JP2019069400A - Heat treatment apparatus, and method of producing powder particle - Google Patents

Abstract

A heat treatment apparatus capable of reducing the fusion of powder particles in the apparatus and producing uniform powder particles with a small particle diameter even when the amount of raw material is increased. A cylindrical processing chamber, powder particle supply means, hot air supply means, cold air supply means, a plurality of discharge ports for discharging powder particles to the outside of the processing chamber, and discharged from the discharge ports. A collecting member for collecting the powder particles, and a collecting means for collecting the powder particles. The hot air supply means includes a swirling member, and the powder particle supply means has the same swirling direction as the hot air. The cold air supply means is provided so that the cold air is supplied in the same direction as the swirling direction of the hot air, and the plurality of discharge ports are provided on the outer periphery of the processing chamber. And a lower end portion of the assembly member, and the assembly member is provided so that the powder particles are introduced in a tangential direction with respect to an inner peripheral surface of the assembly member. [Selection] Figure 2

Description

  The present invention relates to a method of producing powder particles such as toner used in an image forming method such as electrophotography, electrostatic recording, electrostatic printing, or toner jet recording.

In the electrophotographic image forming method, toner for developing an electrostatic charge image is used. The toner production method is roughly classified into a pulverization method and a polymerization method, and a pulverization method is mentioned as a simple production method.
As a general manufacturing method, materials such as a binder resin for fixing on a transfer material, a coloring agent for giving a color as toner, and a wax for improving the releasability between a fixing member and a toner are mixed. Next, these mixtures are melt-kneaded, cooled and solidified to obtain a kneaded product. Further, the obtained kneaded product is refined by a pulverizing means, and if necessary, it is classified into a desired particle size distribution, and then a fluidizing agent or the like is added to obtain a toner to be provided for image formation.

In recent years, with the development of high image quality and high definition in copiers and printers, toner particle sizes have become small, and as particle size distributions of toners, sharp toners that do not contain coarse particles have been required.
In addition, one of the requirements for high image quality is the in-plane gloss uniformity of the image. The uniformity of the in-plane gloss of the image is related to the removability of the fixing member and the toner, and a wax is added to the toner to improve the in-plane gloss uniformity of the image.
Furthermore, as a transfer material for copying machines and printers, it has become necessary to cope with various materials other than ordinary paper, and improvement of the transferability of toner is also required.
In order to meet the above-mentioned requirements, it has become necessary to make wax-containing toner powder particles spherical.

On the other hand, however, if the toner is too spherical, the cleaning ability is reduced, so it is also required to control the degree of sphericity of the toner to achieve both the transferability and the cleaning ability. To meet such requirements, one method of controlling the degree of sphericity of the toner is to melt the surface of the toner by heat treatment to make the toner spherical.
In the sphericization of the toner by heat treatment, in order to make the transferability and the cleaning ability compatible, it is required to suppress the coalescence of the toner at the time of the heat treatment and uniformly perform the heat treatment to make the shape uniform.
However, when the powder particle for toner containing wax is heat-treated, the wax existing inside the powder particle melts and exudes to the surface, thereby increasing the adhesion and melting the powder particle in the heat treatment apparatus. In some cases, it is difficult to stably produce a small particle size and uniform toner.

In order to improve the fusion, the cooling air from the top of the side wall of the heat treatment chamber of the heat treatment apparatus is blown in a slit shape to suppress adhesion and turbulent flow of powder particles, and further introduces the cooling air to the lower side wall of the apparatus. Proposals have been made to improve productivity (see Patent Document 1).
However, in such a device configuration, since the dispersed air flow and the heating air flow of the raw material are swirling flows, the introduced cooling air is vertical, and turbulence may be generated in the device. For this reason, if heat treatment is performed by increasing the processing amount of the powder particles for toner, fusion of the powder particles occurs in the device, and it becomes difficult to stably produce a small particle diameter and sharp toner. There is a case. Furthermore, in this device configuration, the heating air flow is cooled by the dispersed air flow of the raw material, so it is necessary to apply an amount of heat more than necessary for the spheroidization of the powder particles for toner.

Further, a heat treatment apparatus has been proposed which has a turning mechanism for dispersing the raw material, and a heating mechanism for heating the dispersed raw material from the inside (see Patent Document 2).
However, when heat treatment is performed with this device configuration, the dispersed air flow of the raw material and the heating air flow may turn in opposite directions to each other, and the air flow may be disturbed in the device. Also in this apparatus configuration, the heating air flow is cooled by the dispersion air flow of the raw material, and it is necessary to apply an amount of heat more than necessary to make the toner powder particles spherical. For this reason, when the processing amount is increased using powder particles for toner, the powder particles for toner adhere to the top surface, wall surface, and discharge port of the device due to the turbulence of the air flow and excessive heat generated in the device. , Fusion may occur.

On the other hand, the hot air, the raw material and the cold air are supplied in the same swirling direction, the flow of the raw material is regulated by the columnar members in the processing chamber, and the discharge port also maintains the flow of powder particles swirling in a spiral. A heat treatment apparatus provided has been proposed (see Patent Document 3).
However, when the powder particles for toner are heat-treated with this device configuration, if the outlet is a single mouth, blow-out occurs on the bottom surface inside the device, and there is a portion where the wind does not flow. Powder particles may be deposited. If the processing amount of the powder particles for toner is further increased in this state, the temperature of the hot air must be increased by an amount corresponding to the increased processing amount, and thus the deposited powder particles for toner may be fused. There is.

JP-A-59-125742 Japanese Patent Application Laid-Open No. 62-133466 JP, 2013-20245, A

As described above, in the conventional heat treatment apparatus, when heat treating powder particles for toner, a small particle size and uniform toner can be stably and in large quantities without fusing the powder particles for toner in the heat treatment apparatus. There is room for improvement in the manufacturing method of the heat treatment apparatus and the toner for manufacturing.
The object of the present invention is to reduce the fusion of powder particles in the apparatus even if the throughput of the raw material is increased when the powder particles are spheroidized by heat treatment, and the powder particles having small particle size and uniformity. It is an object of the present invention to provide a heat treatment apparatus capable of producing

The inventors of the present invention can reduce the adhesion in the apparatus even if the throughput of the powder particles is increased, and the powder particles are processed by the heat treatment apparatus in order to produce uniform powder particles with a small particle diameter. It has been found that the method of cooling after being discharged from the chamber is important and has led to the present invention.
That is, the present invention is a heat treatment apparatus for heat treating powder particles,
The heat treatment apparatus
(1) A cylindrical processing chamber in which the heat treatment of the powder particles is performed,
(2) powder particle supply means for supplying the powder particles to the processing chamber;
(3) hot air supply means for supplying hot air into the processing chamber;
(4) cold air supply means for supplying cold air into the processing chamber;
(5) a plurality of outlets for discharging the heat treated powder particles out of the processing chamber;
(6) A collective member for conveying powder particles discharged from the discharge port while cooling to the collection means;
(7) recovery means for recovering powder particles discharged from the collecting member;
Have
The hot air supply means is provided at the upper end side of the processing chamber, and comprises a pivoting member for spirally swirling the hot air in the processing chamber,
The powder particle supply means is provided at a lower portion of the hot air supply means so as to supply powder particles in the same direction as the swirling direction of the hot air along the inner circumferential surface of the processing chamber,
The cold air supply means is provided at a lower portion of the powder particle supply means so as to supply cold air in the same direction as the swirling direction of the hot air along the inner circumferential surface of the processing chamber,
A plurality of the discharge ports are provided at an outer peripheral portion and a lower end portion of the processing chamber so as to exist on the same cross section orthogonal to the central axis of the cylindrical processing chamber;
The interior of the collecting member has a structure capable of maintaining the turning of the powder particles,
The inlet of the powder particles to the collecting member is provided such that the powder particles are introduced tangentially to the inner circumferential surface of the collecting member,
The number of the inlets is the same as the number of the outlets of the processing chamber, and the inlets and the outlets are connected in a one-to-one manner via a transport pipe.
The present invention relates to a heat treatment apparatus characterized in that there is one outlet for discharging the powder particles from the collecting member, and the outlet and the recovery means are connected.

  According to the present invention, when the powder particles are spheroidized by heat treatment, the fusion in the apparatus is reduced even if the throughput of the raw material is increased, and the powder particles having a small particle diameter stably can be stably obtained. It can be manufactured.

Schematic perspective view showing an example of the heat treatment apparatus of the present invention Schematic sectional view of the processing chamber and the collecting member on the plane A-A 'in FIG. A pivoting member for spirally swirling hot air used in a heat treatment apparatus Schematic sectional view of the assembly member used in the embodiment Schematic sectional view of another assembly member used in the embodiment Schematic sectional view of another assembly member used in the embodiment Schematic cross-sectional view of another assembly member used in the comparative example Schematic cross-sectional view of heat treatment apparatus used in comparative example Schematic sectional view of another heat treatment apparatus used in the comparative example Schematic cross-sectional view of another heat treatment apparatus used in a comparative example

In the present invention, the descriptions of “more than or equal to or less than xxx” and “o to xxx” indicating numerical ranges mean numerical ranges including the lower limit and the upper limit which are end points unless otherwise noted.
Hereinafter, the present invention will be described in more detail by citing preferred embodiments. First, an outline of a heat treatment apparatus used in the present invention will be described with reference to FIGS. 1, 2 and 3. FIG. 1 is a schematic perspective view showing an example of a heat treatment apparatus according to the present invention. FIG. 2 is a schematic cross-sectional view showing an example of a heat treatment apparatus and an assembly member on the A-A ′ plane in FIG. FIG. 3 is a pivoting member for spirally swirling hot air used in the heat treatment apparatus of the present invention.

As shown in FIG. 1 and FIG. 2, the heat treatment apparatus of the present invention has a processing chamber 1 in which heat treatment of powder particles is performed, and powder particle supply means 2 for supplying powder particles to the processing chamber 1.
In the heat treatment apparatus of the present invention, the shape of the processing chamber 1 is preferably a cylindrical shape having an inner peripheral surface, and the inner diameter T (mm) of the processing chamber 1 is preferably 350 mm ≦ T ≦ 900 mm. If the inner diameter of the processing chamber 1 is within the above range, powder particles can be efficiently produced. When 350 mm ≦ T, the dust concentration of the powder particles in the processing chamber 1 does not easily increase, and the processing amount tends to increase. Further, when T ≦ 900 mm, it is not necessary to enlarge the ancillary equipment of the heat treatment apparatus such as a blower, a heater, or a cold air generator, which is preferable in terms of energy for producing powder particles. The inner diameter T (mm) is more preferably 400 m ≦ T ≦ 550 mm. The term “cylindrical” includes not only a perfect cylinder but also a substantially cylindrical shape in which a part has a conical shape.

  Furthermore, it is preferable that the processing chamber 1 be cooled by a cooling jacket in order to prevent fusion of the powder particles. It is desirable to introduce cooling water (preferably, an antifreeze liquid such as ethylene glycol) into the cooling jacket, and the surface temperature of the cooling jacket on the circumferential surface of the processing chamber is preferably 40 ° C. or less. Since the surface temperature of the inner circumferential surface of the processing chamber is 40 ° C. or less, the wax exudes to the surface of the powder particle when the powder particle for toner containing wax is heat-treated, and the adhesion is increased, Fusion in the heat treatment apparatus can be reduced.

In the heat treatment apparatus, powder particles are accelerated and conveyed by injection air supplied from a high pressure air supply nozzle (not shown), and supplied from the powder particle supply means 2 to the processing chamber 1.
The powder particle supply means 2 is provided in the lower part of the hot air supply means 3 so that the powder particles are supplied along the inner peripheral surface of the processing chamber in the same direction as the swirling direction of the hot air. Further, a plurality of powder particle supply means 2 are provided on the outer peripheral portion of the processing chamber so as to exist on the same cross section orthogonal to the central axis of the cylindrical processing chamber 1. The plurality of powder particle supply means 2 are preferably provided at equal intervals.

  As the number of divisions of the powder particle supply means 2 increases, the powder particles immediately after being introduced into the processing chamber are subjected to heat treatment in a state where the dust concentration is lowered. As a result, as the number of divisions of the powder particle supply means 2 increases, the temperature required for the heat treatment can be lowered. In addition, when the powder particle supply means 2 is divided into a plurality of pieces, the dust concentration per powder particle supply means is reduced by the divided amount when the processing amount is the same. For this reason, when the throughput is increased under the same conditions, the amount of increase in the dust concentration of the powder particles introduced into the processing chamber 1 is reduced as the number of divisions of the powder particle supply means 2 is increased. Even if the throughput of body particles is increased, coalescence particles are reduced.

  Although the number of divisions of the powder supply means depends on the inner diameter T of the processing chamber, for example, when the inner diameter T of the processing chamber is in the above range (particularly preferably 450 mm), 4 to 12 divisions are preferable, and more preferable. Is divided into eight. When the powder supply means is divided into eight parts, it is possible to suppress an increase in coalescent particles of the powder particles even if the processing amount is increased at the time of heat treatment of the powder particles. It is easy to reduce the dust concentration per powder particle supply means as it is four divisions or more, and processing amount can be increased. In addition, since the distance between the outlets of the powder particle supply means is not too close to 12 divisions or less, the dust concentration in the processing chamber is easily reduced.

The heat treatment apparatus of the present invention comprises a hot air supply means 3 for supplying hot air into the processing chamber 1. The hot air supply means 3 is provided on the upper end side of the processing chamber, and includes a pivoting member for spiraling the hot air in the processing chamber (preferably from the top to the bottom).
The heat treatment apparatus also includes cold air supply means for supplying cold air into the processing chamber. The cold air supply means is provided in the lower part of the powder particle supply means 2 so that the cold air is supplied along the inner peripheral surface of the processing chamber in the same direction as the swirling direction of the hot air. The cold air supply means includes a first cold air supply means 4 for supplying cold air for cooling the heat-treated powder particles into the processing chamber 1, and a second cold air for cooling the vicinity of the plurality of outlets 5 in the processing chamber 1. It is preferable to have the supply means 6.
In order to cope with the improvement of the transferability of toner required in recent years, the average circularity of heat-treated powder particles for toner is preferably 0.960 or more, more preferably 0.965 or more. In the present specification, the heat-treated powder particles for toner are also referred to as heat-treated particles for toner.

Therefore, the temperature N (° C.) of the hot air supplied into the processing chamber 1 is preferably 100 ° C. ≦ N ≦ 300 ° C. If the temperature of the hot air is within the above range, it is possible to make the powder particles have a desired average circularity while preventing fusion or coalescence of the powder particles due to excessive heating of the powder particles. Become. When 100 ° C. ≦ N, sphericization of the powder particles is sufficient. In addition, when N ≦ 300 ° C., the processing temperature is not too high, and the powder particles are less likely to be fused in the apparatus. Moreover, enlargement of the hot air generator is unnecessary, which is preferable in terms of energy for producing powder particles.

Further, as shown in FIG. 3, the hot air supply means 3 is equipped with a turning member 10 for turning the hot air in the processing chamber 1 in a spiral shape.
In the heat treatment apparatus of the present invention, a shear force is applied to the powder particles in the treatment chamber 1 by introducing hot air into the treatment chamber 1 while spirally swirling, and heat treatment is performed in the state where the powder particles are dispersed. . For this reason, the collision of the powder particles in the processing chamber 1 is reduced, and the coalescent particles are reduced. The swing member 10 for swirling the hot air may have a configuration that can spirally introduce the hot air into the processing chamber. As the structure, the turning member 10 for turning hot air has the some braid | blade 11, and the structure which can control turning of hot air by the number and angle of those is preferable.

Further, as shown in FIG. 3, since the hot air is introduced in a spiral form between the plurality of blades 11, the gap G (mm) between the blades becomes narrower as the number thereof becomes larger, and the flow velocity of the supplied hot air Will be faster. For example, when the inner diameter T of the processing chamber is in the above range (particularly preferably 450 mm), the gap G (mm) of the blade is preferably 5 mm ≦ G ≦ 40 mm.
In the case of 5 mm ≦ G, the flow velocity of the hot air is too fast, and the heat treatment temperature may not be increased. Further, in the case of G ≦ 40 mm, since the swirling speed of the hot air introduced into the processing chamber 1 becomes appropriate, a sufficient shearing force can be applied to the powder particles, and the coalescence of the powder particles during heat treatment is suppressed. it can.

  Further, the hot air supply means 3 preferably has a substantially conical distribution member 14. Since the hot air supply means 3 has the substantially conical distribution member 14, the bias of the hot air supplied to the processing chamber 1 can be eliminated, and the temperature distribution of the hot air in the processing chamber is uniformed, so powder When heat treating body particles, it is not necessary to apply an excessive temperature.

In the heat treatment apparatus of the present invention, the heat-treated powder particles are cooled by the cold air supplied from the cold air supply means (preferably the first cold air supply means 4 and the second cold air supply means 6).
Like the powder particle supply means 2, the first cold air supply means 4 and the second cold air supply means 6 are preferably provided so that the supplied cold air is supplied along the inner peripheral surface of the processing chamber 1. Furthermore, a plurality of first cold air supply means 4 and second cold air supply means 6 are preferably provided on the outer peripheral portion of the processing chamber so as to be present on the same cross section orthogonal to the central axis of the cylindrical processing chamber. As a result, the swirling flow in the apparatus is strengthened, shear force is applied to the powder particles, and the dispersibility of the powder particles is improved.

Moreover, as the first cold air supply means 4 and the second cold air supply means 6 increase in the number of divisions, the heat-treated powder particles become easier to cool. This makes it possible to reduce the number of powder particles that are the cause of coalescence particles without being cooled after being heat treated.
The number of divisions of the first cold air supply means 4 and the second cold air supply means 6 is preferably the same as the number of divisions of the powder particle supply means 2 from the viewpoint of preventing turbulent flow in the apparatus. For example, FIGS. 1 and 2 show an example of eight divisions. When the division number of the first cold air supply means and the second cold air supply means is the same as the division number of the powder particle supply means, the heat-treated powder particles are easily cooled. In addition, turbulent flow is less likely to occur in the apparatus, and the throughput can be easily increased.

Furthermore, in order to prevent adhesion and fusion of powder particles, the heat treatment apparatus of the present invention preferably includes second cold air supply means 6 for cooling the outlet 5 of the processing chamber 1.
The second cold air supply means 6 prevents the adhesion and fusion of the powder particles by cooling the powder particles that can not be cooled by the first cold air supply means 4.

The heat treatment apparatus of the present invention comprises a plurality of discharge ports 5 for discharging the heat treated powder particles out of the processing chamber. A plurality of discharge ports 5 are provided on the outer peripheral portion and the lower end portion of the processing chamber so as to exist on the same cross section orthogonal to the central axis of the cylindrical processing chamber. As a result, the heat-treated powder particles for toner are discharged out of the processing chamber while maintaining the swirling direction.
By maintaining the swirling flow in the device, the shear force exerted on the powder particles can be maintained, and coalescence particles can be reduced.

  In the heat treatment apparatus, it was found that when the discharge port is a single mouth, blow-up occurs at the bottom of the processing chamber, there is a portion where the wind does not flow, and the heat treated powder particles may be deposited on that portion. The If the throughput of the powder particles is increased in this state, the temperature of the hot air must be increased, and the deposited powder particles may be fused by heat.

  Further, in the heat treatment apparatus of the present invention, the number of discharge ports is preferably equal to the number of powder particle supply means 2. With the same number of outlets and powder particle supply means, the flow in the device can be rectified and coalescent particles can be reduced. In addition, the powder particles that have been heat-treated do not easily deposit on the bottom of the device, and fusion can be suppressed.

In the heat treatment apparatus of the present invention, as shown in FIG. 1, the powder particle supply means 2 and the cold air supply means (preferably the first cold air supply means 4 and the second cold air supply means 6) Provided in The powder particles supplied from the powder particle supply means 2, the first cold air supplied from the first cold air supply means 4, and the second cold air supplied from the second cold air supply means 6 It is supplied in the same direction as the swirling direction of the hot air along the inner circumferential surface.
When the flow of powder particles and cold air supplied to the processing chamber is the same as the swirling direction of the hot air, the shear force applied to the powder particles during heat treatment is increased, so the powder particles are highly dispersed in the processing chamber Do. As a result, even if the dust concentration in the processing chamber is increased, the collision of the powder particles is not increased, and the processing amount of the powder particles can be increased.

In the heat treatment apparatus of the present invention, preferably, the plurality of powder particle supply means and the cold air supply means are arranged at equal intervals in the same cross section orthogonal to the central axis of the cylindrical processing chamber. Further, a plurality of discharge ports are arranged at equal intervals in the same cross section orthogonal to the central axis of the cylindrical processing chamber.
By arranging the plurality of powder particle supply means at equal intervals, the flow in the apparatus is rectified and the dust concentration in the apparatus is uniformed. For this reason, since it is not necessary to apply excess heat more than necessary when heat-spheroidizing powder particles, the amount of coarse particles can be reduced and the amount of processing can be increased.

Similarly, by arranging the plurality of cold air means at equal intervals, the flow in the apparatus is rectified, so that powder particles with a small amount of coarse powder can be obtained.
Further, by disposing the plurality of discharge ports at equal intervals, the flow in the apparatus is further rectified, and powder particles with a small amount of coarse powder can be obtained. In addition, since the bubbling of the bottom of the processing chamber is eliminated, the fusion can be reduced even if the powder particles are heat-treated at a high processing temperature when the processing amount is increased.

The heat treatment apparatus of the present invention has, on the central axis of the processing chamber 1, a regulating means 19 which is a columnar member having a circular cross section and which is disposed to project from the lower end to the upper end of the processing chamber. Is preferred.
In order to prevent fusion of the powder particles, it is preferable to provide a cooling jacket in the regulation means 19 which is a columnar member having a circular cross section. Furthermore, it is desirable to introduce cooling water (preferably, an antifreeze liquid such as ethylene glycol) into the cooling jacket, and the surface temperature of the cooling jacket is preferably 40 ° C. or less.
Moreover, the control means 19 should just be a columnar member which is circular in cross section, and the root part of the columnar member may become thick as it goes to the downstream side of a processing chamber. As a result, the powder particle flow velocity on the downstream side of the processing chamber can be increased, and the dischargeability of the powder particles can be improved, and adhesion, fusion and powder particles at the bottom of the processing chamber can be prevented. it can.
Furthermore, since the discharge port 5 is provided on the outer periphery of the processing chamber 1 so that the swirling direction of the powder particles is maintained, the swirling flow in the apparatus can be maintained, and the powder particles are applied to the powder particles. The centrifugal force and the shear force are maintained, and adhesion and fusion of the powder particles to the regulating means 19 are reduced.

Next, the outline of the assembly member will be described using FIGS. 2 and 4.
The collecting member has a structure in which the inside of the collecting member can maintain the swirl of the powder particles, and is a member for conveying the powder particles discharged from the discharge port 5 of the processing chamber 1 while cooling to the recovery means (not shown) It is.
The structure capable of maintaining the turning of the powder particles is preferably a structure having a circular horizontal cross section. For example, as shown in FIG. 4, it is preferable that the horizontal cross section of at least the internal processing space (for example, the portion where the inlet and the cold air supply means exist) provided in the collecting member is circular. It is only necessary that the swirling of the powder particles be maintained, and a cylindrical or conical shape is preferred. The cylindrical or conical shape facilitates maintaining the swirling flow in the collecting member as described later.
The collecting member and the processing chamber are connected by a transfer pipe. The collecting member is preferably provided below the outlet of the processing chamber.
The cooling means in the collecting member is preferably a means using a cooling jacket into which cooling water (preferably, an antifreeze liquid such as ethylene glycol) is introduced. The surface temperature of the cooling jacket is preferably 40 ° C. or less.

As shown in FIG. 4, the inlet 18 of the collecting member is characterized in that the powder particles are introduced tangentially to the inner circumferential surface of the collecting member. The powder particles are supplied tangentially to the outer peripheral portion of the collecting member, so that a swirling flow occurs in the collecting member and the powder particles discharged from the discharge port 5 are rectified and, at the same time, the cooling jacket It is cooled by For this reason, powder particles that can not be cooled in the heat treatment apparatus are cooled in the collecting member. The inlet 18 of the collecting member is preferably provided so as to introduce powder particles in the horizontal direction and in a tangential direction with respect to the inner circumferential surface of the collecting member. The horizontal direction includes not only perfect horizontal direction but also substantially horizontal direction. That is, it is preferable that the inlet 18 be provided in the direction in which the spiral swirl generated in the processing chamber is maintained.
As a result, the powder particles obtained from the recovery means have less coalescence and have a uniform shape due to the rectification effect by the swirling flow caused by the inlet provided in the tangential direction and the cooling effect by the jacket cooling. Become.
Preferably, the turning direction in the collecting member and the turning direction in the heat treatment apparatus are the same.

As shown in FIGS. 2 and 4, the number of inlets 18 of the collecting member is the same as the number of outlets 5 of the processing chamber, and the collecting member inlet and the outlet are in one-to-one correspondence with each other via the transport pipe 13. It is characterized by being connected.
With the same number of inlets 18 of the collecting member and the outlets 5 of the processing chamber, it is introduced into the collecting member while maintaining the dust concentration of the powder particles discharged from the outlet 5. For this reason, the heat-treated powder particles are introduced into the collecting member in a state in which it is difficult to unite. If the number of inlets of the collecting member is smaller than the number of outlets of the processing chamber, the powder particles may be coalesced while passing through the transport pipe. In addition, when the number of inlets of the collecting member is larger than the number of outlets of the processing chamber, turbulent flow may occur in the collecting member, and powder particles having a uniform shape may not be obtained.

The outlet 17 for discharging the powder particles in the collecting member is one, and the outlet 17 and the recovery means are connected. As shown in FIGS. 2 and 4, it is preferable that the outlet be formed in a funnel shape with its horizontal cross section becoming smaller as it goes downward from the cold air supply means.
With one outlet 17 of the collecting member, even if there are a plurality of outlets 5 in the processing chamber, powder particles can be recovered by one recovery means. In the present invention, it is preferable to use a centrifugal dust collector such as a cyclone as the recovery means.

The collecting member preferably includes powder particle regulating means 15 for rotating the powder particles supplied into the collecting member.
As shown in FIGS. 2 and 4, it is preferable that the collecting member be provided with powder particle regulating means 15 for strengthening the turning of the powder particles introduced into the collecting member. By strengthening the swirl of the powder particles introduced into the collecting member, the flow in the collecting member is further rectified and at the same time the shear force in the collecting member is improved, so that uniform and united particles are obtained. Fewer powder particles can be obtained.
The powder particle control means may be of any configuration as long as the flow velocity of the powder particles in the collecting member is improved, and as shown in FIG. 2 and FIG.

In the collecting member, the powder particles are preferably cooled by cold water and / or cold air.
When the cooling means is cold water and / or cold air, as shown in FIGS. 2 and 4, the cold air supply means so that the cold air is introduced tangentially to the outer peripheral portion of the collecting member as in the collecting member inlet. Preferably, 16 is provided. The introduction direction of the cold air is preferably the same as the swirling direction of the powder particles. By introducing cold air in the tangential direction to the outer peripheral portion of the collecting member and in the same direction as the swirling direction of the powder particles, the powder particles can be cooled without disturbing the flow in the collecting member. From the viewpoint of rectification in the collecting member, the number of inlets of the collecting member and the number of cold air supply means are preferably the same.

The heat treatment apparatus of the present invention is preferably a heat treatment apparatus for treating powder particles containing a binder resin, a colorant and a release agent.
Moreover, it is a manufacturing method of powder particles which has a heat treatment process which heat-treats powder particles using a heat treatment device, and it is preferred that this heat treatment device is a heat treatment device of the present invention. The powder particles are preferably powder particles for toner.
Next, a procedure for producing a toner using the heat treatment apparatus of the present invention will be described.
First, in the raw material mixing step, a predetermined amount of, for example, a binder resin, a colorant, a mold release agent, etc., as a toner raw material, is weighed, blended, and mixed. Examples of the mixing apparatus include Henschel mixer (manufactured by Nippon Coke Co., Ltd.); super mixer (manufactured by Kawata Co., Ltd.); ribo cone (manufactured by Ogawara Seisakusho Co., Ltd.); Nauta mixer, turbulizer, cyclomix (manufactured by Hosokawa Micron Corp.); Mixer (manufactured by Pacific Kiko Co., Ltd.); Loedige mixer (manufactured by Matsubo Co., Ltd.) and the like.

Further, the mixed toner raw materials are melt-kneaded in a melt-kneading process to melt the binder resin etc. and disperse the colorant etc. therein. As an example of a kneading apparatus, a TEM type extruder (made by Toshiba Machine Co., Ltd.); a TEX twin screw kneader (made by Japan Steel Works Co., Ltd.); a PCM kneader (made by Ikegai Iron Works Co., Ltd.); Among these, continuous kneaders such as single-screw or twin-screw extruders are preferable to batch kneaders because of their advantages such as continuous production.
Furthermore, the colored resin composition obtained by melt-kneading the toner raw material is rolled by a two-roll mill or the like after melt-kneading and cooled through a cooling process of cooling by water cooling or the like.

The cooled product of the colored resin composition obtained above is then ground to a desired particle size in a grinding step. In the pulverizing step, first, coarse pulverization is performed using a crusher, a hammer mill, a feather mill, etc., and then finely pulverized using a Cryptron system (manufactured by Kawasaki Heavy Industries, Ltd.), a superrotor (manufactured by Nisshin Engineering), etc. to obtain toner particles. .
The obtained toner fine particles are classified into powder particles for toner having a desired particle diameter in a classification step. Examples of classifiers include Turboplex, Faculty, TSP, TTSP (manufactured by Hosokawa Micron), Elbow Jet (manufactured by Nittetsu Mining Co., Ltd.), and the like.
Subsequently, in the heat treatment step, the obtained powder particles for toner are spheroidized using the heat treatment apparatus of the present invention.

In the toner manufacturing method, inorganic fine particles and the like may be added to the obtained powder particles for toner prior to the heat treatment step. As a method of adding inorganic fine particles and the like to powder particles for toner, a predetermined amount of powder particles for toner and various known external additives are compounded, and Henschel mixer, mechano hybrid (manufactured by Nippon Coke Co., Ltd.), super mixer, novirta The mixture is stirred and mixed using a high-speed stirrer which exerts a shearing force on the powder (made by Hosokawa Micron) as an external adder.
By adding the inorganic fine powder to the powder particles for toner prior to the heat treatment step, the fluidity is imparted to the powder particles, and the powder particles introduced into the processing chamber are dispersed more uniformly, so that the hot air is heated. The toner can be brought into contact with the toner, and a toner with excellent uniformity can be obtained.

The method for producing a toner may have a step of removing coarse particles by classification if necessary, if coarse particles are present after heat treatment. Examples of classifiers that remove coarse particles include Turboplex, TSP, TTSP (manufactured by Hosokawa Micron Corporation), Elbow Jet (manufactured by Nittetsu Mining Corporation), and the like.
Furthermore, after the heat treatment, in order to sift coarse particles etc. if necessary, for example, ultrasonic (made by Ryoei Sangyo Co., Ltd.); Resonator sieve, Gyro Shifter (Tokuju Works Co., Ltd.); Turbos Cleaner (manufactured by Turbo Kogyo Co., Ltd.) Sieving machine such as Hi-Bolter (manufactured by Toyo High-Tech Co., Ltd.) may be used. The heat treatment step may be performed after the above-mentioned fine pulverization or after classification.

Next, the material of the toner will be described.
A well-known resin is used as a binder resin. For example, styrene, a homopolymer of styrene or a styrene derivative such as polyvinyl toluene; styrene-propylene copolymer, styrene-vinyl toluene copolymer, styrene-vinyl naphthalene copolymer, styrene-methyl acrylate copolymer, Styrene-ethyl acrylate copolymer, styrene-butyl acrylate copolymer, styrene-octyl acrylate copolymer, styrene-dimethylaminoethyl acrylate copolymer, styrene-methyl methacrylate copolymer, styrene-methacryl Ethyl acid copolymer, styrene-butyl methacrylate copolymer, styrene-octyl methacrylate copolymer, styrene-dimethylaminoethyl methacrylate copolymer, styrene-vinyl methyl ether copolymer, styrene-vinyl ethyl ether copolymer Polymer Styrene-vinyl methyl ketone copolymer, styrene-butadiene copolymer, styrene-isoprene copolymer, styrene-maleic acid copolymer, styrene-based copolymer such as styrene-maleic acid ester copolymer; polymethyl Methacrylate, polybutyl methacrylate, polyvinyl acetate, polyethylene, polypropylene, polyvinyl butyral, silicone resin, polyester resin, polyester resin, polyamide resin, epoxy resin, polyacrylic resin, rosin, modified rosin, terpene resin, phenolic resin, aliphatic or alicyclic Hydrocarbon resin and aromatic petroleum resin are mentioned. These resins may be used alone or in combination.
Among these, polymers preferably used as the binder resin are resins having a polyester unit such as a styrene copolymer and a polyester resin.

Examples of the polymerizable monomer used for the styrenic copolymer include the following. For example, styrene; o-methylstyrene, m-methylstyrene, p-methylstyrene, α-methylstyrene, p-phenylstyrene, p-ethylstyrene, 2,4-dimethylstyrene, p-n-butylstyrene, p- tert-Butylstyrene, p-n-hexylstyrene, p-n-octylstyrene, p-n-nonylstyrene, p-n-decylstyrene, p-n-dodecylstyrene, p-methoxystyrene, p-chlorostyrene, Styrene derivatives such as 3,4-dichlorostyrene, m-nitrostyrene, o-nitrostyrene, p-nitrostyrene; unsaturated monoolefins such as ethylene, propylene, butylene and isobutylene; butadiene and isoprene Unsaturated polyenes; vinyl chloride, vinylidene chloride, vinyl bromide, fluoride Halogenated vinyls such as nil; vinyl esters such as vinyl acetate, vinyl propionate and vinyl benzoate; methyl methacrylate, ethyl methacrylate, propyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, methacrylic acid α-Methylene aliphatic monocarboxylic acid esters such as n-octyl, dodecyl methacrylate, 2-ethylhexyl methacrylate, stearyl methacrylate, phenyl methacrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate; methyl acrylate, Ethyl acrylate, propyl acrylate, n-butyl acrylate, isobutyl acrylate, n-octyl acrylate, dodecyl acrylate, 2-ethylhexyl acrylate, stearyl acrylate, acrylic acid -Acrylic esters such as chloroethyl and phenyl acrylate; vinyl ethers such as vinyl methyl ether, vinyl ethyl ether and vinyl isobutyl ether; vinyl ketones such as vinyl methyl ketone, vinyl hexyl ketone and methyl isopropenyl ketone; N N-vinyl compounds such as vinylpyrrole, N-vinylcarbazole, N-vinylindole, N-vinylpyrrolidone; vinyl naphthalenes; acrylic acid or methacrylic acid derivatives such as acrylonitrile, methacrylonitrile, acrylamide.

  Furthermore, unsaturated dibasic acids such as maleic acid, citraconic acid, itaconic acid, alkenylsuccinic acid, fumaric acid and mesaconic acid; maleic anhydride, citraconic anhydride, itaconic anhydride, alkenyl succinic anhydride Such as unsaturated dibasic acid anhydrides; maleate methyl half ester, maleate ethyl half ester, maleate butyl half ester, citraconic acid methyl half ester, citraconic acid ethyl half ester, citraconic acid butyl half ester, itaconic acid methyl half ester Half ester of unsaturated dibasic acid such as ester, alkenyl succinic acid methyl half ester, fumaric acid methyl half ester, mesaconic acid methyl half ester; unsaturated dibasic acid ester such as dimethylmaleic acid and dimethylfumaric acid; acrylic And α, β-unsaturated acids such as methacrylic acid, crotonic acid and cinnamic acid; crotonic acid anhydride, α, β-unsaturated acid anhydrides such as cinnamic acid anhydride, the above α, β-unsaturated acids And anhydrides of lower fatty acids; alkenyl malonic acid, alkenyl glutaric acid, alkenyl adipic acid, acid anhydrides thereof and monomers having a carboxyl group such as monoesters thereof.

  Furthermore, acrylic acid or methacrylic acid esters such as 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, etc .; 4- (1-hydroxy-1-methylbutyl) styrene, 4- (1-hydroxy-1) Examples include monomers having a hydroxy group such as -methylhexyl) styrene.

In the present invention, a resin having a polyester unit is particularly preferably used.
The term "polyester unit" means a portion derived from polyester, and specifically, the components constituting the polyester unit include a dihydric or higher alcohol monomer component, a divalent or higher carboxylic acid, and a divalent or higher carboxylic acid. Examples thereof include acid monomer components such as acid anhydrides and divalent or higher carboxylic acid esters.
The component which comprises these polyester units can be made into a part of raw material, and resin which has a condensation-polymerized site | part can be used.

It is preferable that resin which has a polyester unit is a hybrid resin of polyester and a styrene-type copolymer.
As a method of obtaining a reaction product of polyester and a styrene copolymer, in the presence of a polymer containing a monomer component capable of reacting with each of the polyester and the styrene copolymer, either one or both resins may be used. The method of conducting a polymerization reaction is preferable.
For example, among monomers constituting the polyester, those capable of reacting with a styrenic copolymer include, for example, fumaric acid, maleic acid, citraconic acid, unsaturated dicarboxylic acids such as itaconic acid, or anhydrides thereof. .
Among the monomers constituting the styrenic copolymer, those capable of reacting with the polyester include those having a carboxy group or a hydroxy group such as acrylic acid and methacrylic acid, and acrylic acid or methacrylic esters.
The content of the polyester in the hybrid resin is preferably 50% by mass or more, more preferably 70% by mass or more, and still more preferably 85% by mass or more.

  For example, as a dihydric or higher alcohol monomer component, specifically, as a dihydric alcohol monomer component, polyoxypropylene (2.2) -2,2-bis (4-hydroxyphenyl) propane, polyoxypropylene ( 3.3) -2,2-bis (4-hydroxyphenyl) propane, polyoxyethylene (2.0) -2,2-bis (4-hydroxyphenyl) propane, polyoxypropylene (2.0) -poly Alkylene oxide adducts of bisphenol A such as oxyethylene (2.0) -2,2-bis (4-hydroxyphenyl) propane and polyoxypropylene (6) -2,2-bis (4-hydroxyphenyl) propane; Ethylene glycol, diethylene glycol, triethylene glycol, 1,2-propanediol, 1,3- Lopane diol, 1,4-butanediol, neopentyl glycol, 1,4-butenediol, 1,5-pentanediol, 1,6-hexanediol, 1,4-cyclohexanedimethanol, dipropylene glycol, polyethylene glycol, polypropylene Examples include glycol, polytetramethylene glycol, bisphenol A, hydrogenated bisphenol A and the like.

  Examples of trivalent or higher alcohol monomer components include Sorbit, 1,2,3,6-hexanetetrol, 1,4-sorbitan, pentaerythritol, dipentaerythritol, tripentaerythritol, and 1,2,4-butanetriol. 1,2,5-Pentanetriol, Glycerin, 2-Methylpropanetriol, 2-Methyl-1,2,4-butanetriol, Trimethylolethane, Trimethylolpropane, 1,3,5-Trihydroxymethylbenzene, etc. Can be mentioned.

  Examples of divalent carboxylic acid monomer components include aromatic dicarboxylic acids such as phthalic acid, isophthalic acid and terephthalic acid or anhydrides thereof; alkyl dicarboxylic acids such as succinic acid, adipic acid, sebacic acid and azelaic acid or anhydrides thereof And succinic acid or an anhydride thereof substituted with an alkyl group or an alkenyl group having 6 to 18 carbon atoms; unsaturated dicarboxylic acids such as fumaric acid, maleic acid and citraconic acid or an anhydride thereof.

Examples of trivalent or higher carboxylic acid monomer components include trimellitic acid, pyromellitic acid, benzophenonetetracarboxylic acid and polyvalent carboxylic acids such as anhydrides thereof.
Further, as other monomers, polyhydric alcohols such as oxyalkylene ethers of novolac type phenol resin and the like can be mentioned.

Examples of the colorant include the following.
Examples of the black colorant include carbon black; magnetic materials; yellow colorants, magenta colorants and cyan colorants, which are adjusted to be black.
Examples of color pigments for magenta toners include the following. Examples thereof include condensed azo compounds, diketopyrrolopyrrole compounds, anthraquinone compounds, quinacridone compounds, basic dye lake compounds, naphthol compounds, benzimidazolone compounds, thioindigo compounds and perylene compounds. Specifically, C.I. I. Pigment red 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 21, 22, 22, 23, 30, 31, 32, 37, 38, 39, 40, 41, 48: 2, 48: 3, 48
: 4, 49, 50, 51, 52, 53, 54, 55, 57: 1, 58, 60, 63, 64, 68, 81: 1, 83, 87, 88, 89, 90, 112, 114, 122 123, 144, 146, 150, 163, 166, 169, 177, 184, 185, 202, 206, 207, 209, 220, 221, 238, 254, 269; I. Pigment violet 19, C.I. I. Butt red 1, 2, 10, 13, 15, 23, 29, 35 may be mentioned.
Although a pigment may be used alone as a colorant, it is preferable from the viewpoint of the image quality of a full color image to improve the definition by using a dye and a pigment in combination.

  Examples of the magenta toner dye include the following. C. Solvent Red 1, 3, 8, 23, 24, 25, 27, 30, 49, 81, 82, 83, 84, 100, 109, 121, C.I. I. Disperse thread 9, C.I. I. Solvent Violet 8, 13, 14, 21, 27, C.I. I. Oil-soluble dyes such as Disperse Violet 1, C.I. I. Basic red 1, 2, 9, 12, 13, 14, 15, 17, 18, 22, 23, 24, 27, 29, 32, 34, 35, 36, 37, 38, 39, 40, C.I. I. Basic dyes such as Basic Violet 1, 3, 7, 10, 14, 15, 21, 25, 26, 27, 28 and the like.

  Examples of the color pigment for cyan toner include the following. C. I. Pigment blue 1, 2, 3, 7, 15: 2, 15: 3, 15: 4, 16, 17, 60, 62, 66; I. Bat Blue 6, C.I. I. Acid Blue 45, a copper phthalocyanine pigment having a phthalocyanine skeleton substituted with 1 to 5 phthalimidomethyl.

The following may be mentioned as color pigments for yellow. Condensed azo compounds, isoindolinone compounds, anthraquinone compounds, azo metal compounds, methine compounds, allylamide compounds. Specifically, C.I. I. Pigment yellow 1, 2, 3, 4, 5, 6, 7, 10, 11, 12, 13, 14, 15, 16, 17, 23, 62, 65, 73, 74, 83, 93, 95, 97, 109, 110, 111, 120, 127, 128, 129, 147, 155, 168, 174, 180, 181, 185, 191; I. Bat Yellow 1, 3, 20 can be mentioned.
Also, C.I. I. Direct Green 6, C.I. I. Basic Green 4, C.I. I. Dyes such as Basic Green 6 and Solvent Yellow 162 can also be used.

In the above-mentioned toner, it is preferable to use a binder resin in which a coloring agent is mixed in advance to make a master batch. The colorant can be well dispersed in the toner by melt-kneading this colorant master batch and other raw materials (binder resin, release agent, etc.).
When a coloring agent is mixed with the binder resin to make a master batch, the dispersibility of the coloring agent in the toner is improved even if a large amount of coloring agent is used, and the color reproducibility such as color mixing property and transparency is excellent. In addition, it is possible to obtain toner with a large covering power on the transfer material. In addition, by improving the dispersibility of the colorant, it is possible to obtain an image with excellent durability and excellent image quality of toner chargeability.
The addition amount of the colorant is preferably 0.1 parts by mass or more and 30.0 parts by mass or less, and more preferably 1.0 parts by mass or more and 20.0 parts by mass or less with respect to 100 parts by mass of the binder resin. is there.

The release agent is not particularly limited, and known ones can be used.
Hereinafter, things which can be suitably used will be exemplified. Low molecular weight polyethylene, low molecular weight polypropylene, alkylene copolymer, microcrystalline wax, paraffin wax, aliphatic hydrocarbon wax such as Fischer-Tropsch wax; oxide of aliphatic hydrocarbon wax such as oxidized polyethylene wax; Waxes based on fatty acid esters such as aliphatic hydrocarbon ester waxes; and those obtained by partially or wholly deoxidizing fatty acid esters such as deoxidized carnauba wax. Partially esterified fatty acid and polyhydric alcohol such as behenic acid monoglyceride; methyl ester compound having hydroxyl group obtained by hydrogenating vegetable oil and the like.
Among them, hydrocarbon waxes, in particular aliphatic hydrocarbon waxes, are more preferable because they can prevent a decrease in image density during endurance in a high humidity environment.
The amount of the release agent added is preferably 3.0 parts by mass or more and 20.0 parts by mass or less, and more preferably 3.5 parts by mass or more and 16.0 parts by mass with respect to 100 parts by mass of the binder resin. Part or less.

In the present invention, prior to the heat treatment step, the powder particles for toner may be mixed with a fluidizing agent, a transfer aid, a charge stabilizer, etc. in a mixer such as a Henschel mixer.
Further, as the fluidizing agent, any fluidizing agent can be used as long as the fluidity can be increased by comparing before and after addition. For example, fluorine resin powder such as fine powder of vinylidene fluoride, fine powder of polytetrafluoroethylene, fine powder of titanium oxide, fine powder of alumina, and fine powder of silica such as wet process silica and dry process silica; It is possible to use treated silica surface-treated with organosilicon compounds, titanium coupling agents, and silicone oils.

In the case of titanium oxide fine powder, titanium oxide fine particles obtained by sulfuric acid method, chlorine method, volatile titanium compounds such as titanium alkoxide, titanium halide, titanium acetylacetonate at low temperature (thermal decomposition, hydrolysis) are used. As a crystal system, any of anatase type, rutile type, mixed crystal type of these and amorphous type can be used.
And if it is fine alumina powder, Bayer method, modified buyer method, ethylene chlorohydrin method, spark discharge method in water, organoaluminum hydrolysis method, aluminum alum thermal decomposition method, ammonium aluminum carbonate thermal decomposition method, fire of aluminum chloride Alumina fine powder obtained by the decomposition method is used. As the crystal system, any of α, β, γ, δ, ξ, η, ,, θ, χ, 型 -type, mixed crystal type or amorphous type of these may be used, and α, δ, γ, θ, mixed crystal A type and an amorphous type are preferably used.

More preferably, the surface of the fine powder is hydrophobized by a coupling agent or silicone oil.
The hydrophobization treatment method of the surface of the fine powder is a method of treating the surface of the fine powder chemically or physically with an organosilicon compound or the like which reacts or physically adsorbs with the fine powder.

  A preferable method as the above-mentioned hydrophobization treatment method is a method of treating silica fine particles generated by vapor phase oxidation of a silicon halide compound with an organosilicon compound. Examples of organosilicon compounds used in such methods include: Hexamethyldisilazane, trimethylsilane, trimethylchlorosilane, trimethylethoxysilane, dimethyldichlorosilane, methyltrichlorosilane, allyldimethylchlorosilane, allylphenyldichlorosilane, benzyldimethylchlorosilane, brommethyldimethylchlorosilane, α-chlorosilane Ethyltrichlorosilane, β-chloroethyltrichlorosilane, chloromethyldimethylchlorosilane, triorganosilyl mercaptan, trimethylsilyl mercaptan, triorganosilyl acrylate, vinyldimethylacetoxysilane, dimethylethoxysilane, dimethyldimethoxysilane, diphenyldiethoxysilane, hexamethyl Disiloxane, 1,3-divinyltetramethyldisiloxane, 1,3-diphenyltetramethyldi Siloxane and dimethylpolysiloxane having 2 to 12 siloxane units per molecule, and having one hydroxyl group at each terminal unit, Si.

The fluidizer may be used alone or in combination of two or more.
The fluidizing agent is preferably used in an amount of 0.1 to 8.0 parts by mass, and more preferably 0.1 to 4.0 parts by mass, with respect to 100 parts by mass of powder particles for toner. Favorable fluidity can be imparted to the toner when the addition amount is 0.1 parts by mass or more. When the amount is 4.0 parts by mass or less, mixing of the toner and the inorganic fine powder is easy, and surface modification of the toner is easy. The above additives may be used as an external additive in the external addition step.

Next, methods of measuring various physical properties of the toner and methods of measuring various physical properties measured in the following examples are described below.
<Method of measuring weight average particle diameter (D4)>
The weight average particle diameter (D4) of the toner (powder particles for toner or heat treatment particles for toner) is calculated as follows. As a measuring apparatus, a precise particle size distribution measuring apparatus “Coulter Counter Multisizer 3” (registered trademark, manufactured by Beckman Coulter, Inc.) having a 100 μm aperture tube and using a pore electrical resistance method is used. The setting of measurement conditions and the analysis of measurement data use the attached special software "Beckman Coulter Multisizer 3 Version 3.51" (manufactured by Beckman Coulter, Inc.). The measurement is performed with 25,000 channels of effective measurement channels.
As the electrolytic aqueous solution used for the measurement, a solution in which special grade sodium chloride is dissolved in ion exchange water so that the concentration is about 1% by mass, for example, “ISOTON II” (manufactured by Beckman Coulter, Inc.) can be used.
In addition, before performing measurement and analysis, the dedicated software is set as follows.
In the "Change Standard Measurement Method (SOM)" screen of the special software, set the total count number in the control mode to 50000 particles, set the number of measurements once, and the Kd value "standard particle 10.0 μm" (Beckman Coulter Inc. Make the obtained value. The threshold and noise level are automatically set by pressing the "Threshold / noise level measurement button". Also, set the current to 1600 μA, the gain to 2, and the electrolyte to ISOTON II, and check “Aperture tube flush after measurement”.
In the dedicated software “pulse to particle size conversion setting” screen, set the bin interval to logarithmic particle size, the particle size bin to 256 particle size bins, and the particle size range from 2 μm to 60 μm.

The specific measurement method is as follows.
(1) Place about 200 ml of the electrolytic aqueous solution in a 250 ml round bottom beaker for Multisizer 3 only, set it on a sample stand, and stir the stirrer rod counterclockwise at 24 rotations / second. Then, dirt and air bubbles in the aperture tube are removed by the "flash of aperture tube" function of special software.
(2) About 30 ml of the electrolytic aqueous solution is placed in a 100 ml flat bottom beaker made of glass. Among them, “contaminone N” (nonionic surfactant, anionic surfactant, 10% by weight aqueous solution of neutral detergent for pH 7 precision measuring instrument cleaning consisting of organic builders as a dispersing agent, Wako Pure Chemical Industries, Ltd. Add about 0.3 ml of a diluted solution obtained by diluting about 3 times by mass with deionized water.
(3) Two oscillators with an oscillation frequency of 50 kHz are built in with 180 degrees of phase shift, and an ultrasonic dispersion device "Ultrasonic Dispensation System Tetora 150" (manufactured by Nikkaki Bios Co., Ltd.) having an electrical output of 120 W is prepared. About 3.3 L of deionized water is placed in the water tank of the ultrasonic disperser, and about 2 ml of Contaminone N is added to the water tank.
(4) The beaker of said (2) is set to the beaker fixing hole of the said ultrasonic dispersion device, and an ultrasonic dispersion device is operated. Then, the height position of the beaker is adjusted so that the resonance state of the liquid surface of the electrolytic aqueous solution in the beaker is maximized.
(5) While the electrolytic aqueous solution in the beaker of (4) is irradiated with ultrasonic waves, about 10 mg of toner is added little by little to the electrolytic aqueous solution and dispersed. Then, the ultrasonic dispersion processing is continued for another 60 seconds. In ultrasonic dispersion, the water temperature of the water tank is appropriately adjusted so as to be 10 ° C. or more and 40 ° C. or less.
(6) In the round bottom beaker of (1) placed in the sample stand, the electrolytic aqueous solution of (5) in which the toner is dispersed using a pipette is dropped to adjust the measurement concentration to about 5%. . Then, measurement is performed until the number of measurement particles reaches 50,000.
(7) The measurement data is analyzed by the dedicated software attached to the device to calculate the weight average particle diameter (D4). The “average diameter” on the “analysis / volume statistical value (arithmetic mean)” screen is the weight average particle diameter (D4) when the graph / volume% is set with dedicated software.

<Method of calculating fine powder amount>
The amount of fine powder (number%) on a number basis in the toner (powder particles for toner or heat-treated particles for toner) is calculated by analyzing the data after the measurement of the Multisizer 3 described above.
For example, the number percentage of particles of 4.0 μm or less in the toner is calculated by the following procedure. First, the graph of measurement result is set to graph / number% with dedicated software, and the chart of measurement results is displayed as number%. Then, check "<" of the particle size setting part in the "form / particle size / particle size statistics" screen, and enter "4" in the particle size input part below it. When the “Analysis / number statistics (arithmetic mean)” screen is displayed, the numerical value in the “<4 μm” display area 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 (powder particles for toner or heat-treated particles for toner) is calculated by analyzing the data after the measurement of Multisizer 3 described above.
For example, the volume% of particles of 10.0 μm or more in the toner is calculated by the following procedure. First, the chart of the measurement result is displayed as volume% by setting it to graph / volume% with dedicated software. Then, check ">" of the particle size setting part in the "form / particle size / particle size statistics" screen, and input "10" to the particle size input part below it. When the “Analysis / volume statistics (arithmetic mean)” screen is displayed, the numerical value in the “> 10 μm” display area is the volume percentage of particles of 10.0 μm or more in the toner.

<Method of measuring average circularity>
The average circularity of the toner (powder particles for toner or heat-treated particles for toner) is measured by a flow type particle image analyzer “FPIA-3000” (manufactured by Sysmex Corporation) under measurement and analysis conditions at the time of calibration.
The specific measurement method is as follows. First, about 20 ml of ion exchanged water from which impure solids and the like have been removed in advance is placed in a glass container. Among them, “contaminone N” (nonionic surfactant, anionic surfactant, 10% by weight aqueous solution of neutral detergent for pH 7 precision measuring instrument cleaning consisting of organic builders as a dispersing agent, Wako Pure Chemical Industries, Ltd. Add about 0.2 ml of a diluted solution of about 3 times by volume diluted with deionized water. Further, about 0.02 g of a measurement sample is added, and dispersion treatment is performed for 2 minutes using an ultrasonic dispersion device to obtain a dispersion for measurement. At that time, the dispersion is suitably cooled so that the temperature of the dispersion becomes 10 ° C. or more and 40 ° C. or less. As the ultrasonic wave disperser, a table-top type ultrasonic cleaner disperser ("VS-150" (manufactured by velvocrea)) having an oscillation frequency of 50 kHz and an electric output of 150 W is used. Put in replacement water, and add about 2 ml of the Contaminone N to the water tank.
For measurement, a particle sheath “PSE-900A” (manufactured by Sysmex Corporation) was used as a sheath liquid, using the flow type particle image analyzer equipped with a standard objective lens (10 ×). The dispersion prepared in accordance with the above procedure is introduced into the flow type particle image analyzer, and 3000 toners are measured in the total count mode in the HPF measurement mode. Then, the binarization threshold value at the time of particle analysis is set to 85%, the analysis particle diameter is limited to not less than 1.985 μm and less than 39.69 μm, and the average circularity of the toner is determined.
Before measurement, standard latex particles (Duke Scientifi
c “RESEARCH AND TEST PARTICLES Latex M
Perform auto focusing using icrosphere Suspensions 5200A "(diluted with ion-exchanged water). After that, it is preferable to perform focusing every two hours from the start of measurement.
In the embodiment of the present invention, a flow type particle image analyzer which has been subjected to a calibration work by Sysmex and which has received a calibration certificate issued by Sysmex, is used. The measurement was carried out under the measurement and analysis conditions when proof of calibration was received except that the particle diameter of the analysis particle was limited to the circle equivalent diameter of 1.985 μm or more and less than 39.69 μm.

<Method of calculating the ratio b of particles having a circularity of 0.990 or more>
In the present invention, the proportion b of particles having a degree of circularity of 0.990 or more is used as an index indicating the distribution of the degree of circularity, and is represented by the frequency (%). Further, in the present invention, the ratio b of particles having a circularity of 0.990 or more is used as an index of uniformity of heat-treated powder particles for toner (heat-treated particles for toner).
Specifically, the value of the frequency (%) of the range 1.00 of the frequency table and the value of the frequency (%) of 0.990-> 1.000 in the average circularity of toner measured by FPIA-3000 The added value was used.
For example, in the case of the same degree of circularity, the smaller the value of the proportion b of particles having a degree of circularity of 0.990 or more, the toner with excellent uniformity becomes.
In the present invention, the ratio b of particles having a degree of circularity of 0.990 or more is preferably less than 24.0, and more preferably less than 20.0, from the viewpoint of achieving both transferability and cleaning properties. Preferably, it is more preferably less than 16.0.

  Hereinafter, the present invention will be more specifically described with reference to examples of the present invention, reference examples, and comparative examples, but the present invention is not limited to these examples. In the following formulations, parts are by mass unless otherwise specified.

(Production example of resin having polyester unit)
Polyoxypropylene (2.2) -2,2-bis (4-hydroxyphenyl) propane: 64.7 parts (0.18 mol; 100.0 mol% relative to the total number of moles of polyhydric alcohol)
Terephthalic acid: 24.1 parts (0.15 mol; 96.0 mol% based on the total number of moles of polyvalent carboxylic acid)
-Titanium tetrabutoxide (esterification catalyst): 0.5 parts The above material was weighed in a reaction vessel equipped with a cooling pipe, a stirrer, a nitrogen introducing pipe, and a thermocouple. Next, after the inside of the flask was replaced with nitrogen gas, the temperature was gradually raised while stirring, and reaction was performed for 2 hours while stirring at a temperature of 200 ° C.
Furthermore, the pressure in the reaction vessel was lowered to 8.3 kPa and maintained for 1 hour, then cooled to 180 ° C. and returned to atmospheric pressure (first reaction step).
-Acrylic acid: 0.2 parts-Styrene: 8.2 parts-2-ethylhexyl acrylate: 1.6 parts-Dibutyl peroxide (polymerization initiator): 1.5 parts Then, the above mixture is added by a dropping funnel for 1 hour The solution was added dropwise and maintained for 1 hour (StAcization reaction step).
-Trimellitic anhydride: 1.2 parts (0.01 mol; 4.0 mol% relative to the total number of moles of polyvalent carboxylic acid)
-Tert-butyl catechol (polymerization inhibitor): 0.1 part Then, the above material is added, the pressure in the reaction vessel is lowered to 8.3 kPa, and the reaction is performed for 1 hour while maintaining the temperature at 160 ° C, ASTM D36- After confirming that the softening point measured according to 86 reached the desired temperature of 100 ° C., the temperature was lowered to stop the reaction (second reaction step) to obtain a resin having a polyester unit.

(Production example of powder particle A for toner)
Resin with polyester unit (100 parts)
(Weight average molecular weight (Mw): 82500, average molecular weight (Mn): 3600, peak molecular weight: (Mp) 8400)
Paraffin wax (4 parts)
(Maximum endothermic peak temperature 78 ° C)
3,5-Di-t-butylsalicylic acid aluminum compound (1 part)
C. I. Pigment blue 15: 3 (5 parts)
The materials of the above formulation were mixed with a Henschel mixer FM-75 (manufactured by Nippon Coke Co., Ltd.), and then kneaded by a twin-screw kneader PCM-30 (made by Ikegai Corp.) whose temperature was set at 120 ° C. The obtained kneaded product is cooled, roughly crushed to 1 mm or less by a hammer mill, and made into a crushed product, and the obtained crushed product is crushed by a mechanical grinder T-250 (manufactured by Turbo Kogyo Co., Ltd.) Body fine particles were obtained. Subsequently, the obtained powder fine particles were classified by the Faculty F-300 (manufactured by Hosokawa Micron Corporation) to obtain powder particles.
Furthermore, the following materials are introduced into Henschel mixer FM-75 (manufactured by Nippon Coke Co., Ltd.), the peripheral speed of the rotating blades is 50.0 m / sec, and mixing is performed for 3 minutes, whereby the surface of powder particle A is obtained. Thus, a powder particle for toner to which silica and titanium oxide are attached is obtained.
Powdered particles: 100 parts Silica: 3.5 parts (Silica fine particles prepared by sol-gel method are surface-treated with 1.5% by mass of hexamethyldisilazane treatment, and then adjusted to a desired particle size distribution by classification.)
Titanium oxide: 0.5 parts (surface-treated metatitanic acid having crystallinity of anatase form)
The powder particles for toner obtained at this time have a weight average particle diameter (D4) of 6.7 μm, particles having a particle diameter of 4.0 μm or less are 25.5 number%, and particles having a particle diameter of 10.0 μm or more are It was 2.7% by volume. The average circularity was 0.947.
Hereinafter, this is referred to as powder particle A for toner. The results are shown in Table 1.

(Production example of powder particle B for toner)
Powder particle B for toner was obtained by the same manufacturing method as powder particle A for toner, except that the amount of paraffin wax added was 6 parts.
The weight average particle diameter (D4) of the powder particle B for toner obtained at this time, the ratio of particles having a particle diameter of 4.0 μm or less, the ratio of particles having a particle diameter of 10.0 μm or more, and the average circularity are measured. It is shown in Table 1.

(Production example of powder particle C for toner)
Powder particles C for toner were obtained in the same manner as the powder particles A for toner, except that the amount of paraffin wax added was 8 parts.
The weight average particle diameter (D4) of the powder particle C for toner obtained at this time, the ratio of particles having a particle diameter of 4.0 μm or less, the ratio of particles having a particle diameter of 10.0 μm or more, and the average circularity are measured. It is shown in Table 1.

Example 1
The powder particles A for toner were heat-treated using the heat treatment apparatus shown in FIG. 1 and the collective member shown in FIG.
At this time, the inner diameter of the heat treatment apparatus is 450 mm, and the outer diameter of the restricting means 19 which is a columnar member having a circular cross section is 330 mm.
In addition, the raw material supply means was 8 ports and arranged at equal intervals of 45 ° on the same cross section orthogonal to the central axis of the processing chamber. At this time, the upper end of the outlet of the raw material supply means and the lower end of the swirling member of the hot air were made to be in the same plane.
The injection air flow rate supplied from the high pressure air supply nozzle was 0.45 m ³ / min.
Further, the angle of the substantially conical hot air distribution member 14 of FIG. 2 was 60 °.
Furthermore, using the pivoting member shown in FIG. 3, the minimum gap G between the blades of the pivoting member is 9.5 mm, the height is 30 mm, the number of blades is 22, and the cross-sectional area of the outlet of the hot air supply means is 6270 mm ² .
Cold air was supplied in two stages as shown in FIG. 1, and the first and second cold air supply means were supplied in eight divisions in the tangential direction. The cold air supply means at this time was disposed at equal intervals of 45 ° on the same cross section orthogonal to the central axis of the processing chamber.
Furthermore, eight outlets were provided at the lowermost end of the heat treatment apparatus, and arranged at equal intervals of 45 °.
The device configuration at this time is referred to as device configuration 1.
As shown in FIG. 4, the collecting member used in the present embodiment has eight inlets, and the inlets are arranged so that the swirling direction of the powder particles is the same as the swirling direction in the heat treatment apparatus. Were placed tangentially. The number of cold air supply means of the assembly member was also eight, and was provided tangentially as in the case of the inlet. Further, an inner pipe was provided as a means for controlling the powder particles in the collecting member.
The configuration of the assembly member at this time is referred to as an assembly member configuration 1.

The powder particle A for toner is heat-treated using the above apparatus configuration 1 and the collecting member configuration 1 with the processing amount (kg / h) of the powder particle A for toner set to 150 kg / h. Heat-treated particles for toner were obtained.
The conditions at this time were a hot air temperature of 170 ° C. and a hot air flow rate of 28.0 m ³ / min. In addition, the cold air temperature is set to -5 ° C for both the first cold air and the second cold air, and the flow rate of the first cold air is 8.0 m ³ / min divided into 8 to supply cold air of 1.0 m ³ / min into the processing chamber. did. Similarly, the second cold air was divided into eight sections of 4.0 m ³ / min, and each 0.5 m ³ / min cold air was supplied into the processing chamber.
Further, the cold air temperature of the cold air supply means of the collective member was -5 ° C., 4.0 m ³ / min was divided into eight, and cold air of 0.5 m ³ / min was supplied into the collective member.
The conditions of the hot air temperature at that time, the weight average particle diameter (D4) of the heat-treated particles for toner obtained, the ratio of particles with a particle diameter of 4.0 μm or less, the ratio of particles with a particle diameter of 10.0 μm or more, average circularity The measured results are shown in Table 2.

Next, using the above apparatus configuration 1 and the collecting member 1, the toner powder particles A were heat-treated with the throughput (kg / h) of the powder particles A for toner set to 250 kg / h. Heat treated particles for toner of 965 were obtained.
The conditions at this time were a hot air temperature of 215 ° C. and a hot air flow rate of 28.0 m ³ / min. In addition, the cold air temperature is set to -5 ° C for both the first cold air and the second cold air, and the flow rate of the first cold air is 8.0 m ³ / min divided into 8 to supply cold air of 1.0 m ³ / min into the processing chamber. did. Similarly, the second cold air was divided into eight sections of 4.0 m ³ / min, and each 0.5 m ³ / min cold air was supplied into the processing chamber.
Further, the cold air temperature of the cold air supply means of the collective member was -5 ° C., 4.0 m ³ / min was divided into eight, and cold air of 0.5 m ³ / min was supplied into the collective member.
The conditions of the hot air temperature at this time, the weight average particle diameter (D4) of the obtained heat-treated particles for toner, the ratio of particles having a particle diameter of 4.0 μm or less, the ratio of particles having a particle diameter of 10.0 μm or more, The results of measuring the proportion of particles of 0.990 or more are shown in Table 2.

In addition, the difference Δs (volume) between the ratio of particles having a particle diameter of 10.0 μm or more and the ratio of particles having a particle diameter of 10.0 μm or more of the heat-treated particles when the processing amount is 150 kg / h. %) Was taken as an indicator of the ease of increasing the throughput in the heat treatment apparatus of the present invention. Evaluation was made based on the following criteria.
<Evaluation of ease of increase in throughput>
A: 2.0 <Δs
B: 2.0 ≦ Δs <4.0
C: 4.0 ≦ Δs <6.0
D: 6.0 ≦ Δs <8.0
E: 8.0 ≦ Δs

Further, in this example, the ratio b of particles having a circularity of 0.990 or more was used as an index of the uniformity of the heat-treated powder particles for toner, and evaluation was made according to the following criteria.
<Evaluation of the proportion b of particles having a circularity of 0.990 or more (homogeneity)>
A: b <16.0
B: 16.0 ≦ b <20.0
C: 20.0 ≦ b <24.0
D: 24.0 ≦ b <28.0
E: 28.0 ≦ b

Using the heat treatment apparatus and collecting member of the present invention, the heat treatment apparatus is operated for 1 hour at a processing amount (kg / h) of 250 kg / h to obtain a heat treatment particle for toner having an average circularity of 0.965. The fused state of the bottom of the device was visually confirmed and judged based on the following criteria.
<Evaluation of heat treatment equipment for fusion>
A: No fusion is observed at all B: Almost no fusion is observed at level C: A slight fusion is observed at level D: A fusion is observed at level E: A large fusion is found These results Are summarized in Table 2.

  In this example, the turning in the collecting member is strengthened, and even when the throughput is increased from 150 kg / h to 250 kg / h, the increase in coarse powder is very small. In addition, the ratio b of particles having a degree of circularity of 0.990 or more was also small, and a very uniform heat-treated particle for toner was obtained. Further, the heat-treated toner particles for heat treatment did not stay at the bottom of the device, and there was no fusion.

Example 2
In the present example, a heat treatment was performed and evaluation was performed in the same manner as in Example 1 except that the powder particle for toner was changed to the powder particle B for toner. The results are shown in Table 2.
In this embodiment, the powder particle B for toner having a wax added amount of 6 parts by mass was heat-treated in the same manner as the embodiment 1 using the apparatus configuration 1 of FIG. 1 and the collective member configuration 1 of FIG.
As a result, the temperature at which an average circularity of 0.965 was obtained was slightly increased due to the increase of the added amount of wax, and reached 180 ° C. at 150 kg / h and 225 ° C. at 250 kg / h. In this example, although slightly inferior to Example 1, even when the amount of treatment was increased from 150 kg / h to 250 kg / h, the increase in coarse powder was very small. In addition, the ratio b of particles having a degree of circularity of 0.990 or more was also small, and a very uniform heat-treated particle for toner was obtained. Further, the heat-treated toner particles for heat treatment did not stay at the bottom of the device, and there was no fusion.

[Example 3]
In the present example, a heat treatment was performed and evaluation was performed in the same manner as in Example 1 except that the powder particle for toner was changed to the powder particle C for toner. The results are shown in Table 2.
In this example, the powder particle C for toner having a wax added amount of 8 parts by mass was heat-treated in the same manner as in Example 1 using the device configuration 1 of FIG. 1 and the collective member configuration 1 of FIG.
As a result, the temperature at which an average circularity of 0.965 was obtained was a little higher due to the increase of the added amount of wax, and reached 190 ° C. at 150 kg / h and 235 ° C. at 250 kg / h. In this example, although slightly inferior to Examples 1 and 2, even when the amount of treatment was increased from 150 kg / h to 250 kg / h, the increase in coarse powder was very small. In addition, the ratio b of particles having a degree of circularity of 0.990 or more was also small, and a very uniform heat-treated particle for toner was obtained. Further, the heat-treated toner particles for heat treatment did not stay at the bottom of the device, and there was no fusion.

Example 4
In this embodiment, the powder particles for toner to be heat-treated are the powder particles C for toner, and the heat treatment is carried out in the same manner as in Example 3 using the device constitution 1 of FIG. 1 and the collective member constitution 2 of FIG. And evaluated.
As shown in FIG. 5, in the collective member configuration 2 used in the present embodiment, the number of the inlets is eight, and the inlets are made tangential in the same direction as the swirling direction in the heat treatment apparatus. Provided in The number of cold air supply means of the collecting member was also eight, and was provided tangentially as in the case of the inlet.
The results are shown in Table 2.
In the present embodiment, the powder particles for toner having an added amount of wax of 8 parts by mass were heat-treated in the same manner as in Embodiment 3 using the apparatus configuration 1 of FIG. 1 and the collective member configuration 2 of FIG.
In this embodiment, the inner pipe of the assembly member is eliminated, and the swirling flow in the assembly member is slightly weakened. As a result, the temperature for obtaining an average circularity of 0.965 is 190 ° C. at 150 kg / h and 235 ° C. at 250 kg / h, which is inferior to Example 3, but the throughput is increased from 150 kg / h to 250 kg / h However, the increase in coarse powder was small. In addition, the ratio b of particles having a circularity of 0.990 or more was also small, and uniform heat-treated particles for toner were obtained. Further, at the bottom of the device, fusion of heat-treated heat-treated particles was hardly observed.

[Example 5]
In this embodiment, the powder particles for toner to be heat-treated are the powder particles C for toner, and the heat treatment is carried out in the same manner as in Examples 3 and 4 using the device constitution 1 of FIG. 1 and the collective member constitution 3 of FIG. Carried out and evaluated.
As shown in FIG. 6, in the collective member configuration 3 used in the present embodiment, the number of the inlets is eight, and the inlets are made tangential in the same direction as the turning direction in the heat treatment apparatus. Provided in The results are shown in Table 2.
In the present embodiment, the powder particle C for toner having an added amount of wax of 8 parts by mass was heat-treated in the same manner as in the third and fourth embodiments using the device configuration 1 of FIG. 1 and the collective member configuration 3 of FIG.
In this embodiment, the inner pipe of the collecting member and the cold air cooling mechanism are eliminated, the swirling flow in the collecting member is weakened, and the cooling function is also lost.
As a result, the temperature for obtaining an average circularity of 0.965 is 190 ° C. at 150 kg / h and 235 ° C. at 250 kg / h, which is the same as in Examples 3 and 4, but the coarse powder amount of the obtained heat-treated particles for toner Has increased. As a result, although inferior to Examples 3 and 4, even when the treatment amount was increased from 150 kg / h to 250 kg / h, the increase in coarse powder was small. In addition, the ratio b of particles having a circularity of 0.990 or more was a little small, and a somewhat uniform heat-treated particle for toner was obtained. Furthermore, slight fusion of the heat-treated heat-treated particles was observed at the bottom of the heat-treatment apparatus. This is considered to be the result of the swirling flow of the collecting member affecting the swirling flow in the processing chamber.

[Reference Example 1]
In this reference example, the powder particles for toner to be heat-treated were used as powder particles C for toner, and heat-treatment was carried out using the device configuration 1 of FIG. 1 for evaluation. In this reference example, no collective member was used. The results are shown in Table 2.
In this reference example, the temperature for obtaining an average circularity of 0.965 is 190 ° C. at 150 kg / h and 235 ° C. at 250 kg / h, which is the same as in Examples 3, 4 and 5. However, in this reference example The amount of coarse powder of the obtained heat-treated particles for toner increased. As a result, when the treated amount was increased from 150 kg / h to 250 kg / h, the amount of coarse powder slightly increased. In addition, the ratio b of particles having a degree of circularity of 0.990 or more was somewhat large, and heat-treated particles for toner lacking in uniformity were obtained. Further, fusion of the heat-treated heat-treated particles was observed at the bottom of the heat-treatment apparatus.

Comparative Example 1
In this comparative example, the powder particles for toner to be heat-treated are the powder particles C for toner, and the heat treatment is carried out in the same manner as in Example 5 using the device constitution 1 of FIG. 1 and the collective member constitution 4 of FIG. And evaluated.
In addition, as shown in FIG. 7, the number of inlets was eight and the inlets were provided in the normal direction as shown in FIG. The results are summarized in Table 2.
In this comparative example, the powder particles for toner having a wax content of 8 parts by mass were heat-treated in the same manner as in Example 5 using the apparatus configuration 1 of FIG. 1 and the collective member configuration 4 of FIG.
In this comparative example, the inner pipe of the assembly member and the cold air cooling mechanism are eliminated, and the inlet of the assembly member is in the normal direction as shown in FIG. Therefore, no swirling flow occurs in the collecting member and the cooling function is also lost.
As a result, the temperature for obtaining an average circularity of 0.965 is 190 ° C. at 150 kg / h and 235 ° C. at 250 kg / h, which is the same as in Example 5, but the coarse powder amount of the obtained heat-treated particles for toner is It is more than Example 5. As a result, when the throughput was increased from 150 kg / h to 250 kg / h, the increase in coarse powder resulted in a somewhat large increase. In addition, the ratio b of particles having a degree of circularity of 0.990 or more was somewhat large, and heat-treated particles for toner lacking in uniformity were obtained. Further, fusion of the heat-treated heat-treated particles was observed at the bottom of the heat-treatment apparatus.

Comparative Example 2
In this comparative example, the powder particles for toner to be heat-treated are the powder particles C for toner, and the collecting member configuration 5 in which the number of inlets of the collecting portion of the device configuration 1 of FIG. 1 and FIG. The heat treatment was performed in the same manner as in Example 5 using FIG.
In the collecting member configuration 5 used in the present comparative example, the number of inlets of the collecting member is four, and the inlets are provided in the normal direction. The results are shown in Table 2.
In this comparative example, the powder particle C for toner having an added amount of 8 parts by mass of wax using the assembly member configuration 5 in which the number of inlets of the device configuration 1 of FIG. Was heat treated in the same manner as in Example 5.
In this comparative example, the inner pipe of the assembly member and the cold air cooling mechanism are eliminated, the inlet of the assembly member is in the normal direction as shown in FIG. 7, and the number of the inlets is four. Therefore, no swirling flow occurs in the collecting member and the cooling function is also lost. Furthermore, since the inlet of the collecting member is four, the dust concentration of the heat treatment particles for toner introduced into the collecting member is increased.
As a result, the temperature for obtaining an average circularity of 0.965 is 190 ° C. at 150 kg / h and 235 ° C. at 250 kg / h, which is the same as in Example 5, but the coarse powder amount of the obtained heat-treated particles for toner is It is more than Example 5. As a result, when the throughput was increased from 150 kg / h to 250 kg / h, the increase in coarse powder resulted in a somewhat large increase. In addition, the ratio b of particles having a degree of circularity of 0.990 or more was somewhat large, and heat-treated particles for toner lacking in uniformity were obtained. Further, fusion of the heat-treated heat-treated particles was observed at the bottom of the heat-treatment apparatus.

Comparative Example 3
In this comparative example, the powder particles for toner were made into powder particles C for toner, and heat treatment was carried out and evaluated by the heat treatment apparatus of apparatus configuration 2 shown in FIG.
The heat treatment apparatus configuration of this comparative example is configured such that the exhaust port is straight exhaust, the raw material supply port is one, and the hot air is also supplied straight. No collecting member was used in this comparative example. The results are summarized in Table 2.
In this comparative example, the toner powder particles C with a wax addition amount of 8 parts by mass were thermally treated using the device configuration 2.
In addition, the conditions at this time were 28.0 m ³ / min of hot air volume. In addition, the flow rate of the injection air supplied from the high pressure air supply nozzle was 3.6 m ³ / min, and the toner powder particles C were supplied into the apparatus.
Moreover, in this apparatus configuration, since the inside of the apparatus is cooled by taking in the outside air, cold air was not introduced.
In this comparative example, the temperature for obtaining an average circularity of 0.965 was 250 ° C. at 150 kg / h and 300 ° C. at 250 kg / h, and the amount of coarse particles of the heat-treated toner particles obtained was extremely large. As a result, when the throughput was increased from 150 kg / h to 250 kg / h, the increase of the coarse powder resulted to be very large. In addition, the ratio b of particles having a degree of circularity of 0.990 or more was very large, and non-uniform heat-treated particles for toner were obtained. Furthermore, large fusion of the heat-treated heat-treated particles was observed at the bottom of the heat-treatment apparatus.

Comparative Example 4
In this comparative example, the powder particles for toner were made into powder particles C for toner, and heat treatment was carried out and evaluated by the heat treatment apparatus of the device configuration 3 shown in FIG.
In this apparatus configuration, the exhaust port is a single exhaust port, the raw material supply port is one, the toner powder particles and the hot air are swirled in the same direction and supplied into the apparatus. The cold air is provided with a first cold air which is introduced straight to the wall of the apparatus by providing a slit and a second cold air which is introduced from the tangential direction to cool the outlet. No collecting member was used in this comparative example. The results are shown in Table 2.
In this comparative example, the powder particle C for toner having a wax addition amount of 8 parts by mass was heat-treated using the heat treatment apparatus constitution 3.
In addition, the conditions at this time were 28.0 m ³ / min of hot air volume. In addition, the flow rate of the injection air supplied from the high pressure air supply nozzle was 3.6 m ³ / min, and the toner powder particles C were supplied into the apparatus.
In addition, the cold air supply condition in this device configuration is that the cold air temperature is -5 ° C for both the first cold air and the second cold air, the flow rate of the first cold air is 8.0 m ³ / min, and the flow rate of the second cold air is 4 .0 m ³ / min was supplied into the processing chamber.
In this comparative example, the temperature for obtaining an average circularity of 0.965 was 300.degree. C. at 150 kg / h and 400.degree. C. at 250 kg / h, and the amount of coarse powder of the heat-treated particles for toner obtained was extremely large. As a result, when the throughput was increased from 150 kg / h to 250 kg / h, the increase of the coarse powder resulted to be very large. In addition, the ratio b of particles having a degree of circularity of 0.990 or more was large, and non-uniform heat-treated particles for toner were obtained. Furthermore, large fusion of the heat-treated heat-treated particles was observed at the bottom of the heat-treatment apparatus.

Comparative Example 5
In this comparative example, the powder particles for toner were made into powder particles C for toner, and heat treatment was carried out and evaluated by the heat treatment apparatus of the apparatus configuration 4 shown in FIG.
In the heat treatment apparatus configuration 4 of the present invention, the hot air supply unit and the raw material supply unit of the apparatus configuration 3 of FIG. 9 are modified, and toner powder particles and hot air are swirled in opposite directions and supplied into the apparatus. . Further, as shown in FIG. 10, the relationship between the hot air and the raw material supply unit is such that the hot air is supplied from the inside of the raw material supply unit. No collecting member was used in this comparative example. The results are shown in Table 2.
In this comparative example, the powder particle C for toner having a wax addition amount of 8 parts by mass was heat-treated using the heat treatment apparatus constitution 4.
In addition, the conditions at this time were 28.0 m ³ / min of hot air volume. In addition, the flow rate of the injection air supplied from the high pressure air supply nozzle was 3.6 m ³ / min, and the toner powder particles C were supplied into the apparatus.
In addition, the cold air supply condition in this device configuration is that the cold air temperature is -5 ° C for both the first cold air and the second cold air, the flow rate of the first cold air is 8.0 m ³ / min, and the flow rate of the second cold air is 4 .0 m ³ / min was supplied into the processing chamber.
In this comparative example, the temperature for obtaining an average circularity of 0.965 was 350 ° C. at 150 kg / h and 450 ° C. at 250 kg / h, and the amount of coarse powder of the heat-treated particles for toner obtained was extremely large. As a result, when the throughput was increased from 150 kg / h to 250 kg / h, the increase of the coarse powder resulted to be very large. In addition, the ratio b of particles having a degree of circularity of 0.990 or more was large, and non-uniform heat-treated particles for toner were obtained. Furthermore, large fusion of the heat-treated heat-treated particles was observed at the bottom of the heat-treatment apparatus.

表中、温度は、平均円形度０．９６５の熱処理粒子を得るのに要した温度である。重量平均粒径（Ｄ４）、粒径４．０μｍ以下の粒子の割合、粒径１０．０μｍ以上の粒子の割合、円形度が０．９９０以上の粒子の割合は、平均円形度０．９６５としたときの値である。

In the table, the temperature is the temperature required to obtain heat-treated particles having an average circularity of 0.965. Weight average particle size (D4), proportion of particles with a particle size of 4.0 μm or less, proportion of particles with a particle size of 10.0 μm or more, and proportion of particles with a circularity of 0.990 or more Is the value when

1: treatment chamber in which heat treatment of powder particles is performed, 2: powder particle supply means, 3: hot air supply means, 4: first cold air supply means, 5: outlet, 6: second cold air supply means, 7: Dispersion plate, 8: mesh, 9: powder particle for toner, 10: hot air swirl member, 11: blade of hot air swirl member, 12: slit, 13: conveyance pipe, 14: substantially conical hot air distribution member, 15: Powder particle regulation means of the assembly member, 16: cold air supply means of the assembly member, 17: outlet of the assembly member, 18: inlet of the assembly member, 19: regulation means which is a columnar member having a circular cross section

Claims (6)

A heat treatment apparatus for heat treating powder particles, wherein
The heat treatment apparatus
(1) A cylindrical processing chamber in which the heat treatment of the powder particles is performed,
(2) powder particle supply means for supplying the powder particles to the processing chamber;
(3) hot air supply means for supplying hot air into the processing chamber;
(4) cold air supply means for supplying cold air into the processing chamber;
(5) a plurality of outlets for discharging the heat treated powder particles out of the processing chamber;
(6) A collective member for conveying powder particles discharged from the discharge port while cooling to the collection means;
(7) recovery means for recovering powder particles discharged from the collecting member;
Have
The hot air supply means is provided at the upper end side of the processing chamber, and comprises a pivoting member for spirally swirling the hot air in the processing chamber,
The powder particle supply means is provided at a lower portion of the hot air supply means so as to supply powder particles in the same direction as the swirling direction of the hot air along the inner circumferential surface of the processing chamber,
The cold air supply means is provided at a lower portion of the powder particle supply means so as to supply cold air in the same direction as the swirling direction of the hot air along the inner circumferential surface of the processing chamber,
A plurality of the discharge ports are provided at an outer peripheral portion and a lower end portion of the processing chamber so as to exist on the same cross section orthogonal to the central axis of the cylindrical processing chamber;
The interior of the collecting member has a structure capable of maintaining the turning of the powder particles,
The inlet of the powder particles to the collecting member is provided such that the powder particles are introduced tangentially to the inner circumferential surface of the collecting member,
The number of the inlets is the same as the number of the outlets of the processing chamber, and the inlets and the outlets are connected in a one-to-one manner via a transport pipe.
A heat treatment apparatus characterized in that there is one outlet for discharging the powder particles from the collecting member, and the outlet and the recovery means are connected.   The heat processing apparatus according to claim 1, wherein the collecting member includes powder particle control means for rotating the powder particles supplied into the collecting member.   The heat processing apparatus according to claim 1, wherein the powder particles are cooled by cold water and / or cold air in the collecting member.   4. The cold air supply means according to any one of claims 1 to 3, wherein the collecting member has cold air supply means for introducing cold air in the same direction as the swirling direction of the powder particles and in a tangential direction with respect to the inner peripheral surface of the collecting member. Heat treatment apparatus as described.   It is a heat processing apparatus for processing the powder particle containing binder resin, a coloring agent, and a mold release agent, The heat processing apparatus as described in any one of Claims 1-4. A method for producing powder particles, comprising a heat treatment step of heat treating the powder particles using a heat treatment apparatus,
The manufacturing method of the powder particle whose said heat processing apparatus is a heat processing apparatus as described in any one of Claims 1-5.

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