crushed material was pulverized, toner particles having a weight average diameter (D4) of 5.5 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle size of 4.0 μm or less in the toner were obtained. The number% of the particles was 54 number%. The number of coarse particles was 32.

  Further, after the obtained pulverized product was classified, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.04. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 2>
In this embodiment, the temperature of the refrigerant introduced into the rotor 314 is −20 ° C., and the flow rate of the refrigerant is 8 m ³ / min. The conditions were adjusted in the same manner as in Example 1 except that the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was adjusted to 15 ° C. The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely crushed material was pulverized, toner particles having a weight average diameter (D4) of 5.4 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle diameter of 4.0 μm or less in the toner were obtained. The number% of the particles was 57 number%. The number of coarse particles was 25.

  Further, after the obtained pulverized product was classified, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.08. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 3>
In this embodiment, the refrigerant temperature introduced into the rotor 314 is 20 ° C., and the refrigerant flow rate is 12 m ³ / min. The conditions were adjusted in the same manner as in Example 1 except that the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was adjusted to 15 ° C. The evaluation of the main body vibration value at this time was A.

  When the resulting coarsely pulverized product was pulverized, toner particles having a weight average diameter (D4) of 5.6 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec. The number% of the particles was 54 number%. The number of coarse particles was 56.

  Further, after the obtained pulverized product was classified, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.02. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 4>
In this embodiment, the temperature of the refrigerant introduced into the rotor 314 is −10 ° C., and the flow rate of the refrigerant is 15 m ³ / min. The conditions were adjusted in the same manner as in Example 1 except that the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was adjusted to 5 ° C. The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely pulverized product was pulverized, toner particles having a weight average diameter (D4) of 5.3 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle size of 4.0 μm or less in the toner were obtained. The number% of particles was 59 number%. The number of coarse particles was 43.

  Further, after classifying the obtained pulverized product, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.09. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 5>
In this embodiment, the temperature of the refrigerant introduced into the rotor 314 is −10 ° C., and the flow rate of the refrigerant is 5 m ³ / min. The conditions were adjusted in the same manner as in Example 1 except that the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was 25 ° C. The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely crushed material was pulverized, toner particles having a weight average diameter (D4) of 5.7 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle diameter of 4.0 μm or less in the toner were obtained. The number% of particles was 59 number%. The number of coarse particles was 64.

  Further, after classifying the obtained pulverized product, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.03. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 6>
In this embodiment, the temperature of the refrigerant introduced into the rotor 314 is −20 ° C., and the flow rate of the refrigerant is 1 m ³ / min. The conditions were adjusted in the same manner as in Example 1 except that the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was adjusted to 20 ° C. The evaluation of the vibration value of the main body at this time is as follows. Became B.

  When the obtained coarsely crushed material was pulverized, toner particles having a weight average diameter (D4) of 5.4 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle diameter of 4.0 μm or less in the toner were obtained. The number% of the particles was 55 number%. The number of coarse particles was 114.

  Further, after classifying the obtained pulverized product, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.12. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 7>
In this example, the conditions were adjusted in the same manner as in Example 1 except that the refrigerant temperature introduced into the jacket 316 was −10 ° C. and the refrigerant flow rate was adjusted so that the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was 5 ° C. . The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely crushed material was pulverized, toner particles having a weight average diameter (D4) of 5.5 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle size of 4.0 μm or less in the toner were obtained. The number% of particles was 52 number%. The number of coarse particles was 38.

  Furthermore, after the obtained pulverized product was classified, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.05. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 8>
In this example, the conditions were adjusted in the same manner as in Example 1 except that the temperature of the refrigerant introduced into the jacket 316 was 10 ° C. and the refrigerant flow rate was adjusted so that the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was 5 ° C. The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely crushed material was pulverized, toner particles having a weight average diameter (D4) of 5.7 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle diameter of 4.0 μm or less in the toner were obtained. The number% of particles was 52 number%. The number of coarse particles was 128.

  Further, after classifying the obtained pulverized product, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.14. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 9>
In this example, the conditions were adjusted in the same manner as in Example 1 except that the temperature of the refrigerant introduced into the jacket 316 was 0 ° C. and the refrigerant flow rate was adjusted so that the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was 1 ° C. The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely crushed material was pulverized, toner particles having a weight average diameter (D4) of 5.5 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle size of 4.0 μm or less in the toner were obtained. The number% of particles was 53% by number. The number of coarse particles was 39.

  Further, after the obtained pulverized product was classified, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.06. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 10>
In this example, the conditions were adjusted in the same manner as in Example 1 except that the temperature of the refrigerant introduced into the jacket 316 was 0 ° C. and the refrigerant flow rate was adjusted so that the difference between the discharged refrigerant temperature and the introduced refrigerant temperature was 10 ° C. The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely crushed material was pulverized, toner particles having a weight average diameter (D4) of 5.7 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle diameter of 4.0 μm or less in the toner were obtained. The number% of the particles was 54 number%. The number of coarse particles was 107.

  Further, after the obtained pulverized product was classified, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.13. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 11>
In this example, conditions were adjusted in the same manner as in Example 1 except that the temperature of the dehumidified gas introduced into the pulverizer was set to -10 ° C. The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely pulverized product was pulverized, toner particles having a weight average diameter (D4) of 5.3 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle size of 4.0 μm or less in the toner were obtained. The number% of particles was 58 number%. The number of coarse particles was 31.

  Further, after the obtained pulverized product was classified, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.06. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 12>
In this example, the conditions were adjusted in the same manner as in Example 1 except that the temperature of the dehumidifying gas introduced into the pulverizer was 40 ° C. and the discharge temperature of the dehumidifying gas was 55 ° C. The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely crushed material was pulverized, toner particles having a weight average diameter (D4) of 5.7 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle diameter of 4.0 μm or less in the toner were obtained. The number% of the particles was 55 number%. The number of coarse particles was 143.

  Further, after classifying the obtained pulverized product, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.15. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 13>
In this example, conditions were adjusted in the same manner as in Example 1 except that the temperature of the dehumidified gas introduced into the pulverizer was 0 ° C. and the discharge temperature of the dehumidified gas was 20 ° C. The evaluation of the main body vibration value at this time was A.

  When the obtained coarsely pulverized product was pulverized, toner particles having a weight average diameter (D4) of 5.3 μm were obtained by setting the rotational peripheral speed of the rotor 314 to 150 m / sec, and the toner particles having a particle size of 4.0 μm or less in the toner were obtained. The number% of the particles was 57 number%. The number of coarse particles was 42.

  Further, after the obtained pulverized product was classified, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.13. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 14>
In this example, the rotor 314 shown in FIG. 3 was modified as follows.
-Distance Dpr = 373 mm from rotor 314 center point P to rotor 314 surface recess bottom surface r
The distance Dpq = 348 mm from the center point P of the rotor 314 to the outermost shell q of the refrigerant flow path N
Therefore, Dpr-Dpq = 25mm
When the pulverized material was pulverized under the same pulverization conditions as in the above-described pulverizer configuration and Example 1, the obtained coarsely pulverized material was pulverized. Toner particles having D4) of 5.7 μm were obtained, and the number% of particles of 4.0 μm or less in the toner was 56 number%. The number of coarse particles was 37.

  Further, after classifying the obtained pulverized product, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.03. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Example 15>
In this example, the rotor 314 shown in FIG. 3 was modified as follows.
-Distance Dpr = 373 mm from rotor 314 center point P to rotor 314 surface recess bottom surface r
The distance Dpq = 370 mm from the center point P of the rotor 314 to the outermost shell q of the refrigerant flow path N
Therefore, Dpr-Dpq = 3mm
When the pulverized material was pulverized under the same pulverization conditions as in the above-described pulverizer configuration and Example 1, the obtained coarsely pulverized material was pulverized. Toner particles having a D4) of 5.5 μm were obtained, and the number% of particles of 4.0 μm or less in the toner was 58 number%. The number of coarse particles was 92.

  Further, after classifying the obtained pulverized product, the BET specific surface area (BET) of the toner was measured. The BET specific surface area of the toner was 1.10. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Comparative Example 1>
The coarsely pulverized product obtained in Example 1 was pulverized in the same manner as in Example 1.

  At that time, in this comparative example, the coolant was not passed through the coolant channel L shown in FIG.

  The material to be crushed was pulverized under the same pulverization conditions as in Example 1 and Example 1, and the pulverization state of the pulverizer was evaluated in the same manner as in Example 1.

  In this comparative example, as in the example, an attempt was made to confirm the rotational peripheral speed at which the desired weight average diameter of the pulverized product was obtained.

  As a result, since the peripheral speed of the rotor 314 exceeded 125 m / sec, the pulverization chamber temperature rose and there was a risk of fusion, so the pulverization was stopped. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

<Comparative example 2>
The coarsely pulverized product obtained in Example 1 was pulverized using the pulverizer shown in FIG. In this comparative example, pulverization was performed using the rotor 614 and the stator 610 shown in FIG. 5, and pulverization was performed under the following conditions.

  The rotor 614 shown in FIG. 4 has an outer diameter of 750 mm and a total length of 600 mm. The number of stages of the disk 322 is five.

  Further, grinding was performed using the rotor 614 and the stator 610 shown in FIG. 5, and the distance between the rotor 614 and the stator 610 was set to 1 mm.

  Further, the rotor 614 shown in FIG. 4 forms a refrigerant shielding portion along the outer peripheral portion of the central rotating shaft 312 and further cools the inner side of the rotor 614 along the outer peripheral portion of the refrigerant shielding portion. The refrigerant storage portion constituting the refrigerant circulation path was formed.

  Furthermore, a communication hole for communicating the refrigerant storage part with each other was formed.

  Further, the rotor 614 shown in FIG. 4 introduces the refrigerant into the refrigerant reservoir from the end rotor through the refrigerant passage inside the rotation shaft from the rotor joint at the end of the rotor 614 shaft, and at the opposite end. A refrigerant circulation was provided to return from the rotor to the refrigerant passage of the rotating shaft again.

  The material to be crushed was pulverized under the same pulverization conditions as in Example 1 and Example 1, and the pulverization state of the pulverizer was evaluated in the same manner as in Example 1.

  In this comparative example, as in the example, an attempt was made to confirm the rotational peripheral speed at which a desired weight average diameter of the pulverized product was obtained.

  As a result, the pulverization chamber temperature rose from the point where the peripheral speed of the rotor 614 exceeded 125 m / sec, and there was a risk of fusion, so the pulverization was stopped. The above conditions are summarized in Table 1, and the results are summarized in Table 2.

  222 bag filter, 224 suction blower, 229 collection cyclone, 240 hopper, 301 pulverizer, 302 powder discharge port, 310 stator, 311 powder input port, 312 center rotation shaft, 313 casing, 314 rotor, 315 fixed amount Feeder, 316 Jacket, 317 Refrigerant supply port, 318 Refrigerant discharge port, 319 Dehumidified gas generator, 320 Blinchler, 322 Disc, 359 Distributor, 362 Bag filter, 364 Suction blower, 369 Collection cyclone, 380 hopper, 610 fixed Child, 614 rotor, 615 refrigerant shielding part, 616 refrigerant storage part

That is, a mixture containing at least a binder resin and a colorant is melt-kneaded, the obtained kneaded product is cooled, the cooled product is coarsely pulverized, and the obtained coarsely pulverized product is pulverized by a pulverizing means. In the method for producing a toner having at least a step of classifying the pulverized product by classification means,
The pulverizer used in the pulverizing means comprises at least a powder inlet for charging a coarsely pulverized product into the pulverizing means, a stator, a rotor attached to a central rotating shaft, and pulverized powder. A powder outlet for discharging from the pulverizing means,
The stator includes the rotor, and the rotor surface and the rotor surface are arranged so that there is a gap between the rotor and the rotor surface to form a grinding zone;
In the pulverization zone, the object to be crushed is pulverized as the rotor rotates, and the stator and the rotor have a plurality of convex portions and concave portions,
The irregularities are provided parallel to the central rotation axis;
The rotor is
i) Consists of multiple disks connected together,
ii) From one direction of the powder inlet side or the powder outlet side, passing through the center rotation shaft, introducing the refrigerant into the rotor, and the same direction with respect to the refrigerant introduction direction or In the opposite direction, it has a refrigerant flow path Q that passes through the center rotation shaft and discharges the refrigerant from the rotor,
Each disk constituting the rotor is respectively
i) Refrigerant flow path M for conveying the refrigerant introduced by the refrigerant flow path L to the outer layer of the disk;
ii) a refrigerant channel N for conveying the refrigerant conveyed through the refrigerant channel M to the outer layer of the disk in parallel with the central rotation axis; and
iii) having a refrigerant flow path P for returning the refrigerant conveyed through the refrigerant flow path N to the refrigerant flow path Q;
The temperature Trin (° C.) of the refrigerant introduced into the refrigerant flow path L is −20.0 ≦ Trin ≦ 20.0.
The present invention relates to a toner production method.

Claims (8)

A mixture containing at least a binder resin and a colorant is melt-kneaded, the obtained kneaded product is cooled, the cooled product is coarsely pulverized, and the resulting coarsely pulverized product is pulverized by a pulverizing means, and the obtained pulverized product In a method for producing a toner having at least a step of classifying a product by a classifying means,
The pulverizer used in the pulverizing means comprises at least a powder inlet for charging a coarsely pulverized product into the pulverizing means, a stator, a rotor attached to a central rotating shaft, and pulverized powder. A powder outlet for discharging from the pulverizing means,
The stator includes the rotor, and the rotor surface and the rotor surface are arranged so that there is a gap between the rotor and the rotor surface to form a grinding zone;
In the pulverization zone, the object to be crushed is pulverized as the rotor rotates, and the stator and the rotor have a plurality of convex portions and concave portions,
The unevenness is provided in parallel to the central rotation axis, and the rotor includes a cooling coolant channel inside.
The temperature Trin (° C.) of the refrigerant introduced into the refrigerant flow path is −20.0 ≦ Trin ≦ 20.0.
A method for producing a toner, wherein The relationship between the refrigerant temperature Trin (° C.) introduced into the refrigerant channel and the refrigerant temperature Trout (° C.) discharged outside the refrigerant channel is 5.0 ≦ Trout−Trin ≦ 25.0
The toner production method according to claim 1, wherein: The pulverizer includes a cooling jacket on the outer periphery of the stator, and the cooling refrigerant temperature Tjin (° C.) introduced into the jacket is −10.0 ≦ Tjin ≦ 10.0.
The toner production method according to claim 1, wherein the toner production method is a toner. The relationship between the refrigerant temperature Tjin (° C.) introduced into the jacket and the refrigerant temperature Tjout (° C.) discharged outside the jacket is 1.0 ≦ Tjout−Tjin ≦ 10.0
The method for producing a toner according to claim 1, wherein the toner is a toner. The flow rate Ar (m ³ / min) of the cooling refrigerant in the rotor is 1.0 ≦ Ar ≦ 15.0
The method for producing a toner according to claim 1, wherein: The pulverizer introduces a dehumidified gas into the apparatus together with the coarsely pulverized product, and the introduced dehumidified gas has a temperature Thin (° C.) of −10.0 ≦ Thin ≦ 40.0.
The method for producing a toner according to claim 1, wherein the toner is a toner. The temperature Thout (° C.) of the dehumidified gas discharged to the outside of the pulverizer is 20.0 ≦ Thout <60.0.
The method for producing a toner according to claim 1, wherein the toner is a toner. The cooling flow path of the grinder,
Length Dpr (mm) obtained by connecting a straight line from the center point p of the rotor to the bottom surface r of the concave portion of the rotor
A length Dpq (mm) obtained by connecting a straight line from the center point p of the rotor to the outermost shell q of the refrigerant flow path
If
The toner manufacturing method according to claim 1, wherein the toner is provided so as to satisfy the following formula.
1.0 ≦ Dpr−Dpq ≦ 25.0

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