JP5527942B2 - Crusher and toner manufacturing apparatus - Google Patents

Description

  The present invention relates to an apparatus for producing 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, and a method for producing toner using the device. .

  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 CO2 emission, and a pulverizer as shown in FIG. There are many.

  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. Moreover, since it is rarely excessively pulverized, the generation of fine powder is small, and it is possible to improve the classification yield in the subsequent classification process.

  However, as described above, the pulverizer shown in FIG. 6 has a configuration in which pulverization is performed by introducing a powder raw material into a pulverization zone formed between the rotor 314 rotating at high speed and the stator 310. Most of the factors that determine the amount of processing per hour are considered to be determined by the minimum interval between the rotor 314 and the stator 310.

  Therefore, in the pulverizer shown in FIG. 6, it is necessary to further increase the speed of the rotor 314 in order to increase the throughput per unit time while maintaining the desired toner particle diameter. However, the rotational speed of the rotor 314 has a limit point due to the device configuration.

  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.

  In order to prevent adverse effects on quality due to temperature rise in the pulverization chamber and in-machine fusion, if the minimum gap between the rotor 314 and the stator 310 is widened, the processing amount per unit time can be increased, but the desired toner particle diameter. Can not hold. This increases the burden on the next classification step, which is also not preferable in terms of toner productivity.

  In order to suppress the above-described temperature rise in the pulverization chamber, a pulverizer has been proposed in which an inner refrigerant circulation path for circulating the refrigerant to cool the rotor 314 is formed inside the rotor 314 (see Patent Document 1). .

  In the pulverizer disclosed in Patent Document 1, the rotor 314 itself is a single unit in which a plurality of rotors 314 having the same shape are combined. Each of the units is formed with a refrigerant reservoir that constitutes the inner refrigerant circulation path and a communication hole that communicates the refrigerant reservoir with each other along the outer periphery.

  Further, a plurality of communication holes for communicating the refrigerant storage portions with each other are provided along the outer peripheral portion of the unit, and the refrigerant storage portions are disposed on the inner side of the refrigerant storage portions of the units. A refrigerant shielding part is formed for limiting to only the outer peripheral part.

  According to Patent Document 1, an extremely high cooling effect can be obtained by circulating a refrigerant inside the rotor 314, and at the time of pulverization, objects to be crushed are melted and fused to each other, or the rotor 314 and the stator. It is prevented that 310 is fused and cannot be pulverized, and the object to be pulverized is deteriorated by heat. Furthermore, since it is possible to efficiently pulverize a granular material that is vulnerable to heat, productivity can be improved.

  However, when the size of the apparatus is increased with the configuration of the rotor 314 described above, there is a problem in that the main body vibration value in the high-speed rotation region of the rotor 314 is high and the pulverizer is stably operated.

  In the pulverizer, most of the factors that determine the pulverized particle size are considered to depend on the rotational speed of the rotor 314. As described above, if the rotor 314 cannot be stably rotated at a high speed, in order to cope with the small particle diameter toner having a weight average particle diameter of 5 to 7 μm, which has been required from the market in recent years, the processing amount per unit time must be reduced. In other words, it is not satisfactory from the viewpoint of toner productivity.

  Further, when the rotor 314 is rotated at a high speed, the temperature rise in the grinding chamber becomes a problem.

  According to Patent Document 1, at least one of the concave portion of the rotor 314 and the concave portion of the stator 310 is inclined in a direction that hinders the flow of the object to be pulverized, so that the time during which the pulverized particles stay in the pulverization chamber can be increased. For this reason, it is possible to prevent over-pulverization, reduce the particle size, and simultaneously prevent the generation of coarse particles.

  However, when the size of the apparatus is increased with the configuration of the rotor 314 and the stator 310 described above, the temperature rises rapidly in the grinding chamber in the high-speed rotation region of the rotor 314, which causes a problem in terms of stable operation of the grinder.

  In the pulverizer, the temperature rise in 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, it is necessary to reduce the rotational speed of the rotor 314 or the processing amount per unit time, which is also satisfactory from the viewpoint of toner productivity. It is not a thing.

The reason for the increase in the temperature in the grinding chamber, the increase in the vibration value, and the decrease in the cooling efficiency associated with the high-speed rotation of the rotor 314 is not clear, but both are refrigerants in the refrigerant reservoir when the rotor 314 is rotated at high speed. There is room for improvement in terms of stable operation in large equipment.
JP 2004-42029 A

  The object of the present invention is to solve the problems of the prior art, and even in a large pulverizer having a cooling refrigerant flow path inside the rotor 314, the temperature of the pulverization chamber is increased as the rotor 314 rotates at a high speed. Another object of the present invention is to provide a pulverizer capable of reducing an increase in vibration value of the main body and a decrease in cooling efficiency.

  Furthermore, an object of the present invention is to provide a toner manufacturing apparatus that can prevent adverse effects on quality due to an increase in temperature in the pulverization chamber and in-machine fusion, and can improve the throughput per unit time even in a large pulverizer. is there.

  As a result of studies to solve the above-described problems of the prior art, the present inventors have found that in a large pulverizer, the temperature of the pulverization chamber is increased, the vibration value of the main body is increased, and the cooling efficiency is increased as the rotor 314 rotates at high speed. The reason for the decrease is that the unevenness portions of the rotor 314 and the stator 310, the bias due to the change in the weight of the refrigerant itself when the refrigerant is flowing, and the cooling area inside the rotor 314 are insufficient. It came.

That is, the present invention provides a powder inlet for feeding a material to be crushed into the pulverizing means, a stator, a rotor attached to at least the central rotating shaft, and discharging the pulverized powder from the pulverizing means. A pulverizer having at least a powder discharge port for
The stator includes the rotor;
The rotor has a configuration in which a plurality of independent disks are connected, and the stator surface and the rotor surface are arranged so as to form a grinding zone with a predetermined gap. And
Each of the surface of the stator and the surface of the rotor is provided with a plurality of convex portions and concave portions,
The concave portion and the convex portion of the stator and the rotor are provided in parallel to the central rotation axis;
The rotor has a cooling refrigerant flow path inside,
The refrigerant flow path is
(I) Refrigerant flow path L for introducing a refrigerant from one direction of the powder inlet or the powder outlet through the central rotating shaft,
(Ii) a refrigerant channel M for conveying the refrigerant conveyed by the refrigerant channel L to the outer layer portion of the disk;
(Iii) Refrigerant flow path N that conveys the refrigerant conveyed to the outer layer portion of the disk by the refrigerant flow path M in parallel with the central rotational axis;
(Iv) A refrigerant flow path P for conveying the refrigerant conveyed by the refrigerant flow path N from the outer layer portion of the disk toward the central rotating shaft, and
(V) The refrigerant conveyed toward the central rotation axis by the refrigerant flow path P is different from the direction of the powder inlet side or the powder outlet side where the refrigerant is introduced. Refrigerant flow path Q that conveys the refrigerant so that the refrigerant is discharged from the powder discharge port side
Have
Each disk constituting the rotor has the refrigerant flow path M, the refrigerant flow path N, and the refrigerant flow path P independently of each other.
In each disk constituting the rotor, the refrigerant flow path N is a cooling hole provided in parallel to the central rotation axis, and in a cross section of the rotor in a direction perpendicular to the central rotation axis. The present invention also relates to a pulverizer characterized in that the plurality of cooling holes are arranged at regular intervals in the circumferential direction of the rotor.

  According to the present invention, even in a large pulverizer having a cooling refrigerant flow path inside the rotor 314, the temperature of the pulverization chamber is increased, the main body vibration value is increased, and the cooling is performed as the rotor 314 rotates at high speed. A reduction in efficiency can be reduced, and adverse effects on quality due to an increase in temperature in the grinding chamber and in-machine fusion can be prevented.

  Furthermore, according to the present invention, the processing amount per unit time can be improved by pulverizing the toner particles using the pulverizer described above. Furthermore, toner particles having a sharp particle size distribution can be obtained efficiently, stably, and with good toner productivity.

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

  Further, as a result of investigations to solve the above-described problems of the prior art, the inventors have raised the temperature of the crushing chamber, increased the vibration value of the main body, and the cooling efficiency accompanying the high-speed rotation of the rotor 314 in the large pulverizer. The reason for the decrease was thought to be the bias due to the change in the weight of the refrigerant itself when the refrigerant was flowing and the lack of the cooling area inside the rotor 314.

  That is, 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 vibration value of the main body due to the high-speed rotation of the rotor 314 can be reduced. It can be reduced and high cooling efficiency can be obtained.

  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. 1, 2, and 3.

  FIG. 1 shows an example of a schematic view of a rotor 314 and a stator 310 of a crusher used in the present invention, and FIGS. 2 and 3 show an example of a schematic cross-sectional view of the rotor 314 used in the present invention.

The pulverizer according to the present invention includes a powder inlet for charging a material to be pulverized into the pulverizing means, a stator, a rotor attached to at least the central rotating shaft, and the pulverized powder from the pulverizing means. Having at least a powder outlet for discharging,
(1) The stator includes the rotor,
(2) The stator surface and the rotor surface are arranged such that the rotor has a predetermined gap to form a grinding zone;
(3) In the pulverization zone, the object to be pulverized is pulverized as the rotor rotates.
(4) The stator surface and the rotor surface 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,
(6) As shown in FIG. 2, the rotor is characterized by having a cooling coolant flow path therein.

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

  Further, as shown in FIG. 3, the refrigerant flow path in the pulverizer of the present invention is a cooling hole N provided in parallel to the central rotation shaft 312, and the cooling hole N is in the direction of the central rotation axis. In a vertical cross section, the rotor is arranged at regular intervals in the circumferential direction of the rotor.

Further, the cooling hole N in the pulverizer of the present invention is characterized in that a cross-sectional area D in a cross section perpendicular to the central rotational axis direction shown in FIG. 2 is in a range of 18 mm ² or more and 2000 mm ² or less.

  As a result of investigations by the present inventors, in the pulverizer having a plurality of convex portions and concave portions on the surface of the stator 310 and the rotor 314, the concave and convex portions are parallel to the central rotation shaft 312. It has been found that the amount of processing per unit time can be improved by providing the rotor 314 with a cooling refrigerant flow path inside.

  Although it is not clear why the rotor 314 has a cooling refrigerant flow path inside to improve the throughput per unit time, the heat generated during the pulverization of toner particles It is considered that heat can be removed to some extent by passing the coolant through the coolant channel.

Further, the refrigerant flow path inside the rotor 314 of the present invention is as shown in FIG.
(1) From one direction of the powder inlet 311 side or the powder outlet 302 side, the central rotating shaft 312
A refrigerant flow path L for introducing the refrigerant through
(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.

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

  Further, the rotor 314 of the present invention is provided with a refrigerant flow path P for conveying the refrigerant from the outer layer portion of each disk 322 toward the central rotating shaft 312 independently according to the number of the disks 322. The refrigerant can be separately returned to the refrigerant flow path Q from the refrigerant flow path P provided independently in accordance with the number of sheets.

  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 rise, an increase in the body vibration value, and a decrease in cooling efficiency can be reduced, and adverse effects on quality due to a rise in the temperature in the grinding chamber and in-machine fusion can be prevented.

  Furthermore, the throughput per unit time can be improved, and toner particles having a sharp particle size distribution can be obtained efficiently, stably and satisfactorily in terms of toner productivity.

  Note that the rotor 314 of the present invention conveys the refrigerant from the outer layer part of each disk 322 toward the central rotation shaft 312 and / or the refrigerant flow path M for conveying the refrigerant to the outer layer part in each disk 322. It is preferable that the refrigerant flow path P to be configured is composed of a plurality of independent disks 322.

  Further, the rotor 314 of the present invention includes 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 rotation shaft 312. It is preferable that the number of the flow paths in the refrigerant flow path P for conveying the same 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.

Further, as a result of the study by the present inventors, the length obtained by connecting a straight line from the center point p of the rotor 314 to the recess bottom surface r of the rotor 314 shown in FIG. 2 is represented by Dpr and the center point p of the rotor 314. When the length connecting the straight line to the outermost shell q of the refrigerant flow path is defined as Dpq, a cooling refrigerant flow path is provided so as to satisfy the following formula (1). It was found that even at high speed rotation, the vibration value can be reduced and high cooling efficiency can be obtained.
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.

  Further, as a result of the study by the present inventors, as shown in the left diagram of FIG. 3, the cooling refrigerant flow path provided in the rotor 314 is a cooling hole H, and the cooling holes H are arranged at regular intervals. As a result, it has been found that the vibration value associated with the high-speed rotation of the rotor 314 can be reduced and high cooling efficiency can be obtained.

  As a result of investigations by the present inventors, by setting the coolant flow path as the cooling hole H, the cooling hole H can be brought close to the surface layer of the rotor 314 while ensuring the mechanical strength. Furthermore, by using the cooling hole H, efficient cooling with little unevenness can be obtained with the minimum necessary refrigerant.

  Furthermore, the cooling holes H can be arranged by arranging a plurality of cooling holes parallel to the central rotating shaft 312 at regular intervals, thereby obtaining a very large cooling area.

  The shape of the cooling hole H is preferably a cylindrical drill hole from the viewpoint of workability and volumetric accuracy, but the same effect can be obtained by a polygon such as a triangular quadrangle or a star by electric discharge machining or laser machining. can get. Also, a combination thereof may be used.

  Further, the cooling holes H can be arranged in two rows and three rows and a plurality of rows to further improve the cooling efficiency. Furthermore, by disposing the cooling hole N in parallel with the central rotation shaft 312, the swing of the refrigerant can be suppressed and the rotor 314 can be stably rotated at a high speed.

  In addition, the plurality of cooling holes H have the same volume and are arranged at equal intervals to eliminate imbalance due to the presence or absence of the refrigerant, and to stably and rapidly rotate the rotor 314 without being affected by the presence or absence of the refrigerant. Can be rotated.

  In addition, the both end surfaces of the cooling hole H are provided with spaces for connecting the plurality of cooling holes H, and the cylinder is welded or the plate is sealed with a sealing material such as an O-ring.

Furthermore, as a result of the study by the present inventors, the cross-sectional area D in the cross section perpendicular to the central rotation axis direction of the cooling hole H shown in FIG. 2 is in the range of 18 mm ² or more and 2000 mm ² or less. It was found that even at high speed rotation of the rotor 314, the vibration value can be reduced and high cooling efficiency can be obtained.

As a result of studies by the present inventors, when the cross-sectional area D in the cross section perpendicular to the central rotational axis direction of the cooling hole H is less than 18 mm ² , the number of processing steps for manufacturing the cooling hole H increases. The initial cost is not fully satisfactory.

Further, as a result of the study by the present inventors, when the cross-sectional area D in the cross section perpendicular to the central rotation axis direction of the cooling hole H exceeds 2000 mm ² , a sufficient cooling effect cannot be obtained, and the rotor Since the increase in the weight of 314 is accompanied, the rotor 314 is not fully satisfactory from the viewpoint of stable operation during high-speed rotation.

Furthermore, the present invention relates to a toner production apparatus used in a toner production method having a weight average particle size of 4 μm to 12 μm, which contains at least a binder resin and a colorant.
The toner particles are produced through at least a melt-kneading step, a coarse pulverization step, a fine pulverization step, and a classification step,
The toner production apparatus used in the fine pulverization step is:
A powder inlet for feeding the material to be crushed into the pulverizing means, a stator, a rotor attached to at least the central rotating shaft, and a powder discharger for discharging the pulverized powder from the pulverizing means. And at least an exit,
(1) The stator includes the rotor,
(2) The stator surface and the rotor surface are arranged such that the rotor has a predetermined gap to form a grinding zone;
(3) In the pulverization zone, the object to be pulverized is pulverized as the rotor rotates.
(4) The stator surface and the rotor surface are both pulverizers having a plurality of convex portions and concave portions,
(5) The concavo-convex portion is provided along the central rotation axis,
(6) The rotor is characterized by having a coolant flow path for cooling inside.

  As a result of studies by the present inventors, the toner configuration of the toner production apparatus used in the fine pulverization process is set to the above-described configuration, so that the cooling efficiency in the rotor 314 is improved, so that the toner particles in the pulverizer The grindability of the can be improved.

  In other words, by setting the apparatus configuration of the toner manufacturing apparatus used in the fine pulverization step as described above, the throughput per unit time can be improved without increasing the pulverization chamber temperature during toner particle pulverization. From the viewpoint of toner productivity.

  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.

  Although FIG. 6 shows a schematic cross-sectional view of a horizontal general pulverizer, it may be a vertical type and may have a built-in classification rotor. A rotor provided with a number of grooves on a surface rotating at high speed, which is 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 rotating shaft 312 in the casing 313. 314, the rotor 314 is included, the stator 310 is provided with a large number of grooves on the outer surface of the rotor 314 arranged at a constant interval, and a raw material to be treated is introduced. 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 vortexes generated and high-frequency pressure vibrations generated thereby.

  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 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.

  Further, the interdental distance formed by the unevenness is less than 1.0 mm, and the processing amount 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.

  Further, as a more preferable form of toner pulverization, air of + 30 ° C. or less is preferably blown into the pulverizer, the temperature of the air is more preferably +30 to −50 ° C., and +20 to −40 ° C. It is particularly preferred that

  Furthermore, as a more preferable form of pulverization of the toner, the temperature of the coolant flowing through the coolant channel and the jacket 316 is preferably 0 ° C. or less, and more preferably −5 ° C. or less.

  Next, a procedure for producing a toner in the toner production method 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 then pulverized to a desired particle size in a pulverization step.

  In the pulverization step, it is usually roughly pulverized by a crusher such as a crusher, hammer mill, feather mill, etc., and further, an inomizer (manufactured by Hosokawa Micron), a kryptron (manufactured by Kawasaki Heavy Industries), a super rotor (manufactured by Nisshin Engineering), Finely pulverized by a pulverizer such as a turbo mill (manufactured by Turbo Kogyo Co., Ltd.).

  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.

  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 shear force is applied to powders such as Henschel mixer, super mixer, mechano hybrid, nobilta, and cyclomix. Stir and mix using a high-speed stirrer that gives

  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. -1,000,000 are preferred.

  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 ), iron neodymium oxide (NdFe ₂ O ₃ ), iron barium oxide (BaFe ₁₂ O ₁₉ ), iron magnesium oxide (MgFe ₂ O ₄ ), iron manganese oxide (MnFe ₂ O ₄ ), iron lanthanum oxide (LaFeO ₃ ), iron powder (Fe), cobalt powder (Co), nickel powder (Ni) and the like.

  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 compounds, etc.), diorganotin oxides such as dibutyltin oxide, dioctyltin oxide, dicyclohexyltin oxide and dibutyltin as metal salts of higher fatty acids , Dioctyl tin borate include diorgano tin borate such as dicyclohexyl tin 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. What was processed so that the hydrophobization degree measured by the methanol titration test might show the value of the range of 30-80 is especially preferable.

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.

<Measuring method of weight average particle diameter (D4) and number average particle diameter (D1)>
The weight average particle diameter (D4) and number average particle diameter (D1) of the toner are measured by a fine particle size distribution measuring apparatus “Coulter Counter Multisizer 3” (registered trademark, Beckman 2) Effective measurement channel number 25,000 using “Beckman Coulter Multisizer 3 Version 3.51” (manufactured by Beckman Coulter, Inc.) and attached dedicated software “Beckman Coulter Multisizer 3 Version 3.51” for measurement condition setting and measurement data analysis Measurement was performed on the channel, and the measurement data was analyzed 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, the dedicated software was set 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 phases are shifted by 180 degrees, and placed in a water tank of an ultrasonic disperser “Ultrasonic Dissipation System Tetora 150” (manufactured by Nikki Bios) with 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) and the number average particle diameter (D1) are calculated. When the graph / volume% is set with the dedicated software, the “average diameter” on the analysis / volume statistics (arithmetic average) screen is the weight average particle size (D4), and the graph / number% is set with the dedicated software. The “average diameter” on the analysis / number statistic (arithmetic average) screen is the number average particle diameter (D1).

<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 after the above-described measurement of Multisizer 3.
(1) Set the graph / number% in the dedicated software to display the measurement result chart in number%,
(2) Check “<” in the particle size setting part on the format / particle diameter / particle diameter statistics screen, and enter “4” in the particle diameter input part below. And
(3) The numerical value of the “<4 μm” display portion when the analysis / number statistics (arithmetic mean) screen is displayed is the number% of particles of 4.0 μm or less in the toner.

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

For example, the volume% of particles having a particle size of 10.0 μm or more in the toner is measured by the above-described Multisizer 3 measurement.
(1) Set to graph / volume% with the dedicated software and display the measurement result chart in volume%,
(2) Check “>” in the particle size setting part on the format / particle diameter / particle diameter statistics screen, and enter “10” in the particle diameter input part below. And
(3) The numerical value in the “> 10 μm” display area when the analysis / volume statistics (arithmetic mean) screen is displayed is the volume% of particles of 10.0 μm or more 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 measurement sample and place it in an aluminum pan. Use an empty aluminum pan as a reference, and measure 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 the 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 5 to 20 mg, preferably 10 mg.

  This is put in 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 room temperature and humidity in a measurement temperature range of 30 to 200 ° C.

  In this temperature raising process, an endothermic peak of the main peak in the 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 0.5-2.0 g of a sample is correctly weighed in a round bottom flask, and 5 ml of an acetylating reagent is correctly added thereto. Put a small funnel over the mouth of the flask and immerse the bottom of about 1 cm in a glycerin bath at 95-100 ° C. and heat. 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]

<Method for analyzing magnetic iron oxide particles>
(A) Average particle diameter A photograph of a scanning electron microscope (30000 times) was taken and calculated with a ferret diameter.
(B) Magnetic properties Measured with an external magnetic field of 796 kA / m using a vibrating sample magnetometer VSM-P7 manufactured by Toei Kogyo.

  EXAMPLES Hereinafter, although an Example demonstrates this invention, this invention is not limited to these Examples. Part means part by mass.

<Example 1>
(Example of toner production)
Binder resin (polyester resin): 100 parts (Tg 60 ° C., acid value 19.5 mgKOH / g, hydroxyl value 24.8 mgKOH / g, molecular weight: Mp7400, Mn2900, Mw57000)
- iron oxide particles: 90 parts (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 (Hodogaya Chemical Co., Ltd., trade name: T-77)
Fischer-Tropsch wax: 3 parts (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, the rotor 314 shown in FIG. 3 includes 75 cooling coolant passages N therein, and the coolant passages N have the shape of cooling holes, and the cross-sectional area D of the cooling holes is 79 mm ² . did.

  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.

  Further, Dpr, which is the distance from the rotor 314 center point P shown in FIG. 2 to the rotor 314 surface recess bottom surface r, is 373 mm, and from the rotor 314 center point P, the outermost part of the refrigerant flow path N Dpq, which is the distance to the shell q, was 357 mm. Therefore, Dpr-Dpq in this example was 16 mm.

Further, as the pulverization conditions, the cold air temperature generated by the cold air generating means 319 shown in FIG. 6 is set to −15 ° C., the flow rate of the suction blower is set to 24 m ³ / min, and the supply amount of the material to be crushed from the quantitative supply unit 315 is 250 kg / hr.

  Further, the refrigerant temperature passed through the jacket 316 shown in FIG. 6 and the refrigerant temperature passed through the refrigerant flow path L shown in FIG. 3 are set to −10 ° C., and the refrigerant flow rate passed through the jacket 316 and the refrigerant flow rate passed through the refrigerant flow path L are set to 10 l. / Min.

  The material to be pulverized was pulverized with the pulverizer configuration and pulverization conditions described above, and the pulverization state of the pulverizer was evaluated according to the following items.

  In addition, the cold air temperature mentioned above shows the internal temperature of the powder inlet 311 shown in FIG. 6, and the pulverization chamber temperature shows the internal temperature of the powder outlet 302 shown in FIG.

(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) at a rotational peripheral speed of 25 m / sec, 50 m / sec, 100 m / sec, 125 m / sec, and 150 m / sec is measured. 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, less than 50 μm C: 50 μm or more, less than 75 μm D: 75 μm or more, less than 100 μm E: 100 μm or more

  The vibration measurement was performed using a porter vibro (model VM-3004SI) manufactured by IMV. The results are shown in Table 2, and the evaluation of the vibration difference in this example was A.

(Evaluation-2: Evaluation of crushing chamber temperature)
The desired weight average diameter of the pulverized product is set to 5.5 ± 0.2 μm, and the rotational peripheral speed at which the particle diameter is obtained is confirmed. At that time, the pulverization chamber temperature (T-OFF) in a state where the input of the object to be pulverized is stopped is confirmed.

Thereafter, a long run operation for 60 minutes is performed, and the pulverization chamber temperature (T-ON) in a stable state is confirmed. The temperature difference between T-ON and T-OFF was confirmed and evaluated according to the following criteria.
A: Less than 15 ° C B: 15 ° C or more, less than 20 ° C C: 20 ° C or more, less than 25 ° C D: 25 ° C or more, less than 30 ° C E: 30 ° C or more

  The results are shown in Table 2. In this example, toner particles having a rotational average speed of the rotor 314 of 150 m / sec and a weight average diameter of 5.5 μm can be obtained, and (T-OFF) is 20 ° C. T-ON) was 33 ° C., and the evaluation of the temperature difference was A.

<Examples 2, 3, and 4>
The coarsely pulverized product obtained in Example 1 was pulverized in the same manner as in Example 1 except that the position of the refrigerant flow path N was changed as described in Table-1. The results are shown in Table 2.

<Examples 5, 6, 7, and 8>
The coarsely pulverized product obtained in Example 1 was pulverized in the same manner as in Example 1 except that the cross-sectional area and the number of cooling holes H were changed as shown in Table-1. The results are shown in Table 2.

<Example 9>
The coarsely pulverized product obtained in Example 1 was subjected to a cold air temperature generated by the cold air generating means 319 shown in FIG. 6 at 11 ° C., the suction blower flow rate was set to 24 m ³ / min, and the material to be pulverized from the quantitative feeder 315. Was supplied at a rate of 250 kg / hr.

  Further, the refrigerant temperature passed through the jacket 316 shown in FIG. 6 and the refrigerant temperature passed through the refrigerant flow path L shown in FIG. 3 are set to −15 ° C., and the refrigerant flow rate passed through the jacket 316 and the refrigerant flow rate passed through the refrigerant flow path L are set to 15 l. / Min.

  The material to be crushed was pulverized with the pulverizer configuration and pulverization conditions described above, and the pulverization state of the pulverizer was evaluated in the same manner as in Example 1. As a result, the main body vibration value evaluation was A and the pulverization chamber temperature evaluation was B. .

<Example 10>
The coarsely pulverized product obtained in Example 1 was pulverized in the same manner as in Example 1. At that time, in this example, the rotor 314 shown in FIG. 3 was modified as follows. The rest was the same as in Example 1.

  As shown in Table 1, the rotor 314 shown in FIG. 3 had an outer diameter of 1000 mm and a total length of 440 mm. Note that the number of stages of the disk 322 is two.

  Further, Dpr, which is the distance from the rotor 314 center point P shown in FIG. 2 to the rotor 314 surface recess bottom surface r, is set to 498 mm, and from the rotor 314 center point P, the outermost part of the refrigerant flow path N Dpq, which is the distance to the shell q, was 472 mm. Therefore, Dpr-Dpq in this example was 16 mm.

Further, the rotor 314 shown in FIG. 3 has 102 cooling refrigerant passages N therein, and the refrigerant passages N have the shape of cooling holes, and the sectional area D of the cooling holes is 79 mm ² . did.

As the pulverization conditions, the cold air temperature generated by the cold air generating means 319 shown in FIG. 6 is set to −15 ° C., the flow rate of the suction blower is set to 36 m ³ / min, and the supply amount of the material to be crushed from the quantitative feeder 315 is 400 kg / hr. It was.

  Further, the refrigerant temperature passed through the jacket 316 shown in FIG. 6 and the refrigerant temperature passed through the refrigerant flow path L shown in FIG. 3 are set to −10 ° C., and the refrigerant flow rate passed through the jacket 316 and the refrigerant flow rate passed through the refrigerant flow path L are 15 l. / Min. The rest was the same as in Example 1.

  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. The results are shown in Table 2.

<Example 11>
The coarsely pulverized product obtained in Example 1 was pulverized in the same manner as in Example 1. At that time, in this example, the rotor 314 shown in FIG. 3 was modified as follows. The rest was the same as in Example 1.

  As shown in Table 1, the rotor 314 shown in FIG. 3 had an outer diameter of 150 mm and a total length of 440 mm. Note that the number of stages of the disk 322 is two.

  Further, Dpr, which is the distance from the rotor 314 center point P shown in FIG. 2 to the rotor 314 surface recess bottom surface r, is set to 73 mm, and from the rotor 314 center point P to the outermost part of the refrigerant flow path N. Dpq, which is the distance to the shell q, was 57 mm. Therefore, Dpr-Dpq in this example was 16 mm.

Further, the rotor 314 shown in FIG. 3 includes ten cooling refrigerant passages N therein, and the refrigerant passages N have the shape of cooling holes, and the sectional area D of the cooling holes is 79 mm ² . did.

As the pulverization conditions, the cold air temperature generated by the cold air generating means 319 shown in FIG. 6 is set to −15 ° C., the flow rate of the suction blower is set to 3 m ³ / min, and the supply amount of the material to be crushed from the quantitative feeder 315 is 30 kg / hr. It was.

  Further, the temperature of the refrigerant passing through the jacket 316 shown in FIG. 6 and the temperature of the refrigerant passing through the refrigerant flow path L shown in FIG. 3 are set to −10 ° C., and the flow rate of refrigerant passing through the jacket 316 and the flow rate of refrigerant passing through the refrigerant flow path L are 5 l. / Min. The rest was the same as in Example 1.

  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. The results are shown in Table 2.

<Example 12>
The coarsely pulverized product obtained in Example 1 was pulverized in the same manner as in Example 1. At that time, in this example, the same procedure as in Example 1 was performed except that the supply amount of the pulverized material was changed to 275 kg / hr.
The results are shown 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 is not passed through the coolant circulation path L shown in FIG. 3, and the pulverization conditions are generated by the cold air generating means 319 shown in FIG. 6 as shown in Table 3. The cold air temperature was set to −20 ° C., the flow rate of the suction blower was set to 24 m ³ / min, and the supply amount of the material to be crushed from the quantitative supply unit 315 was set to 250 kg / hr.

  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. The results are shown in Table 4.

<Comparative example 2>
The coarsely pulverized product obtained in Example 1 was pulverized using the pulverizer shown in FIG. In this comparative example, grinding was performed using the tooth-shaped rotor 314 and the stator 310 shown in FIG. 5, and grinding was performed under the following conditions.

  As shown in Table 3, the rotor 314 shown in FIG. 4 had an outer diameter of 750 mm and a total length of 440 mm. The number of stages of the disk 322 is five. Further, grinding was performed using the rotor 314 and the stator 310 shown in FIG. 5, and the distance between the rotor 314 and the stator 310 was set to 1 mm.

  Further, the rotor 314 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 314 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 314 shown in FIG. 4 introduces the refrigerant into the refrigerant reservoir from the end rotor through the refrigerant passage inside the rotary shaft from the rotor joint at the end of the rotor 314 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.

As pulverization conditions, as shown in Table 3, the cold air temperature generated by the cold air generating means 319 shown in FIG. 6 is −15 ° C., the flow rate of the suction blower is 24 m ³ / min, The supply amount was 250 kg / hr. The rest was the same as in Example 1.

  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. The results are shown in Table 4.

<Comparative Example 3>
The coarsely pulverized product obtained in Example 1 was pulverized in the same manner as in Example 1 except that the tooth-shaped rotor 314 and stator 310 shown in FIG. 5 were used. The results are shown in Table 4.

<Comparative Example 4>
The coarsely pulverized product obtained in Example 1 was pulverized using a pulverizer equipped with a rotor 314 shown in FIG. 4 and pulverized under the following conditions. Note that the rotor 314 and the stator 310 shown in FIG.

  As shown in Table 3, the rotor 314 shown in FIG. 4 had an outer diameter of 1000 mm and a total length of 440 mm. The number of stages of the disk 322 is five.

As pulverization conditions, as shown in Table 3, the cold air temperature generated by the cold air generating means 319 shown in FIG. 1 is set to −15 ° C., the flow rate of the suction blower is set to 36 m ³ / min. The supply amount was 400 kg / hr. The rest was the same as in Example 1.

  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, the desired weight average diameter of the pulverized product was set to 5.5 ± 0.2 μm, and an attempt was made to confirm the rotational peripheral speed at which the particle diameter was obtained. When the peripheral speed of the rotor 314 exceeded 100 m / sec, the vibration value increased. When the peripheral speed of the rotor 314 exceeded 125 m / sec, the vibration value exceeded 100 μm, so the pulverization was stopped.

<Comparative Example 5>
The coarsely pulverized product obtained in Example 1 was pulverized using a pulverizer equipped with a rotor 314 shown in FIG. 4 and pulverized under the following conditions. Note that the rotor 314 and the stator 310 shown in FIG.

  As shown in Table 3, the rotor 314 shown in FIG. 4 had an outer diameter of 150 mm and a total length of 440 mm. The number of stages of the disk 322 is five.

As pulverization conditions, as shown in Table 3, the cold air temperature generated by the cold air generating means 319 shown in FIG. 6 is set to −15 ° C., the flow rate of the suction blower is set to 3 m ³ / min. The supply amount was 30 kg / hr. The rest was the same as in Example 1.

  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. The results are shown in Table 4.

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.

Explanation of symbols

222 Bag filter 224 Suction blower 229 Collection cyclone 240 Hopper 301 Pulverizer 302 Powder discharge port 310 Stator 311 Powder input port 312 Central rotating shaft 313 Casing 314 Rotor 315 Metering feeder 316 Jacket 317 Cooling water supply port 318 Cooling Water outlet 319 Cold air generator 320 Blainchler 322 Disc

Claims (2)

A powder inlet for feeding the material to be crushed into the pulverizing means, a stator, a rotor attached to at least the central rotating shaft, and a powder discharger for discharging the pulverized powder from the pulverizing means. A crusher having at least an outlet,
The stator includes the rotor;
The rotor has a configuration in which a plurality of independent disks are connected, and the stator surface and the rotor surface are arranged so as to form a grinding zone with a predetermined gap. And
Each of the surface of the stator and the surface of the rotor is provided with a plurality of convex portions and concave portions,
The concave portion and the convex portion of the stator and the rotor are provided in parallel to the central rotation axis;
The rotor has a cooling refrigerant flow path inside,
The refrigerant flow path is
(I) Refrigerant flow path L for introducing a refrigerant from one direction of the powder inlet or the powder outlet through the central rotating shaft,
(Ii) a refrigerant channel M for conveying the refrigerant conveyed by the refrigerant channel L to the outer layer portion of the disk;
(Iii) Refrigerant flow path N that conveys the refrigerant conveyed to the outer layer portion of the disk by the refrigerant flow path M in parallel with the central rotational axis;
(Iv) A refrigerant flow path P for conveying the refrigerant conveyed by the refrigerant flow path N from the outer layer portion of the disk toward the central rotating shaft, and
(V) The refrigerant conveyed toward the central rotation axis by the refrigerant flow path P is different from the direction of the powder inlet side or the powder outlet side where the refrigerant is introduced. Refrigerant flow path Q that conveys the refrigerant so that the refrigerant is discharged from the powder discharge port side
Have
Each disk constituting the rotor has the refrigerant flow path M, the refrigerant flow path N, and the refrigerant flow path P independently of each other.
In each disk constituting the rotor, the refrigerant flow path N is a cooling hole provided in parallel to the central rotation axis, and in a cross section of the rotor in a direction perpendicular to the central rotation axis. A pulverizer, wherein the cooling holes are arranged at regular intervals in the circumferential direction of the rotor. In a toner production apparatus used in a method for producing toner particles having a weight average particle diameter of 4 μm to 12 μm containing at least a binder resin and a colorant,
The toner particles are produced through at least a melt-kneading step, a coarse pulverization step, a fine pulverization step, and a classification step,
The equipment used for the pulverization step is:
A powder inlet for feeding the material to be crushed into the pulverizing means, a stator, a rotor attached to at least the central rotating shaft, and a powder discharger for discharging the pulverized powder from the pulverizing means. A crusher having at least an outlet,
The stator includes the rotor;
The rotor has a configuration in which a plurality of independent disks are connected, and the stator surface and the rotor surface are arranged so as to form a grinding zone with a predetermined gap. And
Each of the surface of the stator and the surface of the rotor is provided with a plurality of convex portions and concave portions,
The concave portion and the convex portion of the stator and the rotor are provided in parallel to the central rotation axis;
The rotor has a cooling refrigerant flow path inside,
The refrigerant flow path is
(I) Refrigerant flow path L for introducing a refrigerant from one direction of the powder inlet or the powder outlet through the central rotating shaft,
(Ii) a refrigerant channel M for conveying the refrigerant conveyed by the refrigerant channel L to the outer layer portion of the disk;
(Iii) Refrigerant flow path N that conveys the refrigerant conveyed to the outer layer portion of the disk by the refrigerant flow path M in parallel with the central rotational axis;
(Iv) A refrigerant flow path P for conveying the refrigerant conveyed by the refrigerant flow path N from the outer layer portion of the disk toward the central rotating shaft, and
(V) The refrigerant conveyed toward the central rotation axis by the refrigerant flow path P is different from the direction of the powder inlet side or the powder outlet side where the refrigerant is introduced. Refrigerant flow path Q that conveys the refrigerant so that the refrigerant is discharged from the powder discharge port side
Have
Each disk constituting the rotor has the refrigerant flow path M, the refrigerant flow path N, and the refrigerant flow path P independently of each other.
In each disk constituting the rotor, the refrigerant flow path N is a cooling hole provided in parallel to the central rotation axis, and in a cross section of the rotor in a direction perpendicular to the central rotation axis. A toner manufacturing apparatus, wherein the plurality of cooling holes are arranged at regular intervals in the circumferential direction of the rotor.

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