JP6533432B2 - Heat treatment apparatus for powder particles and method for producing powder particles - Google Patents

Description

  The present invention relates to a heat treatment apparatus for toner and a method for producing toner, which are 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, first, a binder resin for fixing on a transfer material, a coloring agent for giving a color as toner, a wax for improving the releasability between a fixing member and a toner, etc. are mixed. Next, the mixture is melt-kneaded, cooled and solidified to obtain a kneaded product. Further, the obtained kneaded product is refined by a pulverizing unit, and classified into a desired particle size distribution as needed, and then a fluidizing agent or the like is added to obtain a toner to be used for image formation.

In recent years, as the image quality and definition of copiers and printers have become higher, the performance required for toners has become more severe, and the particle size of toner is small and sharp particle size distribution containing no coarse particles with a diameter of 10 μm or more Is becoming required.
Further, as one of the requirements for high image quality, there is gloss uniformity in the image plane. Since the in-plane gloss uniformity of the image is related to the releasability between the fixing member and the toner, a wax is added to the toner in order to improve the gloss uniformity.

Furthermore, it has become necessary to cope with various materials other than ordinary paper as a transfer material for copying machines and printers, and it is also required to improve the transferability of toner. For this reason, it has become necessary to make the powder particle for toner containing wax into a spherical shape.
To meet such requirements, there is a manufacturing method of melting and spheroidizing powder particles for toner by heat treatment. However, when the powder particle for toner containing wax is heat-treated, the wax inside the powder particle is melted and exudes to the surface of the powder particle for toner, thereby increasing the adhesion. As a result, fusion may occur in the heat treatment apparatus, or coarse particles may increase due to coalescence of the melted toners. Therefore, it has been difficult to stably produce the toner.

Conventional techniques for melting and sphericizing powder for toner by heat treatment include heat treatment having a turning mechanism for dispersing powder particles as a raw material and a heating mechanism for heating the dispersed powder raw material from the inside thereof An apparatus has been proposed (see Patent Document 1).
However, when the powder particles for toner are heat-treated with this device configuration, the dispersed gas flow of the raw material and the heating gas flow are in the opposite turning directions. For this reason, if the throughput of the powder particles is increased, the powder particles may collide with each other to cause coalescence and become coarse particles, or the turbulence of the air flow generated in the device causes the powder particles to adhere to the top surface or wall surface of the device. There was a case where a fusion product occurred.
On the other hand, it has been proposed to suppress the adhesion and turbulent flow of powder particles by blowing cooling air from the upper portion of the side wall of the heat treatment chamber of the heat treatment apparatus into a slit shape to improve productivity (see Patent Document 2). .
However, when the powder particles for toner are heat-treated in this device configuration, the dispersed air stream of the raw material and the heating air stream are swirling, while the introduced cooling air is vertical. For this reason, turbulent air flow is also generated in the apparatus, and when heat treatment is performed by increasing the processing amount of the powder particles for toner containing wax, the powder particles may collide with one another and become coarse particles, or The powder particles may be fused in the apparatus. Furthermore, 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 for the spheroidization of the powder particles, and there is a problem that the thermal efficiency is poor.
On the other hand, a heat treatment apparatus has been proposed in which a turning member for turning and supplying hot air is provided in the apparatus (see Patent Document 3). The processing chamber is a double cylindrical shape formed of a cylindrical outer wall and a cylindrical inner member arranged to regulate the volume inside the outer wall, and the turning member is arranged at the upper portion of the processing chamber. The pivoting member has a plurality of blades, controls the pivoting of the hot air, and increases the thermal efficiency to efficiently generate the swirling flow.
However, when the powder particles for toner are heat-treated with this device configuration, the shape of the blade in Patent Document 3 changes the flowing direction of the hot air sharply near the inlet of the blade. As a result, the hot air passing between the blades does not flow smoothly, and a part of the hot air is not used for the heat treatment of the toner and is wasted because it is not wasted. In addition, stagnation of the flow occurs in the vicinity of the cylindrical internal member at the upper portion of the processing chamber, and a roll-up flow toward the direction of the turning member is generated. The rolled up flow is high temperature, and there is a problem that powder particles in a molten state are united and the ratio of coarse particles is increased. At the same time, there is a problem that the powder particles in the molten state are easily fused to the upper wall surface of the cylindrical internal member.
As described above, in the heat treatment apparatus and manufacturing method of toner in which the toner containing wax is spheroidized by heat treatment, there has been room for improvement with regard to the suppression of the fusion of coarse particles and the inside of the apparatus and the improvement of the thermal efficiency.

JP-A-62-133466 JP 59-125742 JP 2013-20245

  It is an object of the present invention to reduce cohesion between coarse particles and in-apparatus and to suppress the amount of heat input even when increasing the processing amount of raw materials when making powder particles for toner containing wax by heat treatment into a spherical shape. It is an object of the present invention to provide a heat treatment apparatus for toner and a method for producing toner.

In the present invention, as a result of earnest studies to solve the problems of the prior art described above, it was found that there is a relationship between the exudation of wax to the surface of powder particles and the supply method of hot air and cold air of a heat treatment apparatus. We came to invent a manufacturing method.
That is, the present invention is a heat treatment apparatus for powder particles containing wax, wherein the heat treatment apparatus comprises
(1) It is formed of the inner peripheral surface of a cylindrical outer wall and the outer peripheral surface of a cylindrical inner member disposed coaxially with the central axis of the outer wall inside the outer wall, and heat treatment of the powder particles A coaxial double cylindrical processing chamber to be performed,
(2) powder particle supply means for supplying the powder particles to the processing chamber;
(3) hot air supply means for supplying hot air for heat-treating the supplied powder particles;
(4) cold air supply means for supplying cold air for cooling the supplied powder particles into the processing chamber;
(5) discharging means for discharging the heat-treated powder particles out of the processing chamber;
(6) A pivoting member for spirally swirling the hot air in the processing chamber,
The pivoting member is
On the top surface of the inner member, at equal distances from the central axis of the inner member, a plurality of blades of the same shape arranged around the central axis,
In a cross section including the blade and orthogonal to the central axis, the angle defined by the straight line connecting the end of the blade closer to the central axis to the central axis and the straight line tangent to the end It is a heat treatment apparatus for powder particles characterized in that the inlet angle a of the blade satisfies the following formula (1).
−10 ° ≦ a ≦ 10 ° Formula (1)

  According to the method for producing a toner of the present invention, when the powder particles for toner containing wax are spheroidized by heat treatment, exudation of wax to the surface of powder particles and generation of coalescent particles and fusion within device Can be produced, and a large amount of sharp toner with small particle size can be produced.

It is a schematic perspective view showing an example of a heat treatment apparatus according to the present invention. It is a schematic sectional drawing in the AA 'plane in FIG. It is a schematic sectional drawing explaining the inlet angle of the braid | blade used for the heat processing apparatus of this invention. Sectional view showing the flow direction when the inlet angle a of the blade is 71 ° Sectional view showing the flow direction when the inlet angle a of the blade is 0 ° It is a schematic sectional drawing explaining the exit angle and perpendicular | vertical exit angle of the braid | blade used for the heat processing apparatus of this invention. Sectional view showing the flow direction when the outlet angle b of the blade is 90 ° and the vertical outlet angle c is 65 ° Sectional view showing the flow direction when the outlet angle b of the blade is 80 ° and the vertical outlet angle c is 77 ° It is a schematic sectional drawing which shows the position of the powder particle supply means used for the heat processing apparatus of this invention. It is a schematic sectional drawing which shows the position of the 1st cold-air supply means used for the heat processing apparatus of this invention. It is a schematic sectional drawing which shows the position of the 2nd cold-air supply means and discharge means which are used for the heat processing apparatus of this invention. It is a schematic sectional drawing of the process chamber upper part used for the heat processing apparatus of this invention. Sectional view showing the direction of flow when the radius of curvature R of the upper end of the double cylindrical member is 0 mm Sectional view showing the direction of flow when the radius of curvature R of the upper end of the double cylindrical member is 7 mm It is a schematic sectional drawing of the heat processing apparatus used for the comparative example 3 of this invention. It is a schematic sectional drawing of the heat processing apparatus used for the comparative example 4 of this invention. It is a schematic sectional drawing of the heat processing apparatus used for the comparative example 5 of this invention.

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.

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 taken along the line A-A 'in FIG.
As shown in FIG. 1 and FIG. 2, the heat treatment apparatus of the present invention has a cylindrical outer wall 1 and a cylindrical shape coaxially arranged with the central axis of the outer wall 1 so as to regulate the volume inside the outer wall 1. It has a coaxial double cylindrical processing chamber 3 formed by the internal member 2 and in which heat treatment of powder particles is performed. The heat treatment apparatus of the present invention further comprises a hot air supply means 4 for supplying hot air to the processing chamber, a powder particle supply means 5 for supplying powder particles, a first cold air supply means 6 for supplying cold air, and a second cold air supply. It has means 7 and discharge means 8 for discharging powder from the processing chamber.

  When the throughput of the outer wall 1 is about 30 kg / hr, the inner peripheral surface diameter T (mm) is preferably 100 mm ≦ T ≦ 300 mm, and more preferably 100 mm ≦ T ≦ 200 mm. If the diameter of the inner peripheral surface of the outer wall 1 is within the above range, the powder particles can be heat-treated efficiently. If the inner circumferential surface diameter T of the outer wall 1 is 100 mm or more, the powder particle concentration in the processing chamber 3 does not become too large, and the amount of processing can be increased. Further, if the inner circumferential surface diameter T is 300 mm or less, the cooling from the wall surface with respect to the volume of the processing chamber is not too strong, and the thermal efficiency does not decrease.

  When the treatment amount is about 250 kg / hr, the inner circumferential diameter T (mm) is preferably 350 mm ≦ T ≦ 900 mm, and more preferably 350 mm ≦ T ≦ 550 mm. If the diameter of the inner peripheral surface of the outer wall 1 is within the above range, the powder particles can be heat-treated efficiently. If the inner peripheral surface diameter T of the outer wall 1 is 350 mm or more, the powder particle concentration in the processing chamber 3 does not become too large, and the amount of processing can be increased. Further, if the inner peripheral surface diameter T of the outer wall 1 is 550 mm or less, the cooling from the wall surface with respect to the volume of the processing chamber is not too strong, and the thermal efficiency does not decrease. Furthermore, if the inner peripheral surface diameter T of the outer wall 1 is 900 mm or less, there is no need 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 manufacturing energy of toner.

  The processing chamber 3 is constituted by the outer wall 1 and the internal member 2. The outer wall 1 and the inner member 2 are preferably cooled by a cooling jacket to prevent fusion of the powder particles. Cooling water (preferably, an antifreeze liquid such as ethylene glycol) is introduced into the cooling jacket, and the surface temperature of the inner surface of the processing chamber is preferably 40 ° C. or less. By setting the surface temperature of the inner surface of the processing chamber to 40 ° C. or less, it is possible to reduce the fusion in the heat treatment apparatus when the powder particles for toner containing wax are heat treated.

  The hot air supply means 4 is provided upstream of the processing chamber 3 and supplies hot air for heat treating the powder particles. The average circularity of the heat-treated powder particles is preferably 0.960 or more, and more preferably 0.965 or more, in order to cope with the improvement of the transferability of the toner required in recent years. Therefore, the temperature N (° C.) at the outlet of the hot air supply means 4 is preferably 100 ° C. ≦ N ≦ 300 ° C. for the hot air supplied into the processing chamber. If N is 100 ° C. or more, the powder particles can be sufficiently sphericized, and if 300 ° C. or less, the powder particles become too hot to cause coalescence of particles or cause fusion within the apparatus. Absent.

The heat treatment apparatus of the present invention also includes a pivoting member 9 for swirling the hot air in a spiral shape.
FIG. 3 is a schematic cross-sectional view for explaining the pivoting member 9.
The pivoting member 9 comprises a plurality of blades 11 of the same shape arranged on the top surface of the inner member 2 at equal distances from the central axis 10 of the inner member, as shown in FIG. .
In a cross section orthogonal to the central axis 10 including the blade,
The straight line connecting the end of the blade closer to the central axis 10 and the central axis 10 is a straight line 12,
When a straight line in contact with the end portion is a straight line 13,
It is characterized in that the inlet angle a of the blade defined by the angle formed by the straight line 12 and the straight line 13 satisfies the following equation (1).
−10 ° ≦ a ≦ 10 ° Formula (1)
FIGS. 4 and 5 show the results of an air flow simulation of the heat treatment apparatus, with the outer peripheral surface diameter of the outer wall 1 being 150 mm and the outer peripheral surface diameter of the internal member 2 being 110 mm.

4 and 5 show the direction of the flow of the hot air in the direction of the arrows in a cross section orthogonal to the central axis of the processing chamber at the height center of the turning member 9, and the magnitude of the velocity of the hot air is the density of the color of the arrow (Range) is shown.
FIG. 4 is a cross-sectional view showing the flow direction when the inlet angle a of the blade is 71 °.
FIG. 5 is a cross-sectional view showing the flow direction when the inlet angle a of the blade is 0 °.
Both hot air flow rates are 3.0 m ³ / min. As can be seen from FIG. 4, when the inlet angle a is large, the flow direction of the hot air changes rapidly near the inlet of the blade 11, so the hot air passing between the blades does not flow smoothly, and vortices are generated in the blade. This leads to a reduction in thermal efficiency. On the other hand, as shown in FIG. 5, when the inlet angle a of the blade is 0 °, the hot air flows smoothly near the inlet of the blade. Therefore, the hot air passing between the blades can be used for the heat treatment of the toner without waste.

Further, when confirmed in an actual machine, it was found that the toner can be heat-treated without significantly increasing the temperature of the hot air if it is in the range of −10 ° ≦ a ≦ 10 °. That is, it was found that within this range, no noticeable decrease in thermal efficiency was observed during heat treatment of the toner.
If the inlet angle a is out of this range, it is necessary to raise the temperature of the hot air to compensate for the decrease in thermal efficiency, and powder particles are likely to be coalesced due to the rise in the hot air temperature.

FIG. 6 is a schematic cross-sectional view illustrating the outlet angle and the vertical outlet angle of the blade used in the heat treatment apparatus of the present invention.
As shown in FIG. 6, in a cross section including the blade 11 and orthogonal to the central axis 10,
A straight line connecting the end of the blade far from the central axis 10 and the central axis 10 is a straight line 14,
When a straight line in contact with the end is taken as the tangent 15,
The outlet angle of the blade defined by the angle between the straight line 14 and the tangent 15 is b.
Further, a straight line connecting an end remote from the central axis 10 of the first blade and the central axis 10 is a straight line 16,
Let a straight line 17 be a straight line passing through the end remote from the central axis 10 of the first blade among the normals of the second blade adjacent to the first blade in the turning direction,
When a straight line passing through the end far from the central axis 10 of the first blade and orthogonal to the straight line 17 is a straight line 18,
Let the vertical exit angle of the blade defined by the angle between straight line 16 and straight line 18 be c.
At this time, in the turning member 9 according to the present invention, it is preferable to satisfy the following formula (2).
0 ° ≦ b−c ≦ 10 ° Formula (2)
FIGS. 7 and 8 show the results of an air flow simulation of the heat treatment apparatus, with the outer peripheral surface diameter of the outer wall 1 being 150 mm and the outer peripheral surface diameter of the inner member 2 being 110 mm.

7 and 8 show the direction of the flow of the hot air in the direction of the arrow in a cross section orthogonal to the central axis of the processing chamber at the height center of the turning member 9, and the magnitude of the velocity of the hot air is the density of the color of the arrow (Range) is shown.
FIG. 7 shows the results when the outlet angle b is 90 ° and the vertical outlet angle c is 65 °, and b−c = 25 °.
FIG. 8 shows the results when the outlet angle b is 80 ° and the vertical outlet angle c is 77 °, and b−c = 3 °. Both hot air flow rates are 3.0 m ³ / min.

  The average value of the circumferential velocity when one of the hot air outlets between the blades 11 was divided into three equal parts was calculated using the simulation result. The calculated positions are shown as a1, a2, a3 in FIG. 7 and as b1, b2, b3 in FIG. The respective calculated values are a1 = 37.0 m / s, a2 = 34.1 m / s, a3 = 25.6 m / s, b1 = 45.8 m / s, b2 = 43.2 m / s, b3 = 37. It became 4 m / s.

  Here, the variation in circumferential velocity at the hot air outlet is calculated using (the circumferential velocity difference between both ends of the blade / the circumferential velocity on the outer side of the blade) using this calculated value. In FIG. 7, (a1−a3) / a1 = (37.0−25.6) / (37.0) = 0.31. On the other hand, in FIG. 8, (b1−b3) / b1 = (45.8−37.4) / (45.8) = 0.18. From this, it can be seen that the blade shape of FIG. 8 has smaller variation in circumferential velocity at the hot air outlet than the blade shape of FIG. 7.

That is, it has been found that when the difference between the outlet angle b of the blade 11 and the vertical outlet angle c is small, the variation in the circumferential velocity of the hot air flowing out of the blade is reduced. Further, as a result of further examination, it was found that the variation is minimized when b−c = 0 °.
When the variation in circumferential velocity of the hot air flowing out of the blade is reduced, sufficient centrifugal force can be applied to the powder particles without bias, and the coalescence of the powder particles can be suppressed. In addition, it was found that the variation in the circumferential velocity should be 0.20 or less in order to keep the unity of the powder particles within the allowable value by comparison with the examination of the actual machine. At that time, the variation is 0.20 when b−c = 10 °, so if 0 ° ≦ b−c ≦ 10 °, sufficient centrifugal force can be given to the powder particles, Coalescence of powder particles can be suppressed within an allowable value.

  The hot air supply means 4 preferably further has a substantially conical distribution member 19. Since the hot air supply means has a substantially conical distribution member, it is possible to eliminate the bias of the hot air supplied to the processing chamber 3 and to eliminate the need to apply an excessive temperature when heat treating the powder particles.

  The powder particle supply means 5 is provided downstream of the hot air supply means 4 so as to be supplied to the inner peripheral surface of the outer wall 1, and the powder particles are conveyed by the carrier gas from a high pressure air supply nozzle (not shown) It is supplied to the processing chamber 3.

FIG. 9 is a schematic cross-sectional view showing the position of powder particle supply means used in the heat treatment apparatus of the present invention.
The powder particle supply means 5 is arranged such that the carrier gas is supplied along the tangent of the inner peripheral surface of the outer wall and in the same direction as the hot air spiral flow in the apparatus as shown in FIG. As a result, the turbulent air flow at the moment when the carrier air flow containing the powder particles enters the processing chamber 3 can be prevented, so the generation of coarse particles can be suppressed.

  A plurality of powder particle supply means 5 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 3. The powder particle concentration per bit can be reduced as the number of divisions of the powder particle supply means increases. Therefore, the temperature of the hot air required for the heat treatment can be reduced according to the number of divisions. When the amount of powder particles processed increases for the same reason, it becomes possible to prevent the generation of coalescent particles.

  The number of divisions of the powder supply means of the heat treatment apparatus of the present invention is preferably between four and eight divisions, more preferably four divisions, for example, when the inner peripheral surface diameter of the outer wall 1 is 150 mm. When the powder supply means is divided into four, it has the greatest effect on the reduction of the temperature of the hot air and the suppression of the generation of coalescent particles. If the number of divisions is four or more, the above-described reduction effect of the powder concentration per one powder particle supplying means and the increase of the processing amount can be expected. If the number of divisions is 8 or less, the outlets of the powder particle supply means are not too close to each other, and the dividedly introduced powder particles do not rejoin in the processing chamber.

  The first cold air supply means 6 and the second cold air supply means 7 are disposed downstream of the powder particle supply means 5 and supply cold air for cooling the powder particles.

FIG. 10 is a schematic cross-sectional view showing the position of the first cold air supply means.
The first cold air supply means 6 is cylindrical so that the supplied cold air is supplied along the inner peripheral surface of the outer wall 1 as shown in FIG. A plurality of the members are provided on the same cross section orthogonal to the central axis of the outer wall of the housing. As a result, it is possible to prevent turbulence at the moment when cold air is introduced into the apparatus, and to suppress the generation of coalescent particles.

A region surrounded by the powder particle supply means 5 and the first cold air supply means 6 below the powder particle supply means 5 and above the first cold air supply means 6 is a heat treatment zone of the powder particles. Therefore, the first cold air supply means 6 may be disposed at a position where the thermal deformation of the powder particles is sufficiently completed.
In the first cold air supply means 6, as the number of divisions increases, the efficiency of cooling the heat-treated powder particles increases. As a result, the uneven cooling of the powder particles is suppressed, and it becomes possible to produce powder particles with uniform circularity. In the example shown in FIG. 10, the number of divisions of the first cold air supply means 6 is four, which is the same as that of the powder particle supply means 5.

FIG. 11 is a schematic cross-sectional view showing the positions of the second cold air supply means and the discharge means.
The second cold air supply means 7 is divided into three as shown in FIG. 11 so that the supplied cold air is supplied along the inner peripheral surface of the outer wall 1 and the inner periphery of the outer wall is maintained so as to maintain the swirling flow in the apparatus. Place at the bottom of the face. This makes it possible to suppress powder particles that stay and fuse to the bottom surface.

The discharging means 8 is disposed at the lower end portion of the inner peripheral surface of the outer wall as shown in FIG. 11, and discharges the heat-treated powder particles out of the processing room. Further, as shown in FIGS. 1 and 2, the discharge means 8 is provided to maintain the swirling direction of the swirling powder particles.
As a result, the centrifugal force applied to the powder particles can be used to rapidly discharge the powder particles to the outside of the apparatus while preventing disturbance of the powder particles, and adhesion to the outer wall 1 and the internal member 2 and fusion are reduced. Ru. A blower (not shown) is provided at the end of the discharge means 8 and is configured to be suctioned and transported by the blower.

  The relationship between the total flow rate QIN of the compressed air, the hot air and the cold air supplied into the heat treatment apparatus and the air flow QOUT drawn by the blower is preferably adjusted to satisfy the relation of QIN ≦ QOUT. If QIN ≦ QOUT, the pressure in the apparatus becomes a negative pressure, so the toner particles in the processing chamber are easily discharged to the outside of the apparatus, and it is possible to prevent the powder particles from receiving excessive heat. As a result, since it is possible to reduce the increase of coalescent particles and the fusion in the apparatus, it is possible to manufacture toner for a long time.

The inner member 2 is disposed coaxially with the outer wall central axis so as to regulate the outer wall 1 and the volume inside the outer wall.
As a result, the processing chamber 3 becomes a coaxial double cylindrical shape, the toner flow velocity is increased, and the dischargeability of powder particles can be improved, and adhesion and fusion in the vicinity of the discharge means 8 and coalescence of powder particles can be achieved. It can be prevented.

FIG. 12 is a schematic cross-sectional view of the upper portion of the processing chamber used in the heat treatment apparatus of the present invention.
As shown in FIG. 12, assuming that the curvature radius of the upper end portion of the inner member 2 is R, the radius of the inner peripheral surface of the outer wall 1 (inner peripheral surface diameter) and the radius of the outer peripheral surface of the inner member 2 (outer peripheral surface diameter) It is preferable to satisfy Formula (3) when the difference (inner and outer cylinder radius difference) is d.
R ≧ 0.1 × d equation (3)
FIGS. 13 and 14 show the results of an air flow simulation of the heat treatment apparatus, wherein the diameter of the inner peripheral surface of the outer wall 1 is 150 mm and the diameter of the outer peripheral surface of the inner member 2 is 110 mm.

FIG. 13 is a cross-sectional view showing the flow direction when the radius of curvature R is 0 mm.
FIG. 14 is a cross-sectional view showing the flow direction when the radius of curvature R is 7 mm.
13 and 14 show the direction of the flow of the hot air in the direction of the arrows in the cross section parallel to the central axis of the processing chamber 3 including the central axis, and the magnitude of the velocity of the hot air is the color density of the arrow (range) It shows by.
FIG. 13 shows the results when the radius of curvature R = 0 mm for the inner and outer cylinder radius difference d = 20 mm, that is, when R / d = 0. FIG. 14 shows the results when the radius of curvature R = 7 mm for the inner and outer cylinder radius difference d = 20 mm, that is, when R / d = 0.35. Both hot air flow rates are 3.0 m ³ / min.

As can be seen from FIG. 13, when the radius of curvature R is 0 mm, the hot air flowing from the turning member 9 to the processing chamber 3 becomes a sharp bend flow, and is directed to the top of the processing chamber and in the vicinity of the internal member 2 in the direction of the turning member A roll up flow occurs.
On the other hand, as shown in FIG. 14, by giving the upper end portion of the cylindrical inner member a curvature, the hot air flows along the roundness of the upper end portion of the cylindrical inner member, and the upper portion of the processing chamber is cylindrical. Winding up flow generated near the inner member is suppressed.
When the flow up is suppressed, fusion to the wall surface of the upper portion of the cylindrical inner member can be reduced. By the way, although the upward flow is also generated at the upper left of FIGS. 13 and 14, since toner does not enter this part, fusion does not occur.

As a result of changing the radius of curvature in an actual machine and repeating studies, it was found that when the radius of curvature R ≧ 0.1 × d, the fusion to the wall surface of the upper portion of the cylindrical internal member can be reduced to a hardly detectable state. In addition, it was found that when the radius of curvature R0.50.5 × d, the fusion could be reduced to a state where it can not be seen at all.
However, when the radius of curvature is increased, the hot air outlet of the turning member 9 extends up and down, the area of the hot air outlet increases, and therefore the hot air velocity may be reduced and the thermal efficiency may be reduced.
Therefore, the curvature radius R is preferably controlled in the following range in consideration of coexistence of reduction of fusion and thermal efficiency.
(0.1 × d) ≦ R <(1.0 × d)

Next, a procedure for producing a toner using the toner particle producing apparatus of the present invention will be described.
[Toner manufacturing procedure]
Raw material mixing process
First, in the raw material mixing step, predetermined amounts of at least a resin and a colorant are weighed and mixed and mixed as toner raw materials. Examples of the mixing apparatus include Henschel mixer (manufactured by Japan Coke Industry Co., Ltd.); super mixer (manufactured by Kawata Co., Ltd.); Ribocon (manufactured by Ogawara Seisakusho Co., Ltd.); Nauta mixer, turbulizer, cyclomix ( Hosokawa Micron Co., Ltd .; Spiral pin mixer (Pacific Kiko Co., Ltd.); Loedige mixer (Matsubo Co., Ltd.) and the like.

Melt-kneading process
Furthermore, the mixed toner raw materials are melt-kneaded in a melt-kneading process to melt the resins, and disperse the colorant and the like therein. Examples of the kneading apparatus include a TEM type extruder (manufactured by Toshiba Machine Co., Ltd.); a TEX twin screw kneader (manufactured by Japan Steel Works Ltd.); a PCM kneader (manufactured by Ikegai Co., Ltd.); Coke Industry Co., Ltd.) and the like. A continuous type mixer such as a single screw or twin screw extruder is preferable to a batch type mixer because of its advantages such as continuous production.
<Cooling process>
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.

<Crushing process>
The cooled product of the colored resin composition obtained above is then ground to a desired particle size in a grinding step. In the crushing step, first, coarse crushing is performed using a crusher, a hammer mill, a feather mill, etc., and further fine crushing using a Cryptron system (manufactured by Kawasaki Heavy Industries, Ltd.), Super Rotor (manufactured by Nisshin Engineering Co., Ltd.), etc. Toner particles are obtained.

<Classification process>
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 separator, TTSP separator (manufactured by Hosokawa Micron Co., Ltd.), and Elbow Jet (manufactured by Nittetsu Mining Co., Ltd.).

<Heat treatment process>
Subsequently, in the heat treatment step, the obtained powder particles for toner are subjected to spheroidizing treatment using the heat treatment apparatus of the present invention.
In the toner manufacturing method of the present invention, inorganic fine particles and the like may be added to the obtained powder particles for toner before the heat treatment step, as needed. As a method of adding inorganic fine particles and the like to powder particles for toner, a high-speed agitator which imparts a shearing force to powder is used as an external additive machine by blending predetermined amounts of powder particles for toner and various known external additives. Stir and mix.
The following high-speed stirrers may be mentioned as high-speed stirrers that apply shear force to powder.
Henschel mixer, mechano hybrid (made by Nippon Coke Industry Co., Ltd.)
Super mixer, Nobilta (manufactured by Hosokawa Micron Corporation), etc.

  In the toner production method of the present invention, the inorganic fine powder is added to the powder particle for toner before the heat treatment step, whereby the powder particle for toner is imparted with fluidity and introduced into the processing chamber It becomes possible for the powder particles for toner to be dispersed more uniformly and to be in contact with the hot air. As a result, toner having excellent uniformity can be obtained.

The method for producing a toner according to the present invention 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 separator, TTSP separator (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 and the like as required, for example, ultrasonic (made by Ryoei Sangyo Co., Ltd.); Resonator Sieve, Gyro Shifter (Tokuju Works Co., Ltd.); It is also possible to use a sieving machine such as Freund Turbo Co., Ltd .; High Bolter (manufactured by Toyo High Tech Co., Ltd.).
The heat treatment step of the present invention may be after the above-mentioned fine pulverization or after classification.

[Toner constituent material]
Next, toner constituent materials used in the method for producing a toner of the present invention will be described.
As the binder resin used in the present invention, known resins are used. For example, polystyrene, homopolymer of styrene derivative such as polyvinyltoluene; styrene-propylene copolymer, styrene-vinyltoluene copolymer, styrene -Vinyl naphthalene copolymer, styrene-methyl acrylate copolymer, styrene-ethyl acrylate copolymer, styrene-butyl acrylate copolymer, styrene-octyl acrylate copolymer, styrene-dimethylaminoethyl methacrylate Copolymer, Styrene-Methyl Methacrylate Copolymer, Styrene-Ethyl Methacrylate Copolymer, Styrene-Butyl Methacrylate Copolymer, Styrene-Octyl Methacrylate Copolymer, Styrene-Dimethylaminoethyl Methacrylate Copolymer , Styrene-vinyl methyl ether Polymer, styrene-vinyl ethyl ether copolymer, styrene-vinyl methyl ketone copolymer, styrene-butadiene copolymer, styrene-isoprene copolymer, styrene-maleic acid copolymer, styrene-maleic acid ester copolymer Styrene copolymers such as coalescing agents; polymethyl methacrylate, polybutyl methacrylate, polyvinyl acetate, polyethylene, polypropylene, polyvinyl butyral, silicone resin, polyester resin, polyamide resin, epoxy resin, polyacrylic resin, rosin, modified rosin, terpene Resin, phenol resin, aliphatic or alicyclic hydrocarbon resin, aromatic petroleum resin may be mentioned, and these resins may be used alone or in combination.
Among these, a polymer preferably used as the binder resin of the present invention is a resin having a styrene copolymer and a polyester unit.

  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, 3,4-Dichlorostyrene, m-nitrostyrene, o-nitrostyrene, styrene and its derivatives such as p-nitrostyrene; unsaturated monoolefins such as ethylene, propylene, butylene and isobutylene; non-butadienes such as butadiene and isoprene Saturated polyenes; vinyl chloride, vinylidene chloride, vinyl bromide, fluorine Vinyl halides such as vinyl; vinyl esters such as vinyl acetate, vinyl propionate, vinyl benzoate; methyl methacrylate, ethyl methacrylate, propyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, n- methacrylate Α-Methylene aliphatic monocarboxylic acid esters such as 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, 2-acrylate acrylate Acrylic acid esters such as role ethyl 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-vinyl pyrrole, N-vinyl compounds such as N-vinylcarbazole, N-vinylindole and N-vinylpyrrolidone; vinyl naphthalenes; acrylic acid or methacrylic acid derivatives such as acrylonitrile, methacrylonitrile and acrylamide.

  Further, unsaturated dibasic acids such as maleic acid, citraconic acid, itaconic acid, alkenylsuccinic acid, fumaric acid and mesaconic acid; such as maleic anhydride, citraconic anhydride, itaconic anhydride, alkenyl succinic anhydride and the like Unsaturated dibasic acid anhydrides; maleic acid methyl half ester, maleic acid ethyl half ester, maleic acid 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 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 acid, methacrylic acid Α, β-unsaturated acids such as hydrofluoric acid, crotonic acid and cinnamic acid; crotonic acid anhydride, α, β-unsaturated acid anhydrides such as cinnamic acid anhydride, the α, β-unsaturated acids and lower fatty acids And monomers thereof having a carboxyl group such as alkenyl malonic acid, alkenyl glutaric acid, alkenyl adipic acid, their acid anhydrides and their monoesters.

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) And monomers having a hydroxy group such as -methylhexyl) styrene.
In the present invention, a resin having a polyester unit is particularly preferably used. The above-mentioned "polyester unit" means a portion derived from polyester, and specifically, the components constituting the polyester unit include an alcohol monomer component having a valence of 2 or more, a carboxylic acid having a valence of 2 or more, and Examples thereof include acid monomer components such as carboxylic acid anhydrides and divalent or higher carboxylic acid esters.

In the toner used in the present invention, a component having these polyester units can be used as a part of the raw material, and a resin having a condensation-polymerized part can be used.
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-propylene glycol, 1, -Propylene glycol, 1,4-butanediol, neopentyl glycol, 1,4-butenediol, 1,5-pentanediol, 1,6-hexanediol, 1,4-cyclohexanedimethanol, dipropylene glycol, polyethylene glycol And polypropylene 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.

As the divalent carboxylic acid monomer component, 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; There may be mentioned succinic acid or an anhydride thereof substituted with an alkyl group or 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 used in the present invention 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, anthraquinones, 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; C.I. 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, copper phthalocyanine pigment in which phthalocyanine skeleton is substituted by 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. Then, the colorant can be well dispersed in the toner by melt-kneading the colorant master batch and other raw materials (binder resin, wax, etc.).
When a colorant is mixed with the binder resin and masterbatched, even if a large amount of colorant is used, the dispersibility of the colorant is not deteriorated and the dispersibility of the colorant in the toner particles is improved, Excellent color reproducibility such as color mixing and transparency. 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.

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 and the like 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, fine powder of wet process silica, fine powder of silica such as dry process silica, silane compounds, organic compounds It is possible to use treated silica that has been surface-treated with a silicon compound, a titanium coupling agent, or silicone oil.

  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 containing a hydroxyl group bonded to Si at each of the terminally located units.
The fluidizer may be used alone or in combination of two or more.

The fluidizing agent is used in an amount of 0.1 to 8.0 parts by mass, preferably 0.1 to 4.0 parts by mass, based on 100 parts by mass of the powder particles for toner. If the addition amount is less than 0.1 parts by mass, the powder particles for toner can not be provided with fluidity, which is not preferable. On the other hand, if it exceeds 4.0 parts by mass, mixing of the powder particles for toner and the inorganic fine powder becomes difficult, which is not preferable in the production of the heat treatment of the powder particles for toner.
The above additives may be used as an external additive in the external addition step.
The methods of measuring the various physical properties of the toner and the methods of measuring the 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 is calculated as follows. As a measuring device, a Coulter Counter Multisizer 3 (registered trademark, manufactured by Beckman Coulter, Inc.), which is a precise particle size distribution measuring device by a pore electrical resistance method equipped with a 100 μm aperture tube, is used. For setting of measurement conditions and analysis of measurement data, attached special software "Beckman Coulter Multisizer 3 Version 3.51" (manufactured by Beckman Coulter, Inc.) is used. The measurement is performed with 25,000 channels of effective measurement channels.
The electrolytic aqueous solution used for the measurement may be a solution in which special grade sodium chloride is dissolved in ion-exchanged water to a concentration of about 1% by mass, for example, "ISOTON II" (manufactured by Beckman Coulter Co., Ltd.) .

Before performing measurement and analysis, the dedicated software settings were made as follows.
In the "Change Standard Measurement Method (SOM)" screen of the dedicated software, set the total count number in the control mode to 50000 particles, set the number of measurements once, and the Kd value "standard particles 10.0 μm" (Beckman Coulter ( The value obtained using the stock company) is set. 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 aqueous electrolytic solution in a 250 mL round bottom beaker for Multisizer 3 dedicated to a glass, set it on a sample stand, and stir the stirrer rod counterclockwise at 24 rotations / sec. Then, dirt and air bubbles in the aperture tube are removed by the "aperture flush" function of special software.

  (2) Place about 30 mL of the aqueous electrolytic solution 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 dispersant, Wako Pure Chemical Industries, Ltd. And about 0.3 mL of a diluted solution obtained by diluting about 3 times by volume with deionized water.

  (3) Prepare two ultrasonic oscillators with an oscillation frequency of 50 kHz with a phase shift of 180 degrees, and prepare an ultrasonic disperser "Ultrasonic Dispersion System Tetora 150" (manufactured by Nikkaki Bios Co., Ltd.) with an electrical output of 120 W . Place about 3.3 l of ion-exchanged water in the water tank of the ultrasonic disperser, and add about 2 mL of Contaminone N into 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 the above (1) placed in the sample stand, the electrolyte aqueous solution of the above (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 when the graph / volume% is set by dedicated software is the weight average particle diameter (D4).

<Method of calculating fine powder amount>
The amount of fine powder (number%) based on the number in the 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 is calculated by analyzing the data after the measurement of the 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 particles is measured by a flow type particle image analyzer "FPIA-3000" (manufactured by Sysmex Corporation) under the measurement and analysis conditions at the time of the calibration operation.
The specific measurement method is as follows. First, about 20 mL of ion-exchanged water from which impure solids and the like have been previously removed 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 dispersant, Wako Pure Chemical Industries, Ltd. 2.) add about 0.2 mL of a diluted solution diluted about 3 times by volume 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 an ultrasonic wave disperser, a table-top type ultrasonic cleaner disperser ("VS-150" (manufactured by VERVOCREEER CORPORATION)) having an oscillation frequency of 50 kHz and an electric output of 150 W is used. Add a fixed amount of ion exchange water, and add about 2 mL of the Contaminone N into the water bath.

  For measurement, a particle sheath “PSE-900A” (manufactured by Sysmex Corp.) was used as a sheath liquid, using the flow type particle image analyzer equipped with a standard objective lens (10 ×). The dispersion adjusted according to the above procedure is introduced into the flow type particle image analyzer, and 3,000 toner particles 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%, and the diameter of an analysis particle is limited to not less than 1.985 μm and less than 39.69 μm, and the average circularity of toner particles is determined.

In the measurement, automatic focusing is performed using standard latex particles (dilution of “RESEARCH AND TEST PARTICLES Latex Microsphere Suspensions 5200A” manufactured by Duke Scientific Inc. with ion-exchanged water) before the start of the measurement. After that, it is preferable to perform focusing every two hours from the start of measurement.
In the embodiment of the present application, a flow type particle image analyzer which has been subjected to a calibration work by Sysmex Corporation and which has received a certificate of calibration issued by Sysmex Corporation 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 analysis was limited to the circle equivalent diameter of 1.985 μm or more and less than 39.69 μm.

<Method of calculating percentage of particles having a circularity of 0.990 or more>
In the present invention, the proportion 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 expressed by frequency (%). 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.

EXAMPLES Hereinafter, the present invention will be more specifically described with reference to examples of the present invention and comparative examples, but the present invention is not limited to these examples.
(Production example of powder particle A for toner)
Resin having polyester unit: 100 parts by mass (weight average molecular weight (Mw): 82450, number average molecular weight (Mn): 3650, peak molecular weight: (Mp) 8550)
Paraffin wax: 4 parts by mass (maximum endothermic peak temperature 78 ° C.)
3,5-di-t-butylsalicylic acid aluminum compound: 1.0 parts by mass C.I. I. Pigment blue 15: 3.5 parts by mass

  The materials of the above formulation are mixed with Henschel mixer FM-75 (manufactured by Nippon Coke Industry Co., Ltd.), and then the temperature is set at 120 ° C. by a twin-screw kneader PCM-30 (manufactured by Ikegai Co., Ltd.) Kneaded. 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 Freund Turbo Co., Ltd.) The powder fine particles were obtained. Subsequently, the obtained powder fine particles were classified by means of Faculty F-300 (manufactured by Hosokawa Micron Corporation) to obtain powder particles.

Furthermore, powder particles are introduced by charging the following materials into a Henschel mixer FM-75 (manufactured by Nippon Coke Industry Co., Ltd.), setting the peripheral speed of the rotating blade to 50.0 m / sec, and mixing for 3 minutes. Toner powder particles were obtained in which silica and titanium oxide were attached to the surface of A.
Powder particles: 100 parts by mass Silica: 3.5 parts by mass (Silica fine particles prepared by the 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 by mass (surface-treated metatitanic acid having crystallinity of anatase form.)

The powder particles for toner obtained at this time have 25.0 number% of particles having a weight average particle diameter (D4) of 6.7 μm and a particle diameter of 4.0 μm or less, and particles having a particle diameter of 10.0 μm or more. It was 2.7% by volume.
Furthermore, as a result of measuring average roundness with FPIA 3000, the average roundness was 0.946.
Hereinafter, this is referred to as powder particle A for toner.
These results are summarized in Table 1.

(Production example of powder particle B for toner)
In this production example, powder particles B for toner were obtained by the same production method as powder particles A for toner except that the amount of paraffin wax added was 6 parts by mass.
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 summarized in Table 1.

(Production example of powder particle C for toner)
In this production example, powder particles C for toner were obtained by the same manufacturing method as the powder particles A for toner except that the amount of paraffin wax added was 8 parts by mass.
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 summarized in Table 1.

Example 1
In the present embodiment, the powder particles A for toner were heat-treated using the heat treatment apparatus shown in FIGS. In the present embodiment, the inner peripheral diameter of the cylindrical outer wall of the device is 150 mm, and the outer peripheral diameter of the cylindrical inner member is 110 mm.
The heat treatment apparatus comprises a pivoting member for pivoting the hot air, the pivoting member comprising a plurality of blades. The vertical height of the blade was 15 mm. The shape of the blade was a shape in which two arcs are connected as shown in FIG.
The inlet angle a shown in FIG. 3 is 0 °, the outlet angle b shown in FIG. 6 is 80 °, and the vertical outlet angle c is 80 °. Therefore, bc = 0. The number of blades was ten.

The powder particle supply means is divided into four as shown in FIG. 9, and the cross section orthogonal to the processing chamber central axis so as to coincide with the angle of helical flow in the main body at 90 ° intervals on the same section orthogonal to the central axis of the processing chamber. In the direction of the lower end of the main body. Powder supply means The vertical length of each outlet was 60 mm, the horizontal length was 4 mm, the outlet cross-sectional area was 240 mm ² , and the total cross-sectional area was 960 mm ² . The flow rate of the carrier gas supplied from the high pressure air supply nozzle was 0.02 m ³ / min for each port.

The cold air supply means comprises first and second two stages as shown in FIG.
The first cold air supply means was divided into four as shown in FIG. 10, and the distance from the lower end of the powder supply means outlet to the upper end of the first cold air supply means was 100 mm. At the same cross section orthogonal to the central axis of the processing chamber, each port is equally spaced by 45 °, and an angle of 27 ° toward the lower end of the main body with respect to the cross section orthogonal to the central axis of the processing chamber to coincide with the angle of helical flow in the main body Placed with. The vertical length of each outlet of the first cold air supply means was 80 mm, the horizontal length was 4 mm, the outlet cross sectional area was 320 mm ² , and the total cross sectional area was 1280 mm ² .

The second cold air supply means was divided into four as shown in FIG. 11, and the second cold air supply means was disposed in parallel at a total of 180 ° at intervals of 90 ° so that the lower end of the second cold air supply means coincides with the bottom. The vertical length of each outlet of the second cold air supply means was 80 mm, the horizontal length was 4 mm, the outlet cross sectional area was 320 mm ² , and the total cross sectional area was 1280 mm ² .
As shown in FIG. 11, the discharge means was disposed parallel to the bottom of the second cold air supply means so that the lower end of the discharge means was aligned with the bottom at the opposite position of the central opening. In addition, the discharge means inlet had a length of 75 mm, a width of 30 mm, and a cross-sectional area of 2250 mm ² .

As shown in FIG. 12, the cylindrical inner member was disposed coaxially with the central axis of the outer wall so as to regulate the volume of the cylindrical outer wall and the inside of the outer wall. The upper end portion of the cylindrical internal member has a radius of curvature R = 10 mm with respect to the inner and outer cylindrical radius difference d = 20 mm of the processing chamber. At this time, R / d = 0.5.
The above device configuration is referred to as device configuration 1.

The powder particle A for toner was heat-treated using the apparatus configuration 1 with the processing amount (kg / hr) of the powder particle A for toner set to 20 kg / hr, to obtain heat-treated particles for toner having an average circularity of 0.965.
<Operating condition 1>
The operating conditions at this time (hereinafter, also described as operating condition 1) were as follows.
The hot air temperature was 170 ° C., and the hot air volume was 7.0 m ³ / min.
The first cold air temperature is -5 ° C., total flow to 0.2 m ³ / min was fed cold air respectively the mouth 0.05 m ³ / min into the processing chamber.
The second cold air temperature is -5 ° C., total flow to 0.15 m ³ / min was fed cold air respectively the mouth 0.05 m ³ / min into the processing chamber.
The operating time was 1 hour.
The condition at this time is operation condition 1.

The heat-treated powder particles for toner obtained at this time were as follows.
The weight average particle size (D4) is 6.8 μm,
24.4 number percent of particles with a particle size of 4.0 μm or less,
3.6% by volume of particles with a particle size of 10.0 μm or more,
There were very few coarse particles.
Moreover, although the fusion | melting condition in the main body was visually confirmed after driving | operation, the fusion thing was not recognized at all.

Next, using the apparatus configuration 1, the powder particle A for toner was heat-treated at a throughput of 30 kg / hr for powder particle A for toner, to obtain heat-treated particles for toner having an average circularity of 0.965.
The conditions at this time were a hot air temperature of 200 ° C. and a hot air volume of 10.0 m ³ / min. The first cold air temperature is -5 ° C., total flow to 0.2 m ³ / min was fed cold air respectively the mouth 0.05 m ³ / min into the processing chamber. Similarly the second cold air temperature is -5 ° C., total flow to 0.15 m ³ / min was fed cold air respectively the mouth 0.05 m ³ / min into the processing chamber.

The heat-treated powder particles for toner obtained at this time were as follows.
Weight average particle diameter (D4) is 6.9 μm,
24.1% by number of particles with a particle size of 4.0 μm or less,
3.9% by volume of particles having a particle size of 10.0 μm or more.
In addition, the increase in volume percentage of particles with a particle size of 10.0 μm or more at 30 kg / hr treatment is 0.3% as compared with 20 kg / hr treatment, and the coarse powder is very high even if the amount of treatment is increased It was too small. Moreover, although the fusion | melting condition in the main body was confirmed after driving | operation, the fusion | fusion thing was not recognized at all.
The evaluation of the heat treatment result of the toner obtained above was performed based on the following criteria.

<Evaluation of coarse powder amount>
The ratio s (volume%) of particles of 10.0 μm or more contained in the obtained powder particles for toner after heat treatment was used as a standard of evaluation of the amount of coarse powder, and was judged based on the following criteria.
A: s <5.0
B: 5.0 ≦ s <10.0
C: 10.0 ≦ s <15.0
D: 15.0 ≦ s <20.0
E: 20.0 s s

<Evaluation of the increase in the amount of coarse powder when the treatment amount is increased>
The difference Δs between the coarse powder ratio (volume%) at the time of 30 kg / hr treatment and the coarse powder ratio (volume%) at the 20 kg / hr treatment is used as an indicator of the easiness of increasing the processing amount in the heat treatment apparatus of the present invention. , Judging based on the following criteria.
A: Δs <2.0
B: 2.0 ≦ Δs <4.0
C: 4.0 ≦ Δs <6.0
D: 6.0 ≦ Δs <8.0
E: 8.0 ≦ Δs

<Evaluation of heat treatment equipment for fusion>
After one hour of operation under the conditions of each example, the supply of powder particles for toner was stopped. Then, insert the scope part of the industrial videoscope “IPLEX SA II R” (Olympus Co., Ltd.) from the side of the heat treatment equipment or the inspection port (not shown) of the powder particle transport route piping, and check the fusion status. , Judging based on the following criteria.
A: Fusing material is not observed at all Level B: Fusing material is slightly found, but no problem in operation C: Fusing is observed, D: No problem in operation D: Fusing is observed, Unable to operate Level E: Large fused material was observed, unable to operate Level These results are summarized in Table 2.

Example 2
In the present example, the powder particle B for toner was processed using the device configuration 1.
The operating condition was the same as the operating condition 1 except that the temperature of the hot air was set to 180 ° C.
As a result, the toner processing amount was 20 kg / hr, and heat-treated particles for toner having an average circularity of 0.965 were obtained. The amount of wax added to the powder particle B for toner was 6 parts by mass, which is more than that of the powder particle A for toner, so the temperature of the hot air for obtaining an average circularity of 0.965 was increased.

Next, using the apparatus configuration 1, the powder particle B for toner was heat-treated at a throughput of 30 kg / hr for powder particle B for toner to obtain heat-treated particles for toner having an average circularity of 0.965.
The operating condition at this time was the same as the operating condition 1 except that the temperature of the hot air was 210 ° C.
The hot air temperature was higher than that of Example 1, but the amount of coarse powder s was very small, which was an evaluation A. In addition, the difference Δs in the amount of coarse powder was very small and the evaluation A, even when the amount of treatment was increased from 20 kg / hr to 30 kg / hr. Further, the heat treatment particles for heat treatment that had been heat treated did not fuse at all inside the device, and the evaluation A was made.
These results are summarized in Table 2.

[Example 3]
In the present embodiment, the powder particle C for toner was heat-treated using the device configuration 1.
The operating condition was the same as the operating condition 1 except that the temperature of the hot air was 190 ° C.
As a result, the toner processing amount was 20 kg / hr, and heat-treated particles for toner having an average circularity of 0.965 were obtained. The powder particle B for toner has a wax added amount increased to 8 parts by mass more than the powder particle B for toner, so the hot air temperature for obtaining an average circularity of 0.965 is high compared to Example 1 and Example 2. became.

Next, similarly, using the apparatus configuration 1, the powder particle B for toner was heat-treated at a processing amount of 30 kg / hr for powder particle C for toner, to obtain heat-treated particles for toner having an average circularity of 0.965.
The operating condition at this time was the same as the operating condition 1 except that the hot air temperature was 220 ° C.
The hot air temperature was higher than that of Example 1, but the amount of coarse powder s was very small, which was an evaluation A. In addition, the difference Δs in the amount of coarse powder was very small and the evaluation A, even when the amount of treatment was increased from 20 kg / hr to 30 kg / hr. Further, there was no fusion of the thermally treated heat-treated particles inside the device, and it was evaluated as A.
These results are summarized in Table 2.

Example 4
In the present embodiment, based on the device configuration 1, the upper end portion of the cylindrical internal member has a radius of curvature R = 2 mm with respect to the inner and outer cylindrical radius difference d = 20 mm of the processing chamber. At this time, R / d = 0.1. The powder particle C for toner was heat-treated with this device constitution as the device constitution 2.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 190 ° C. when the toner processing amount is 20 kg / hr and 220 ° C. when the toner processing amount is 30 kg / hr. As compared to Example 3, the hot air temperature was the same.

The coarse powder amount s was 4.5% by volume at 20 kg / hr, and was 4.9% by volume at 30 kg / hr. For this reason, even if the treated amount was increased from 20 kg / hr to 30 kg / hr, the difference Δs in the amount of coarse powder was 0.4% by volume, which was an evaluation A. Moreover, fusion was hardly seen, and it was evaluation B.
From these results, it was found that when the ratio of the curvature radius R and the inner / outer cylinder radius difference d was R / d = 0.1, fusion could be suppressed although inferior to Example 3.
These results are summarized in Table 2.

[Example 5]
In the present embodiment, based on the device configuration 1, the upper end portion of the cylindrical internal member has a radius of curvature R = 20 mm with respect to the inner and outer cylinder radius difference d = 20 mm of the processing chamber. At this time, R / d = 1. The powder particle C for toner was heat-treated with this device constitution as device constitution 3.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 200 ° C. when the toner processing amount is 20 kg / hr and 230 ° C. when the toner processing amount is 30 kg / hr. Compared to Example 3, a hot air that was 10 ° C. higher was required. It is considered that this is because the area of the hot air outlet of the turning member becomes large due to the increase of the radius of curvature, and therefore the speed of the hot air becomes slow and the thermal efficiency decreases.

The coarse powder amount s was 4.5% by volume at 20 kg / hr, and was 6.0% by volume at 30 kg / hr. Therefore, the difference Δs in the amount of coarse powder when the amount to be treated was increased from 20 kg / hr to 30 kg / hr was 1.5 volume%, which was an evaluation A. There was no adhesion at all, and it was evaluation A.
From these results, it was found that when the ratio of the curvature radius R and the inner / outer cylinder radius difference d is R / d = 1, the fusion can be suppressed although the thermal efficiency is lowered compared to the third embodiment.
These results are summarized in Table 2.

[Example 6]
In the present embodiment, the outer peripheral surface diameter of the cylindrical internal member is set to 90 mm based on the device configuration 1. In addition, the upper end portion of the cylindrical internal member has a radius of curvature R = 3 mm with respect to the inner and outer cylindrical radius difference d = 30 mm of the processing chamber. At this time, R / d = 0.1. The powder particle C for toner was heat-treated with this device constitution as device constitution 4.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 200 ° C. when the toner processing amount is 20 kg / hr and 230 ° C. when the toner processing amount is 30 kg / hr. Compared to Example 3, a hot air that was 10 ° C. higher was required. It is considered that this is because the difference in radius between the inner and outer cylinders is large, so that the velocity of the hot air passing through the processing chamber is slow and the thermal efficiency is lowered.

The coarse powder amount s was 4.5% by volume at 20 kg / hr, and was 5.5% by volume at 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the amount to be treated was increased from 20 kg / hr to 30 kg / hr was 1.0 volume%, which was an evaluation A. Moreover, fusion was hardly seen, and it was evaluation B.
From these results, it was found that fusion could be suppressed as in Example 4 even if the inner / outer cylinder radius difference d was increased if R / d = 0.1.
These results are summarized in Table 2.

[Example 7]
In the present embodiment, the outer peripheral surface diameter of the cylindrical internal member is 130 mm based on the device configuration 1. Further, the upper end portion of the cylindrical internal member has a radius of curvature R = 10 mm with respect to the inner and outer cylindrical radius difference d = 10 mm of the processing chamber. At this time, R / d = 1. The powder particle C for toner was heat-treated with the device constitution as the device constitution 5.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 200 ° C. when the toner processing amount is 20 kg / hr and 230 ° C. when the toner processing amount is 30 kg / hr. Compared to Example 3, a hot air that was 10 ° C. higher was required. It is considered that this is because the area of the hot air outlet of the turning member becomes large due to the increase of the radius of curvature, and therefore the speed of the hot air becomes slow and the thermal efficiency decreases.

The coarse powder amount s was 4.7% by volume at 20 kg / hr, and was 6.5% by volume at 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the amount to be treated was increased from 20 kg / hr to 30 kg / hr was 1.8% by volume, which was an evaluation A. Moreover, there was no fusion at all, and it was evaluation A.
From these results, it was found that fusion can be suppressed as in Example 5 even if R / d = 1, even if the inner and outer cylinder radius difference d is reduced.
These results are summarized in Table 2.

Example 8
In the present embodiment, the upper end portion of the cylindrical internal member on the basis of the apparatus configuration 1 has a curvature radius R of 0 mm with respect to the inner and outer cylindrical radius difference d of 20 mm of the processing chamber. At this time, R / d = 0. The powder particle C for toner was heat-treated with the device constitution as the device constitution 6.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 190 ° C. when the toner processing amount is 20 kg / hr and 220 ° C. when the toner processing amount is 30 kg / hr. As compared to Example 3, the temperature of the hot air was the same.

The coarse powder amount s was 4.7% by volume at 20 kg / hr, and was 6.6% by volume at 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the throughput was increased from 20 kg / hr to 30 kg / hr was 1.9% by volume, which was an evaluation A. With respect to fusion, slight fusion was observed on the upper wall surface of the inner member, which was rated C.
This is because, by setting R / d = 0, an upflow occurs in the upper part of the processing chamber and in the vicinity of the cylindrical internal member.
These results are summarized in Table 2.

[Example 9]
In the present embodiment, based on the device configuration 6, the outlet angle b of the blade of the turning member is 90 °, and the vertical outlet angle c is 80 °. Therefore, it becomes bc = 10 degrees. The powder particle C for toner was heat-treated with this device constitution as device constitution 7.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 190 ° C. when the toner processing amount is 20 kg / hr and 220 ° C. when the toner processing amount is 30 kg / hr. As compared to Example 8, the temperature of the hot air was the same.

The coarse powder amount s was 4.9% by volume at 20 kg / hr, and was 6.8% by volume at 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the throughput was increased from 20 kg / hr to 30 kg / hr was 1.9% by volume, which was an evaluation A. With respect to fusion, slight fusion was observed on the upper wall surface of the inner member, which was rated C.
From these results, it was found that when b−c = 10 °, the coalescence of powder particles during heat treatment was slightly increased.
These results are summarized in Table 2.

[Example 10]
In the present embodiment, based on the device configuration 7, the outlet angle b of the blade of the turning member is 90 °, and the vertical outlet angle c is 79 °. Therefore, bc = 11 °. The powder particle C for toner was heat-treated using the device constitution as the device constitution 8.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 190 ° C. when the toner processing amount is 20 kg / hr and 220 ° C. when the toner processing amount is 30 kg / hr. As compared to Example 9, the hot air temperature was the same.

The coarse powder amount s was 5.0% by volume at 20 kg / hr, and was 7.1% by volume at 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the throughput was increased from 20 kg / hr to 30 kg / hr was 2.1 volume%, which was an evaluation B. With respect to fusion, slight fusion was observed on the upper wall surface of the inner member, which was rated C.
In the simulation, it was confirmed that the variation in circumferential velocity of the hot air flowing out of the blade exceeds the allowable value when bc> 10 °. For this reason, it is considered that the coalescence of the powder particles at the time of the heat treatment is increased and the evaluation of the difference Δs of the coarse powder amount is deteriorated.
These results are summarized in Table 2.

[Example 11]
In the present embodiment, based on the device configuration 8, the inlet angle a of the blade of the pivoting member is 10 °. The powder particle C for toner was heat-treated with the device constitution as the device constitution 9.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is set to 210 ° C. when the toner processing amount is 20 kg / hr and 230 ° C. when the toner processing amount is 30 kg / hr. In comparison with Example 10, a hot air of 20 ° C. higher was necessary at the time of 20 kg / hr treatment, and a hot air of 10 ° C. higher was necessary at the treatment of 30 kg / hr. This is considered to be due to a slight decrease in thermal efficiency because the flow direction of the hot air changes near the inlet of the blade and the hot air passing between the blades does not flow smoothly.

The coarse powder amount s was 5.2% by volume at 20 kg / hr, and was 9.5% by volume at 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the throughput was increased from 20 kg / hr to 30 kg / hr was 4.3 volume%, which was evaluation C. With respect to fusion, slight fusion was observed on the upper wall surface of the inner member, which was rated C.
From these results, it was found that the coalescence of the powder particles during heat treatment slightly increases because the temperature of the hot air rises when a = 10 °.
These results are summarized in Table 2.

[Example 12]
In the present embodiment, based on the device configuration 8, the inlet angle a of the blade of the turning member is set to -10 °. The powder particle C for toner was heat-treated by using this device configuration as a device configuration 10.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is set to 210 ° C. when the toner processing amount is 20 kg / hr and 230 ° C. when the toner processing amount is 30 kg / hr. In comparison with Example 10, a hot air of 20 ° C. higher was necessary at the time of 20 kg / hr treatment, and a hot air of 10 ° C. higher was necessary at the treatment of 30 kg / hr. This is considered to be due to a slight decrease in thermal efficiency because the flow direction of the hot air changes near the inlet of the blade and the hot air passing between the blades does not flow smoothly.

The coarse powder amount s was 5.4% by volume at 20 kg / hr, and was 9.8% by volume at 30 kg / hr. Therefore, the difference Δs in the amount of coarse powder when the throughput was increased from 20 kg / hr to 30 kg / hr was 4.4% by volume, which is an evaluation C. Further, with regard to fusion, slight fusion was observed on the wall surface of the upper portion of the cylindrical internal member, which was rated C.
From these results, it was found that the coalescence of the powder particles during heat treatment slightly increases because the temperature of the hot air rises when a = −10 °.
These results are summarized in Table 2.
Although the above-mentioned present example makes the diameter of the inner skin of the cylindrical outer wall of an apparatus 150 mm, the present invention is not limited to this condition. It is possible to heat-treat more toner powder particles by increasing the inner peripheral diameter.

Comparative Example 1
In this comparative example, the inlet angle a of the blade of the turning member was set to 11 ° based on the device configuration 9. The powder particle C for toner was heat-treated using the device constitution as the device constitution 11.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 220 ° C. when the toner processing amount is 20 kg / hr and 240 ° C. when the toner processing amount is 30 kg / hr. Compared to Example 11, a hot air that was 10 ° C. higher was required. This is considered to be due to a slight decrease in thermal efficiency because the flow direction of the hot air changes near the inlet of the blade and the hot air passing between the blades does not flow smoothly.

The coarse powder amount s was 5.4% by volume at 20 kg / hr, and was 10.0% by volume at 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the throughput was increased from 20 kg / hr to 30 kg / hr was 4.6% by volume, which is an evaluation C. Further, with regard to fusion, slight fusion was observed on the wall surface of the upper portion of the cylindrical internal member, which was rated C.
From these results, it was found that the hot air temperature became high when a> 10 °, and the coalescence of powder particles during heat treatment increased, and the evaluation of the coarse powder amount s deteriorated.
These results are summarized in Table 2.

Comparative Example 2
In the present comparative example, based on the device configuration 10, the inlet angle a of the blade of the turning member is set to -11 °. The powder particle C for toner was heat-treated by using this device configuration as a device configuration 12.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 220 ° C. when the toner processing amount is 20 kg / hr and 240 ° C. when the toner processing amount is 30 kg / hr. As compared to Example 12, a hot air that was 10 ° C. higher was required. This is considered to be due to a slight decrease in thermal efficiency because the flow direction of the hot air changes near the inlet of the blade and the hot air passing between the blades does not flow smoothly.

The coarse powder amount s was 5.6% by volume at 20 kg / hr, and was 10.2% by volume at 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the throughput was increased from 20 kg / hr to 30 kg / hr was 4.6% by volume, which is an evaluation C. Further, with regard to fusion, slight fusion was observed on the wall surface of the upper portion of the cylindrical internal member, which was rated C.
From these results, it was found that the hot air temperature increased when a <-10 °, and the coalescence of powder particles during heat treatment increased, and the evaluation of the coarse powder amount s deteriorated.
These results are summarized in Table 2.

Comparative Example 3
FIG. 15 shows the configuration of the apparatus used in this comparative example. The powder particle C for toner was heat-treated with the constitution of the device as the device constitution 13 to obtain a heat-treated particle for toner having an average circularity of 0.965. In this apparatus, the discharge means 158 has a straight exhaust, the powder supply means 155 has a single bit, and the hot air supply means 154 supplies the hot air straight. The relationship between the total cross-sectional area of the exhaust port of the discharge means 158 and the total cross-sectional area of the outlet (supply port) of the powder supply means 155 at this time is: total cross-sectional area of exhaust port> total cross-sectional area of supply port ing. The toner powder particles supplied from the powder supply means 155 collide with the dispersion plate 151 and are dispersed to the left and right.

  The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 250 ° C. when the toner processing amount is 20 kg / hr and 340 ° C. when the toner processing amount is 30 kg / hr. Further, in the present apparatus configuration, since the inside of the apparatus is cooled by taking in the outside air from the mesh 152, cold air is not introduced. Therefore, the temperature of the hot air rose in comparison with Example 3.

The amount of coarse powder s was 18.3% by volume at the time of 20 kg / hr treatment, and was 27.5% by volume at the treatment of 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the throughput was increased from 20 kg / hr to 30 kg / hr was 9.2 volume%, which was an evaluation E. In addition, regarding fusion, a large level of fusion was found inside the device that causes problems in operation, and it was rated E.
These results are summarized in Table 2.

Comparative Example 4
FIG. 16 shows the configuration of the apparatus used in this comparative example. (A) is the figure which looked at the hot-air supply means 164 and the powder supply means 165 from the top. (B) is sectional drawing which shows schematic structure of the whole apparatus. The powder particle C for toner was heat-treated using the device constitution as the device constitution 14 to obtain a heat-treated particle for toner having an average circularity of 0.965. In this apparatus, the discharge means 168 is a single straight exhaust, the powder supply means 165 is a single hole, and the powder particles for toner supplied from the powder supply means 165 and the hot air supplied from the hot air supply means 164 are reverse. It is configured to be turned and supplied into the apparatus. The cold air supply means is provided with a first cold air supply means 166 introduced straight from the wall of the apparatus by providing the slit 161, and a second cold air supply means 167 introduced tangentially to cool the discharge means 168. It is done.

The differences between the operating condition and the operating condition 1 in the present comparative example are as follows.
Hot air temperature 300 ° C, when toner processing amount is 20kg / hr
400 ° C when the toner processing amount is 30 kg / hr.
Flow rate of cold air supplied from the first cold air supply means 0.2 m ³ / min,
Flow rate of cold air supplied from the second cold air supply means 0.15 m ³ / min.
The temperature of the hot air rose as compared to Example 3.

The coarse powder amount s was 20.0% by volume at the time of 20 kg / hr treatment, was 30.0% by volume at the 30 kg / hr treatment, and was rated E. For this reason, the difference Δs of the amount of coarse powder when the amount to be treated was increased from 20 kg / hr to 30 kg / hr was 10.0 volume%, which was an evaluation E. In addition, regarding fusion, a large level of fusion was found inside the device that causes problems in operation, and it was rated E.
These results are summarized in Table 2.

Comparative Example 5
FIG. 17 shows the configuration of the apparatus used in this comparative example. (A) is the figure which looked at the hot-air supply means 174 and the powder supply means 175 from the top. (B) is sectional drawing which shows schematic structure of the whole apparatus. The powder particle C for toner was heat-treated by using the constitution of the device as the device constitution 15 to obtain a heat-treated particle for toner having an average circularity of 0.965. In the apparatus configuration of this comparative example, the hot air supply means and the powder supply means of the apparatus configuration 14 shown in the comparative example 4 are modified, and the toner powder particles 171 and the hot air are swirled in the same direction and supplied into the apparatus. It is a structure. The relationship between the hot air supply means 174 and the powder supply means 175 is such that hot air is supplied from the outside of the powder supply means 175 as shown in FIG. Further, similar to the device shown in FIG. 16, the device shown in FIG.

The differences between the operating condition and the operating condition 1 in the present comparative example are as follows.
Hot air temperature 350 ° C when the toner processing amount is 20 kg / hr.
Flow rate of cold air supplied from the first cold air supply means 0.2 m ³ / min,
Flow rate of cold air supplied from the second cold air supply means 0.15 m ³ / min.
As compared with Example 3, the temperature of the hot air at 20 kg / hr was increased.

The coarse powder amount s was 20.0% by volume at 20 kg / hr treatment, and at 30 kg / hr treatment, the average circularity of 0.965 could not be obtained even if the hot air temperature was raised to 450 ° C. Therefore, it was not possible to evaluate the coarse powder amount s, the coarse powder amount difference Δs and the fusion.
These results are summarized in Table 2.

[Reference Example 1]
The apparatus configuration used in the present embodiment is configured such that the inlet angle a in the shape of the blade is largely deviated from the range of −10 ° ≦ a ≦ 10 ° based on the device configuration 1, and is 71 °. Furthermore, the upper end portion of the cylindrical internal member has a curvature radius R of 0 mm with respect to the inner and outer cylindrical radius difference d of 20 mm of the processing chamber. At this time, R / d = 0. On the other hand, the outlet angle b of the blade of the turning member was 71 °, and the vertical outlet angle c was 69 °. Therefore, b−c = 2 °. With this apparatus configuration as an apparatus configuration 16, the toner powder particles A were heat-treated to obtain toner heat-treated particles having an average circularity of 0.965.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is set to 200 ° C. when the toner processing amount is 20 kg / hr and 220 ° C. when the toner processing amount is 30 kg / hr. In comparison with Example 1, hot air at a temperature of 30 ° C. was required at the time of 20 kg / hr treatment. Also, at the time of 30 kg / hr treatment, a high temperature of 20 ° C. was required.

The amount of coarse powder s was 5.0% by volume at the time of 20 kg / hr treatment, and 13.0% by volume at the treatment of 30 kg / hr. For this reason, the difference Δs of the amount of coarse powder when the amount to be treated was increased from 20 kg / hr to 30 kg / hr was 8.0 volume%, which was an evaluation E. Further, with regard to fusion, fusion was observed on the wall surface of the upper part of the cylindrical internal member, and it was rated D.
From these results, it is considered that the hot air temperature rises because of a> 10 °, the coalescence of powder particles during heat treatment increases, and the evaluation of the coarse powder amount s and the difference Δs of the coarse powder amount deteriorates. Further, by setting R / d = 0, it is considered that rolling up flow is generated in the upper part of the processing chamber and in the vicinity of the cylindrical internal member, and the evaluation of fusion is deteriorated.
These results are summarized in Table 2.

Reference Example 2
In this reference example, the powder particles C for toner were heat-treated using the device configuration 16 to obtain heat-treated particles for toner having an average circularity of 0.965.
The operating condition is the same as the operating condition 1 except that the temperature of the hot air is 230 ° C. when the toner processing amount is 20 kg / hr and 250 ° C. when the toner processing amount is 30 kg / hr. Compared to Example 3, a hot air at 40 ° C. higher was required at 20 kg / hr treatment. In addition, at the time of 30 kg / hr treatment, a high temperature of 30 ° C. was required.

The amount of coarse powder s was 6.0% by volume at the time of 20 kg / hr treatment and 15.0% by volume at the treatment of 30 kg / hr. Therefore, the difference Δs in the amount of coarse powder when the throughput was increased from 20 kg / hr to 30 kg / hr was 9.0 volume%, which was an evaluation E. Further, with regard to fusion, fusion was observed on the wall surface of the upper part of the cylindrical internal member, and it was rated D.
From these results, it is considered that the evaluation of the coarse powder amount s, the coarse powder amount difference Δs, and the fusion was deteriorated due to the same reason as in Reference Example 1.
These results are summarized in Table 2.

1: Outer wall 2: internal member 3: treatment chamber 4, 154, 164, 174: hot air supply means 5, 155, 165, 175: powder particle supply means 6, 166: first cold air supply means 7, 167: second Cold air supply means 8, 158, 168: Discharge means 9: Hot air swirling member 10: Center axis 11 of cylindrical internal member: Blade 12 of hot air swirling member: Connect the end of the blade closer to the central axis to the central axis Straight line 13: straight line 14 contacting the end of the blade closer to the central axis 14: straight line connecting the end of the blade farther from the central axis to the central axis 15: straight line contacting the end of the blade farther from the central axis 16: A straight line 17 connecting the end of the blade far from the central axis to the central axis 17: the central axis 10 of the first blade among the normals of the first blade and the second blade adjacent on the turning direction side A straight line passing the end far from 8: straight line 19 passing through the end remote from the central axis 10 of the first blade and orthogonal to the straight line 17: substantially conical hot air distribution member 151: dispersing plate 152: mesh 161: slit 171: toner Powder particles

Claims (5)

What is claimed is: 1. A heat treatment apparatus for powder particles containing wax, said heat treatment apparatus comprising
(1) It is formed of the inner peripheral surface of a cylindrical outer wall and the outer peripheral surface of a cylindrical inner member disposed coaxially with the central axis of the outer wall inside the outer wall, and heat treatment of the powder particles Coaxial double cylindrical processing chamber to be performed,
(2) powder particle supply means for supplying the powder particles to the processing chamber;
(3) hot air supply means for supplying hot air for heat-treating the supplied powder particles;
(4) cold air supply means for supplying cold air for cooling the supplied powder particles into the processing chamber;
(5) discharging means for discharging the heat-treated powder particles out of the processing chamber;
(6) A pivoting member for spirally swirling the hot air in the processing chamber,
The pivoting member is
On the top surface of the inner member, at equal distances from the central axis of the inner member, a plurality of blades of the same shape arranged around the central axis,
In a cross section including the blade and orthogonal to the central axis, the angle defined by the straight line connecting the end of the blade closer to the central axis to the central axis and the straight line tangent to the end An apparatus for heat treating powder particles, wherein the inlet angle a of the blade satisfies the following formula (1).
−10 ° ≦ a ≦ 10 ° Formula (1) In a cross section including the blade and orthogonal to the central axis,
A straight line connecting the end of the blade far from the central axis and the central axis is a 1-1th straight line,
When the straight line in contact with the end portion is the 1-2nd straight line,
Let b be the outlet angle of the blade defined by the angle between the 1-1st straight line and the 1-2nd straight line, b
A straight line connecting an end of the first blade far from the central axis and the central axis is a 2-1th straight line,
A straight line passing through the end of the first blade which is farther from the central axis of the first blade among the normals of the first blade and the second blade adjacent to the turning direction is a second 2-2 straight line;
When a straight line passing through the end far from the central axis 10 of the first blade and orthogonal to the 2-2 straight line is the 2-3 straight line,
The heat processing apparatus according to claim 1, wherein the following equation (2) is satisfied, where c represents the vertical exit angle of the blade defined by the angle formed by the 2-1 straight line and the 2-3 straight line.
0 ° ≦ b−c ≦ 10 ° Formula (2) The radius of curvature of the upper end of the inner member is R,
When the difference between the radius of the inner circumferential surface of the outer wall (inner circumferential diameter) and the radius of the outer circumferential surface of the inner member (diameter of the outer circumferential surface) (difference between inner and outer cylindrical radii) is d, the following equation (3) is given The heat processing apparatus of Claim 1 or 2 to satisfy | fill.
R ≧ 0.1 × d equation (3)   The heat treatment apparatus according to any one of claims 1 to 3, wherein the powder particles further contain a binder resin and a colorant. A method for producing a toner, which is to obtain a toner through a heat treatment step of heat treating powder particles containing a binder resin and a colorant using a heat treatment apparatus,
A method for producing a toner, wherein the heat treatment apparatus is a heat treatment apparatus for powder particles according to any one of claims 1 to 4.