JP6516420B2 - 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 powder particles and a method for producing powder particles that are suitable for toners used in image forming methods 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 of the pulverizing method, first, a binder resin for fixing on a transfer material, a coloring agent for giving a color as a toner, a raw material such as wax for improving the releasability between a fixing member and a toner Mix. Next, these mixtures are melt-kneaded, cooled and solidified to obtain a kneaded product. Further, the obtained kneaded product is refined by a pulverizing means, and if necessary, it is classified into a desired particle size distribution, and then a fluidizing agent or the like is added to obtain a toner to be provided for image formation.

  In recent years, as the image quality and definition of copiers and printers have become higher, the performance required for toners has become more severe, the particle size of the toner is smaller, and the particle size distribution of the toner is a particle size distribution that does not contain coarse particles. The uniform toner has come to be required.

  Also, one of the requirements for high image quality is the in-plane gloss uniformity of the image. 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 in-plane gloss uniformity of the image.

  Furthermore, as a transfer material for copying machines and printers, it has become necessary to cope with various materials other than ordinary paper, and improvement of the transferability of toner is also required.

  For this reason, it has become necessary to make the powder particle for toner containing wax into a spherical shape.

  To meet such requirements, a method of melting and powderizing the toner powder by heat treatment is mentioned as one of the manufacturing methods of making the toner spherical.

  However, when the powder particles for toner containing wax are heat-treated, the wax present inside the powder particles may melt and leak out to the surface, which may cause contamination of developing members of copying machines and printers. Also, when the wax exudes to the surface, the adhesion of the powder particles is increased, and fusion occurs in the heat treatment apparatus, and it may be difficult to stably produce a toner containing no coarse particles. is there.

  Conventional techniques for melting and spheroidizing powder for toner by heat treatment include a swirling mechanism for dispersing powder particles which are raw materials, and a heating mechanism for heating the dispersed powder raw materials from the inside thereof A heat treatment 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 heated gas flow are in the opposite turning directions. For this reason, when the throughput of powder particles is increased, the powder particles may adhere to the top surface or wall surface of the device due to the turbulence of the air flow generated in the device, and a fused material may be generated.

  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 with 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 if heat treatment is performed with an increase in the processing amount, fusion of powder particles may occur. Furthermore, in this device configuration, the heating air flow is cooled by the dispersed air flow of the raw material, so it is necessary to apply an amount of heat more than necessary for the spheroidization of the powder particles. For this reason, if heat treatment is performed with an increase in the processing amount of powder particles for toner containing wax, fusion occurs in the device, and it becomes difficult to stably produce a small particle diameter and sharp toner. There was a case.

  On the other hand, a cylindrical processing chamber in which heat treatment of powder particles is performed, hot air supply means for supplying hot air for heat treatment of powder particles, and powder particle supply means for supplying powder particles And cold air supply means for supplying cold air for cooling the heat treated powder particles, and the injection direction of the powder particles injected from the powder particle supply means outlet can be jetted in any direction A heat treatment apparatus has been proposed which is provided with an adjustment mechanism so that cold air is supplied along the inner circumferential surface of the processing chamber in the same direction as the swirling direction of the hot air (see Patent Document 3).

  However, when heat treating the toner with this device configuration, the direction of rotation of the hot air that descends while rotating in the device and the direction of rotation of the cold air for cooling the powder particles are the same, but while rotating in the device There is an angle between the moving direction determined by the falling hot air, the carrier gas of the powder particles, and the introducing direction of the cold air for cooling the powder particles, and the number of introduced materials and the number of introduced cold air differ. Therefore, if the processing amount of the powder particles for toner containing wax is increased and the temperature of the hot air is raised, the powder particles in the molten state collide and unite due to the turbulence of the air flow generated in the apparatus. The proportion of coarse particles increases.

  As described above, when the toner containing wax is spheroidized by heat treatment, it is possible to suppress the exudation of the wax to the powder particle surface and the fusion within the apparatus, and the toner having a uniform shape without containing coarse particles. There is room for improvement in the heat treatment apparatus and manufacturing method of the toner which are produced in large quantities efficiently and stably.

  In the present invention, coarse particles in the toner mean a particle group having a particle size of 10 μm or more.

Japanese Patent Application Laid-Open No. 62-133466 JP-A-59-125742 JP, 2013-3181, A

  The object of the present invention is to solve the above-mentioned problems and suppress the exudation of the wax to the powder particle surface even when the powder particle for toner containing wax is spheroidized by heat treatment, and the fusion in the apparatus It is an object of the present invention to provide a method of producing a toner that can reduce the

  Furthermore, another object of the present invention is that, when the powder particle for toner containing wax is spheroidized by heat treatment, even if the throughput of the powder particle is increased, it does not contain coarse particles, and the shape is An object of the present invention is to provide a toner manufacturing method capable of efficiently manufacturing uniform 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 heat treating powder particles,
The heat treatment apparatus
(1) A processing chamber having a cylindrical inner peripheral surface on which the heat treatment of the powder particles is performed,
(2) powder particle supply means for supplying the powder particles by a carrier gas for transporting 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 heat-treated powder particles;
(5) Control means provided in the processing chamber for controlling the flow of the hot air and the supplied powder particles;
(6) an outlet for discharging the heat-treated powder particles out of the processing chamber;
The hot air supply means comprises a turning member for adjusting the turning speed and the lowering speed of the hot air,
The restricting means is provided on the central axis of the cylindrical processing chamber so as to restrict the descending speed of the hot air or a mixed gas composed of the hot air and the powder particles and the carrier gas. And a columnar member having a circular cross section, which is disposed so as to protrude toward the end portion of the raw material supply means,
The outlet of the hot air supply means is provided opposite to the end of the regulation means on the side of the raw material supply means,
The powder particle supply means is provided at the outer peripheral portion of the processing chamber, and is introduced into the processing chamber from a cross section orthogonal to the central axis of the cylindrical processing chamber and the powder particle supply means outlet. When an angle formed by the introduction direction of the powder particles is α (°), the angle α (°) is
17 (°) ≦ α ≦ 37 (°)
Means for supplying the powder particles into the processing chamber so as to satisfy the condition and to rotate in the same direction as the hot air ,
The cold air supply means is provided on the outer periphery of the treatment chamber, and has a cross section orthogonal to the central axis of the cylindrical treatment room, and introduction of the cold air introduced into the treatment room from the cold air supply means outlet. When the angle formed by the direction is β (°), the angle β (°) is
17 (°) ≦ β ≦ 37 (°)
And means for supplying the cold air so as to turn in the same direction as the mixed gas .

  According to the toner manufacturing method of the present invention, when the powder particles for toner containing wax are spheroidized by heat treatment, the exudation of wax to the surface of the powder particles and the fusion within the apparatus are suppressed, and small particles are produced. A large amount of sharp diameter toner can be manufactured.

It 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 of FIG. 1 along the A-A ′ plane. It is a turning member for turning hot air spirally, which is used in the heat treatment apparatus of the present invention. It is a schematic sectional drawing of a substantially conical-shaped hot-air distribution member used for the heat processing apparatus of this invention. It is a schematic sectional drawing which shows the powder supply means position used for the heat processing apparatus of this invention. It is the schematic for demonstrating the powder particle introduction direction of this invention. It is the schematic for demonstrating the cold wind introduction | transduction direction of this invention. 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 hot air of the heat processing apparatus used for the comparative example 4 of this invention, and a raw material supply part. It is a schematic sectional drawing which shows the cold-air supply means position used for the heat processing apparatus of this invention.

The heat treatment apparatus of the present invention is
A processing chamber having a cylindrical inner peripheral surface on which the heat treatment of the powder particles is performed;
Powder particle supply means for supplying the powder particles by a carrier gas for conveying the powder particles to the processing chamber;
Hot air supply means for supplying hot air for heat treatment of the supplied powder particles;
Cold air supply means for supplying cold air for cooling the heat-treated powder particles;
Regulating means provided in the processing chamber for regulating the flow of the hot air and the supplied powder particles;
And an outlet for discharging the heat-treated powder particles out of the processing chamber,
The hot air supply means comprises a turning member for adjusting the turning speed and the lowering speed of the hot air,
The restricting means is provided on the central axis of the cylindrical processing chamber so as to restrict the descending speed of the hot air or a mixed gas composed of the hot air and the powder particles and the carrier gas. And a columnar member having a circular cross section, which is disposed so as to protrude toward the end portion of the raw material supply means,
The powder particle supply means has an angle α (°) formed by a cross section orthogonal to the central axis of the cylindrical processing chamber and the introduction direction of the powder particles introduced from the powder particle supply means outlet. But,
17 (°) ≦ α ≦ 37 (°)
The cold air supply means has an angle .beta. (.Degree.) Formed by a section orthogonal to the central axis of the cylindrical processing chamber and the direction of introduction of the cold air introduced from the cold air supply means outlet,
17 (°) ≦ β ≦ 37 (°)
The basic composition is to satisfy the

  Hereinafter, the present invention having the above-described configuration 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 FIG. 1, FIG. 2, FIG. 3, FIG.

  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. Further, FIG. 3 is a pivoting member for spirally swirling the hot air used in the heat treatment apparatus of the present invention. Furthermore, FIG. 4 is a schematic cross-sectional view of a substantially conical hot air distribution member used in the heat treatment apparatus of the present invention. Furthermore, FIG. 5 is a schematic cross-sectional view showing the number of inlets of the powder supply means used in the heat treatment apparatus of the present invention. FIG. 6 is a schematic view for explaining the powder particles introduced from the powder particle supplying means used in the heat treatment apparatus of the present invention and the introduction direction of the carrier fluid. FIG. 7 is a schematic view illustrating the introduction direction of cold air introduced from the cold air supply means used in the heat treatment apparatus of the present invention.

  As shown in FIG. 1 and FIG. 2, the heat treatment apparatus of the present invention comprises a treatment chamber 1, powder particle supply means 2, hot air supply means 3, cold air supply means 4, restriction means 5, and an outlet. Have six.

  In the heat treatment apparatus of the present invention, the shape of the processing chamber 1 may be a cylindrical shape, but the inner diameter T (mm) of the processing chamber is preferably 250 (mm) ≦ T ≦ 900 (mm). If the inner diameter of the processing chamber is within the above range, heat treatment particles can be efficiently produced. When the inner diameter T (mm) of the processing chamber is T <250 (mm), the dust concentration of the powder particles in the processing chamber may be increased, and the processing amount of the powder particles may not be increased. When 900 (mm) <T, it is necessary to increase the size of the ancillary equipment of the heat treatment apparatus such as a blower, a heater, and a cold air generator, which may be undesirable in terms of the energy for producing the toner.

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

  Hot air for heat treating powder particles in the heat treatment apparatus of the present invention is supplied from the hot air supply means 3.

  In order to cope with the improvement of the transferability of toner required in recent years, the average circularity of heat-treated powder particles for toner is preferably 0.960 or more, more preferably 0.965 or more. Is required.

  Therefore, the temperature N (° C.) at the outlet of the hot air supply means 3 is preferably 100 (° C.) ≦ N ≦ 300 (° C.) in the hot air supplied into the processing chamber. If the temperature at the outlet of the hot air supply means is within the above range, powder particles are uniformly spheroidized while preventing fusion or coalescence of the powder particles due to excessive heating of the powder particles. It becomes possible.

  When the temperature N (° C.) is N <100 (° C.), the powder particles may not be sufficiently spheroidized. When 300 (° C.) <N, the processing temperature is too high, and the powder particles may be fused in the apparatus.

  Further, as shown in FIG. 3, the hot air supply means 3 of the present invention is equipped with a turning member 8 for turning the hot air in the processing chamber 1 in a spiral manner.

  In the heat treatment apparatus of the present invention, the swing member 8 for swirling the hot air may have a configuration capable of spirally introducing the hot air into the processing chamber. As the structure, as shown in FIG. 3, the turning member 8 for turning the hot air has a plurality of blades 9, and the turning of the hot air can be controlled by the number and angle of the blades. Further, as shown in FIG. 3, in the heat treatment apparatus of the present invention, since the hot air is introduced in a spiral form between the plurality of blades 9, the gap G (mm) between the blades becomes narrower as the number thereof increases. , The flow velocity of the supplied hot air will be faster. In the present invention, for example, when the inner diameter T of the processing chamber is 450 mm, the gap G (mm) of the blade is preferably 5 mm ≦ G ≦ 40 mm. When performing heat treatment of powder particles for toner at G <5 mm, the flow velocity of the hot air may be too fast, and the heat treatment temperature may have to be increased. Also, in the case of 40 mm <G, the swirling speed of the hot air introduced into the processing chamber becomes slow, so that sufficient centrifugal force can not be applied to the powder particles, and coalescence of powder particles during heat treatment increases. You may

  The toner supplied into the processing chamber is heat-treated while being subjected to centrifugal force by the swirling flow. As a result, the collision of the powder particles with one another is reduced, the number of coalesced particles of the powder particles at the time of heat treatment is reduced, and it is possible to obtain a toner having a uniform shape.

  Further, the outlet 3 a of the hot air supply means of the heat treatment apparatus of the present invention is opposed to the upper end portion of the columnar member 5. In addition, this columnar member has a substantially conical distribution member 7 for distributing the supplied hot air in the circumferential direction at the center of the upper end portion thereof.

  Also, as shown in FIG. 4, the substantially conical distribution member may have a cross section extending from upstream to downstream, and may be triangular as in 7-a or 7-b. It may be trapezoidal. Furthermore, although the shape as shown in 7-c of FIG. 4 may be used, the hot air can be uniformly distributed when the cross section is a triangle. The angle θ ° of the base shown in 7-a and 7-b of FIG. 4 is preferably 5 ° ≦ θ ≦ 85 °, and more preferably 30 ° ≦ θ ≦ 75 °.

  When the hot air supply unit of the heat treatment apparatus according to the present invention has such a configuration, the hot air supplied from the hot air supply unit flows in a cylindrical processing chamber while uniformly swirling.

  In addition, it is preferable that the wind speed Vh (m / s) of the hot air introduce | transduced into the process chamber from the turning member of a hot air supply means is 25 (m / s) <= Vh <= 85 (m / s). If the flow velocity of the hot air is within the above range, the shear force applied to the toner is improved, and the powder particles are heat-treated in a more dispersed state.

  In addition, when the wind speed Vh (m / s) of the hot air introduced from the turning member into the processing chamber becomes Vh <25 (m / s), the hot air turning in the processing chamber is weakened, and the powder particles are sufficiently rotated. In some cases, the dispersion of powder particles may not be improved. In addition, when 85 (m / s) <V, the flow velocity of the hot air in the processing chamber may be too fast, and a sufficient heat treatment may not be performed.

  In the heat treatment apparatus of the present invention, the powder particle supply means for supplying powder particles to the processing chamber is an apparatus outer peripheral portion downstream of the hot air supply means outlet portion 3a as shown in the powder supply means 2 of FIG. It is characterized by being provided with two or more.

  Further, the powder supply means 2 is provided on the side surface of the processing chamber, and the powder particles are transported by the carrier fluid supplied from the high pressure air supply nozzle (not shown) and supplied to the processing chamber.

  Further, as shown in FIG. 5, the powder supply means of the heat treatment apparatus of the present invention 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. The number is preferably 2 to 16 and more preferably 5 to 12. When the powder supply means provided on the outer peripheral portion of the processing chamber is introduced from 5 to 12 so as to be present on the same cross section orthogonal to the central axis of the cylindrical processing chamber, the processing amount is increased during heat treatment. Even if it is increased, it is possible to suppress the increase of coalescent particles of the powder particles while maintaining the average circularity of the powder particles for toner after the heat treatment.

  For example, when the inner diameter T of the processing chamber is 450 mm, the number of powder particle supply means provided on the outer peripheral portion of the processing chamber is on the same cross section orthogonal to the central axis of the cylindrical processing chamber. It is preferable that there are eight places.

  If the number of powder particle supply means provided on the outer peripheral portion of the processing chamber is 5 to 12 so as to be on the same cross section orthogonal to the central axis of the cylindrical processing chamber, the processing chamber is introduced into the processing chamber It is impossible to make the density of the dust concentration dense and thin by overlapping the flow of the powder particles from the adjacent powder particle supply means in a state where the dust concentration is lowered, and performing uniform heat treatment It is possible to reduce the amount of heat required for the heat treatment.

  When the number of inlets of powder particle supply means provided on the outer peripheral portion of the processing chamber is smaller than 5 so as to be on the same cross section orthogonal to the central axis of the cylindrical processing chamber, the processing amount of toner In the same case, the ratio of coarse particles formed by coalescence of the molten particles and the particles may increase due to an increase in dust concentration per mouth.

  On the other hand, if the number of inlets of the powder particle supply means provided on the outer peripheral portion of the processing chamber so as to be on the same cross section orthogonal to the central axis of the cylindrical processing chamber is greater than 12; The distance between the inlets of the adjacent powder particle supply means becomes short, and part of the powder particles introduced from the powder particle supply means overlap, which causes the density of dust to be uneven, making it impossible to carry out uniform heat treatment. is there.

  When the inner diameter T is 450 mm, the number of powder particle supply means provided on the outer peripheral portion of the processing chamber is eight so as to be on the same cross section orthogonal to the central axis of the cylindrical processing chamber. In the case of the portion, the powder particles can be supplied without gaps to the falling hot air while being rotated, and the heat transfer from the hot air to the powder particles may be efficient.

  That is, in the range of 250 (mm) よ う T 900 900 (mm), the outer peripheral portion of the processing chamber is such that the inner diameter T exists on the same cross section orthogonal to the central axis of the cylindrical processing chamber at the same temperature. When the number of introduction ports of the powder particle supply means provided in the above is 5 to 12, the circularity of the toner particles after the heat treatment becomes high. Furthermore, since the apparatus is configured to be supplied into the processing chamber from the device outer peripheral portion, the contact time with the swirling hot air in the processing chamber can be increased, and the heat treatment can be performed efficiently.

  In addition, when powder particles and its carrier fluid are introduced at an angle to the flow of hot air that descends while rotating, the flow rate is the portion where "hot air" and "powder particles and its carrier fluid" collide. A lot of "hot air" will push "powder particles and its carrier fluid".

  The central axis of the cylindrical processing chamber and the angle formed by the cross section orthogonal to the central axis of the cylindrical processing chamber and the introduction direction of the powder particles introduced from the powder particle supply means outlet When the orthogonal cross section and the falling angle of the hot air are deeper, the “hot air” pushes the hot air supply means side of the “powder particles and the carrier fluid thereof”. On the other hand, the center of the cylindrical processing chamber is defined by an angle formed by a cross section orthogonal to the central axis of the cylindrical processing chamber and the introduction direction of the powder particles introduced from the powder particle supply means outlet. When the cross section orthogonal to the axis and the falling angle of the hot air are shallow, the "hot air" pushes the outlet side of the "powder particles and its carrier fluid".

  At the portion of "powder particles and its carrier fluid" pushed by "hot air", the dust density of the powder particles is increased, and the trajectory of the particles is easily disturbed. For this reason, the probability that the melted powder particles collide with each other may increase, and the ratio of the coalesced and coarsened particles may increase.

Therefore, in the powder particle supply means of the heat treatment apparatus of the present invention, in FIG. 6, the cross section 11 (11 is a cross section) perpendicular to the central axis (12 in FIG. 6) of the cylindrical processing chamber The angle α (°) formed by the direction of degeneracy to the line) and the introduction direction 13 of the powder particles introduced from the powder particle supply means outlet is
17 (°) ≦ α ≦ 37 (°)
I am satisfied. This reduces the difference in angle between the powder particles and the carrier fluid with respect to the downward flow of the hot air while rotating, or the angle is matched, which is preferable in reducing the proportion of coalescent particles. . More preferably,
22 (°) ≦ α ≦ 32 (°)
To be satisfied.

This is a powder particle of a formulation that is particularly susceptible to fusion when α = 0 (°). The direction of the hot air at the outlet of the powder particle supply means and the cross section orthogonal to the central axis of the cylindrical processing chamber The angle of the hot air at the outlet of the powder particle supply means is 22 ° to 32 °. Based on this, in consideration of manufacturing errors, the range of the angle α of the powder particle feeding means is 17 (°) ≦ α ≦ 37 (°)
And

  In the case where the inner diameter T is 450 mm, it is preferable that α = 27 (°) because it matches the angle of the hot air that descends with an angle of 27 (°).

  In the powder particle supply means of the present invention, the center of the powder particle and the duct through which the carrier fluid passes passes through the center of the cross section where the cylindrical processing chamber and the powder particle supply means connect and the central axis of the processing chamber It is characterized in that the angle formed by the orthogonal cross sections is α (°).

  When α (°) is larger than 37 (°), the distance between the powder particles introduced from the adjacent toner introduction port and the transport fluid becomes wide, and the percentage of the hot air that drops without mixing with the powder particles Can increase the efficiency of heat transfer from the hot air to the powder particles. For this reason, since the powder particles are not sufficiently heat-treated, it is necessary to raise the temperature of the hot air in order to perform the heat treatment sufficiently. However, when the temperature of the hot air is higher, the proportion of the powder particles coalesced and coarsening is increased, and fusion may occur at the outlet of the powder particle supply means, which is not preferable.

  When α (°) is smaller than 17 (°), the powder particles and the carrier fluid thereof are introduced at an angle to the flow of the hot air, and turbulence occurs in the flow field at the mixing portion. As a result of the occurrence of the disturbance, the probability that the particles collide with each other increases, and the ratio of the particles to be integrated and coarsened sometimes increases, which is not preferable.

  In the heat treatment apparatus of the present invention, the cold air supply means for cooling the heat treated powder particles is disposed downstream of the powder particle supply means outlet as shown in the cold air supply means 4 of FIGS. It is characterized by

  By arranging the cold air supply means downstream of the powder particle supply means, the introduced cold air does not excessively cool the heat treatment zone in the processing chamber, and the heat treatment necessary for spheroidizing the powder particles To prevent the temperature from becoming excessive.

  The temperature R (° C.) supplied from the cold air supply means 4 is preferably −50 ° C. ≦ R ≦ 30 ° C. If the temperature of the cold air is within the above range, the powder particles can be efficiently cooled, and fusion or coalescence of the powder particles can be achieved without inhibiting uniform spheroidizing treatment of the powder particles. It can be prevented.

  Further, the cold air supply means 4 of the heat treatment apparatus according to the present invention is a cylinder as shown in FIG. 10 so that the cold air supplied from the cold air supply means is supplied to the outer peripheral portion of the processing chamber along the inner peripheral surface of the processing chamber. Preferably, they are provided at a plurality of locations so as to be present on the same cross section orthogonal to the central axis of the processing chamber. The number of cold air supply means provided on the outer periphery of the processing chamber to be on the same cross section orthogonal to the central axis of the cylindrical processing chamber is the same as the number of powder particle supply means, or It is preferable that it is more than.

  Specifically, when the number of powder particle supply means provided on the outer peripheral portion of the processing chamber is four so as to exist on the same cross section orthogonal to the central axis of the cylindrical processing chamber, The number of cold air supply means is preferably four or more so as to exist on the same cross section orthogonal to the central axis of the cylindrical processing chamber. More preferably, it is 4-16 places. Further, when the number of powder particle supply means is eight so as to exist on the same cross section orthogonal to the central axis of the cylindrical processing chamber, the same cross section orthogonal to the central axis of the cylindrical processing chamber It is preferable that the number of cold air supply means provided on the outer peripheral portion of the processing chamber so as to be present on the upper side is eight or more. More preferably, it is 8-16 places.

  The number of inlets of the powder particle supplying means is four, so that it exists on the same cross section orthogonal to the central axis of the cylindrical processing chamber, and exists on the same cross section orthogonal to the central axis of the cylindrical processing chamber When the number of cold air supply means provided on the outer peripheral portion of the processing chamber is smaller than four, the powder particle supply means is present on the same cross section orthogonal to the central axis of the cylindrical processing chamber. The powder particles introduced from the above are mixed with the hot air and descend as a mixed fluid while maintaining the trajectory of the powder particles while the cross-sectional shape thereof expands, shrinks, and changes its shape. This mixed fluid is mixed and cooled with the cold air when it descends to the cold air supply means portion, but if the number of the cold air supply means is smaller than the group of the four powder particles introduced from the four places, it is immediately A mass of directly cooled powder particles and a mass of powder particles which are not directly cooled are formed. As a result, the cooling may vary, the flow may be disturbed, and the percentage of particles which are not cooled and which are separated from the orbit and collide with other particles may increase. Not desirable.

  The center of the cylindrical processing chamber is provided with four powder particle supply means 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 When the number of cold air supply means provided on the outer peripheral portion of the processing chamber is greater than 16 so as to exist on the same cross section orthogonal to the axis, but the flow rate of cold air is the same, the central axis of the cylindrical processing chamber The flow velocity of the cold air from the cold air supply means may be slower than the flow velocity of the mixed fluid so that it exists on the same cross section orthogonal to the above. As a result, the flow is disturbed at the cold air introduction means, and the particles separated from the orbit may collide with other particles, which may increase the ratio of the coarsened particles.

  The number of introduction ports of powder particle supply means provided on the outer peripheral portion of the processing chamber is eight so as to be on the same cross section orthogonal to the central axis of the cylindrical processing chamber, When the number of cold air supply means provided on the outer peripheral portion of the processing chamber is smaller than eight so as to exist on the same cross section orthogonal to the central axis, the same cross section orthogonal to the central axis of the cylindrical processing chamber The powder particles introduced from the powder particle supply means are mixed with the hot air and descend as a mixed fluid while maintaining the trajectory of the powder particles while the cross-sectional shape of the powder particles is expanded, reduced, or changed in shape. Do. This mixed fluid is mixed and cooled with the cold air when it descends to the cold air supply means portion, but if the number of the cold air supply means is smaller than the group of eight powder particles introduced from eight places, it is immediately A mass of directly cooled powder particles and a mass of powder particles which are not directly cooled are formed. As a result, the cooling may vary, the flow may be disturbed, and the percentage of particles which are not cooled and which are separated from the orbit and collide with other particles may increase. Not desirable.

  The number of introduction ports of the powder particle supply means is eight on the same cross section orthogonal to the central axis of the cylindrical processing chamber, and exists on the same cross section orthogonal to the central axis of the cylindrical processing chamber As described above, although the number of cold air supply means is more than 16 points, when the cold air flow rate is the same, the flow rate of cold air from the cold air supply means may be slower than the flow rate of the mixed fluid. As a result, the flow is disturbed at the cold air introduction means, and the particles separated from the orbit may collide with other particles, which may increase the ratio of the coarsened particles.

  The powder particles and the carrier fluid are introduced into the processing chamber at the same angle as the falling angle of the hot air and descend while rotating. When cold air from the cold air supply means is introduced into the processing chamber at an angle with respect to the descending angle of the hot air and the mixed fluid formed by the powder particles and the carrier fluid, the part where the cold air is introduced In some cases, the powder particles may collide and coalesce into coarse particles before being cooled.

  Therefore, as in the present invention, the cross section orthogonal to the central axis of the cylindrical processing chamber and the introduction direction of the powder particles introduced from the outlet of the cold air supply means match the falling angle of the mixed fluid, The ratio of coalescent particles can be reduced without disturbing the flow of powder particles in the

In the cold air supply means of the heat treatment apparatus of the present invention, in FIG. 7, the cross section 14 (14 is a cross section) orthogonal to the central axis (15 in FIG. 7) of the cylindrical processing chamber, but in FIG. Angle (β), which is defined by the direction in which the cooling air is introduced and the direction 16 of introducing cold air introduced from the outlet of the cold air supply means,
17 (°) ≦ β ≦ 37 (°)
I am satisfied. As a result, the direction of the mixed fluid descending while rotating and the direction formed by the cold air are the same, or the difference in the angle between the direction of the mixed fluid and the direction formed by the cold air is reduced, which is preferable in reducing the ratio of coalescent particles .

More preferably,
22 (°) ≦ β ≦ 32 (°)
To be satisfied.

By the way, with the equipment configuration of α = 0 (°), the powder particles of the formulation that is particularly susceptible to fusion, and the cross section which is perpendicular to the falling direction of the hot air at the cold air supply means outlet and the central axis of the cylindrical processing chamber When the difference of the angle was confirmed, the angle of the hot air in the cold air supply means exit part was 22 degrees-32 degrees. Based on this, the cold air supply means is 17 (°) ≦ β ≦ 37 (°) in consideration of manufacturing errors.
And

  In the case where the inner diameter T is 450 mm, it is preferable that β = 27 (°) because it coincides with the angle of the mixed fluid that descends with an angle of 27 (°).

  In the cold air supply means of the present invention, the center of the duct through which the cold air passes passes through the center of the cross section where the cylindrical processing chamber and the powder particle supply means connect, and the angle formed by the cross section orthogonal to the central axis of the processing chamber is β It is characterized in that it is (°).

  When the flow of powder particles is disturbed, the number of colliding and coalescing particles increases and the ratio of coarsened particles increases, so a flow field with less turbulence is preferable.

α (°) and β (°) are
α-10 (°) β β (°) α α + 10 (°)
Since it becomes a flow field with little disorder from introduction | transduction of powder particle | grains to completion | finish of cooling as it is, since the coarse powder ratio can be reduced, it is preferable. More preferably,
α (°) and β (°) are
α-5 (°) β β (°) α α + 5 (°)
It is.

  When β (°) is larger than 37 (°), the gap between the cold air and the cold air introduced from the adjacent cold air inlets widens, and the ratio of powder particles passing through the gap increases. As a result, the time until the start of cooling of the powder particles may vary, and the ratio of the particles that are not cooled may collide with and coalesce with other particles and increase, which is not preferable.

  When β (°) is smaller than 17 (°), cold air is introduced at an angle to the flow of high-temperature powder particles, and turbulence occurs in the flow field at the mixing portion. As a result of the occurrence of the disturbance, the probability that the particles collide with each other increases, and the ratio of the particles to be integrated and coarsened sometimes increases, which is not preferable.

  Furthermore, it is preferable that the volume and temperature of the introduced cold air can be independently controlled. For example, as shown in FIG. 1, it is preferable that two or more stages of cold air supply means be provided so as not to be in the same circumferential direction. In this case, as shown in FIG. 1, the first stage cold air (4-1) and the second stage cold air (4-2) are for cooling the powder particles introduced into the processing chamber, 3 The stage (4-3) can be functionally separated from the cold air to cool the powder particles on the bottom of the apparatus.

  Furthermore, as shown in the discharge port 6 of FIGS. 1 and 2, the discharge port for discharging the heat treated powder particles from the lower end portion side of the processing chamber is processed so as to maintain the swirling direction of the swirled powder particles. It is characterized in that it is provided at the outer periphery of the chamber.

  Thus, the swirling flow in the apparatus can be maintained, and the centrifugal force applied to the powder particles reduces adhesion and fusion to the regulating means 5 for regulating the flow of the powder particles. In the heat treatment apparatus of the present invention, the powder particle collecting means may be at the lowermost end in the apparatus in the direction to maintain the swirling flow. In addition, a blower (not shown) is provided at the tip of the discharge port, and is configured to be suctioned and transported by the blower.

  In the heat treatment apparatus of the present invention, the relationship between the total flow rate QIN of the compressed air, the hot air and the cold air supplied into the apparatus and the air flow QOUT drawn by the blower is adjusted to satisfy the relation of QIN ≦ QOUT. Is preferred. 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 toner particles from receiving excessive heat. As a result, it is possible to prevent the increase of coalesced powder particles and the fusion in the apparatus, and it is possible to manufacture the toner stably even in long-term use.

  Further, in the heat treatment apparatus of the present invention, in order to regulate the flow of powder particles, a columnar member having a circular cross-section like the regulation means 5 of FIG. 2 is projected from the lower end to the upper end of the processing chamber. It is preferable to arrange it on the central axis of the processing chamber.

  As a result, the toner flow velocity at the end portion of the powder particle collection means can be increased, and the dischargeability of the powder particles can be improved, and adhesion, fusion and powder particles in the collection portion can be prevented. Can.

  In the heat treatment apparatus of the present invention, the ratio V (volume%) of the regulation means 5 for regulating the flow of powder particles in the treatment chamber is preferably 5 volume% ≦ V ≦ 60 volume%. By being in the said range, the flow velocity of the powder particle in a processing chamber can be controlled, and it is thought that the dispersibility and dischargeability of powder particle improve. If the restriction means 5 for restricting the flow of powder particles occupies V in the processing chamber at V <5 volume%, the swirl of toner in the processing chamber is weakened, so that sufficient for powder particles. And the dispersion of powder particles may not be improved. If 60 volume% <V, the flow velocity of the powder particles in the processing chamber may be too fast, and sufficient heat treatment may not be performed.

  The columnar member is preferably provided with a cooling jacket in order to prevent fusion of the powder particles. Furthermore, it is desirable to introduce cooling water (preferably, an antifreeze solution such as ethylene glycol) into the cooling jacket, and the surface temperature of the cooling jacket is preferably 40 ° C. or less.

  Next, a procedure for producing a toner using the toner particle producing apparatus of the present invention will be described.

  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 Nippon Coke Co., Ltd.); super mixer (manufactured by Kawata Co., Ltd.); ribo cone (manufactured by Ogawara Seisakusho Co., Ltd.); Nauta mixer, turbulizer, cyclomix (manufactured by Hosokawa Micron Corp.); Mixer (manufactured by Pacific Kiko Co., Ltd.); Loedige mixer (manufactured by Matsubo Co., Ltd.) and the like.

  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 kneader include a TEM type extruder (manufactured by Toshiba Machine Co., Ltd.); a TEX twin screw kneader (manufactured by Japan Steel Works Co., Ltd.); a PCM kneader (manufactured by Ikegai Iron Works Co., Ltd.); The continuous kneader such as a single-screw or twin-screw extruder is preferable to a batch-type kneader because of its superiority such as continuous production.

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

  The cooled product of the colored resin composition obtained above is then ground to a desired particle size in a grinding step. In the pulverizing step, first, coarse crushing is carried out with a crusher, hammer mill, feather mill etc., and further finely grinding with a Cryptron system (made by Kawasaki Heavy Industries), Superrotor (made by Nisshin Engineering) etc. to obtain toner particles. .

  The obtained toner fine particles are classified into powder particles for toner having a desired particle diameter in a classification step. Examples of classifiers include Turboplex, Faculty, TSP separator, TTSP separator (manufactured by Hosokawa Micron), Elbow Jet (manufactured by Nittetsu Mining Co., Ltd.), and the like.

  Subsequently, in the heat treatment step, the obtained powder particles for toner are 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 predetermined amount of powder particles for toner and various known external additives are compounded, and Henschel mixer, mechano hybrid (manufactured by Nippon Coke Co., Ltd.), super mixer, novirta The mixture is stirred and mixed using a high-speed stirrer which exerts a shearing force on the powder (made by Hosokawa Micron) as an external adder.

  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, and a toner with 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 for removing coarse particles include turboplex, TSP separator, TTSP separator (manufactured by Hosokawa Micron), elbow jet (manufactured by Nittetsu Mining Co., Ltd.), and the like.

  Furthermore, after the heat treatment, in order to sift coarse particles etc. if necessary, for example, ultrasonic (made by Ryoei Sangyo Co., Ltd.); Resonator sieve, Gyro Shifter (Tokuju Works Co., Ltd.); Turbos Cleaner (manufactured by Turbo Kogyo Co., Ltd.) ) A sieving machine such as Hi-Bolter (manufactured by Toyo High-Tech Co., Ltd.) may be used.

  The heat treatment step of the present invention may be after the above-mentioned pulverization or after classification.

  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. 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.

  Examples of the wax used for the toner of the present invention include the following. Low molecular weight polyethylene, low molecular weight polypropylene, alkylene copolymer, microcrystalline wax, paraffin wax, hydrocarbon-based wax such as Fischer-Tropsch wax; oxide of hydrocarbon-based wax such as oxidized polyethylene wax or block copolymers thereof Waxes based on fatty acid esters such as carnauba wax; Deoxidized a part or all of fatty acid esters such as deoxidized carnauba wax. Further, the following may be mentioned. Saturated linear fatty acids such as palmitic acid, stearic acid, and montanic acid; unsaturated fatty acids such as brassic acid, eleostearic acid and valinaric acid; stearyl alcohol, aralkyl alcohol, behenyl alcohol, carnavir alcohol, seryl alcohol, Saturated alcohols such as sill alcohol; polyhydric alcohols such as sorbitol; fatty acids such as palmitic acid, stearic acid, behenic acid, montanic acid, stearyl alcohol, aralkyl alcohol, behenyl alcohol, carnauvir alcohol, ceryl alcohol, Esters with alcohols such as silalcohols; fatty acid amides such as linoleic acid amide, oleic acid amide, lauric acid amide; methylenebisstearic acid amide, ethylenebiscapric acid And saturated fatty acid bisamides such as ethylene bis lauric acid amide and hexamethylene bis stearic acid amide; ethylene bis oleic acid amide, hexamethylene bis oleic acid amide, N, N 'dioleyl adipic acid amide, N, N' dioleyl Unsaturated fatty acid amides such as sebacic acid amide; aromatic bisamides such as m-xylene bis-stearic acid amide, N, N 'distearyl isophthalic acid amide; calcium stearate, calcium laurate, zinc stearate, magnesium stearate Aliphatic metal salts (generally referred to as metal soaps); waxes grafted onto aliphatic hydrocarbon waxes using vinyl monomers such as styrene and acrylic acid; fatty acids such as behenic acid monoglycerides Priced Al Partial esters of Lumpur; methyl ester compounds having hydroxyl groups obtained by hydrogenation of vegetable fats and oils.

  Among these waxes, paraffin wax, hydrocarbon wax such as Fischer-Tropsch wax, or fatty acid ester wax such as carnauba wax are preferable from the viewpoint of improving low temperature fixability and hot offset resistance. In the present invention, hydrocarbon-based waxes are more preferable in that the hot offset resistance is further improved.

  In the present invention, the wax is preferably used in an amount of 1 to 20 parts by mass with respect to 100 parts by mass of the binder resin.

  In the endothermic curve at the time of temperature rise measured with a differential scanning calorimetry (DSC) device, the peak temperature of the maximum endothermic peak of the wax is preferably 45 ° C. or more and 140 ° C. or less. It is preferable that the peak temperature of the maximum endothermic peak of the wax is in the above-mentioned range since both the storage stability of the toner and the hot offset resistance can be achieved.

  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-mentioned additive 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 apparatus, a precise particle size distribution measuring apparatus “Coulter Counter Multisizer 3” (registered trademark, manufactured by Beckman Coulter, Inc.) having a 100 μm aperture tube and using a pore electrical resistance method is used. The setting of measurement conditions and the analysis of measurement data use the attached special software "Beckman Coulter Multisizer 3 Version 3.51" (manufactured by Beckman Coulter, Inc.). The measurement is performed with 25,000 channels of effective measurement channels.

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

  Before measurement and analysis, dedicated software was set as follows.

  In the "Change Standard Measurement Method (SOM)" screen of the special software, set the total count number in the control mode to 50000 particles, set the number of measurements once, and the Kd value "standard particle 10.0 μm" (Beckman Coulter, Make the obtained value. The threshold and noise level are automatically set by pressing the "Threshold / noise level measurement button". Also, set the current to 1600 μA, the gain to 2, and the electrolyte to ISOTON II, and check “Aperture tube flush after measurement”.

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

  The specific measurement method is as follows.

  (1) Place about 200 ml of the electrolytic aqueous solution in a 250 ml round bottom beaker for Multisizer 3 only, set it on a sample stand, and stir the stirrer rod counterclockwise at 24 rotations / second. Then, dirt and air bubbles in the aperture tube are removed by the "aperture flush" function of special software.

  (2) About 30 ml of the electrolytic aqueous solution is placed in a 100 ml flat bottom beaker made of glass. Among them, “contaminone N” (nonionic surfactant, anionic surfactant, 10% by weight aqueous solution of neutral detergent for pH 7 precision measuring instrument cleaning consisting of organic builders as a dispersing agent, Wako Pure Chemical Industries, Ltd. Add about 0.3 ml of a diluted solution obtained by diluting about 3 times by mass with deionized water.

  (3) Two oscillators with an oscillation frequency of 50 kHz are built in with 180 degrees of phase shift, and an ultrasonic dispersion device "Ultrasonic Dispensation System Tetora 150" (manufactured by Nikkaki Bios Co., Ltd.) having an electrical output of 120 W is prepared. About 3.3 liters of ion exchange water is placed in the water tank of the ultrasonic disperser, and about 2 ml of Contaminone N is added to the water tank.

  (4) The beaker of said (2) is set to the beaker fixing hole of the said ultrasonic dispersion device, and an ultrasonic dispersion device is operated. Then, the height position of the beaker is adjusted so that the resonance state of the liquid surface of the electrolytic aqueous solution in the beaker is maximized.

  (5) While the electrolytic aqueous solution in the beaker of (4) is irradiated with ultrasonic waves, about 10 mg of toner is added little by little to the electrolytic aqueous solution and dispersed. Then, ultrasonic dispersion processing is continued for another 60 seconds. In addition, 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 with 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 removed in advance is placed in a glass container. Among them, “contaminone N” (nonionic surfactant, anionic surfactant, 10% by weight aqueous solution of neutral detergent for pH 7 precision measuring instrument cleaning consisting of organic builders as a dispersing agent, Wako Pure Chemical Industries, Ltd. Add about 0.2 ml of a diluted solution of about 3 times by volume diluted with deionized water. Further, about 0.02 g of a measurement sample is added, and dispersion treatment is performed for 2 minutes using an ultrasonic dispersion device to obtain a dispersion for measurement. At that time, the dispersion is suitably cooled so that the temperature of the dispersion becomes 10 ° C. or more and 40 ° C. or less. As the ultrasonic wave disperser, a table-top type ultrasonic cleaner disperser ("VS-150" (manufactured by velvocrea)) having an oscillation frequency of 50 kHz and an electric output of 150 W is used. Put in replacement water, and add about 2 ml of the Contaminone N to the water tank.

  For measurement, a particle sheath “PSE-900A” (manufactured by Sysmex Corporation) was used as a sheath liquid, using the flow type particle image analyzer equipped with a standard objective lens (10 ×). The dispersion 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 invention, a flow type particle image analyzer which has been subjected to a calibration work by Sysmex and which has received a calibration certificate issued by Sysmex, is used. The measurement was carried out under the measurement and analysis conditions when proof of calibration was received except that the particle diameter of 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 a polyester unit: 100 parts by mass (weight average molecular weight (Mw): 82450, 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 After mixing the materials of the above formulation with a Henschel mixer FM-75 (manufactured by Nippon Coke Co., Ltd.), a twin-screw kneader PCM-30 (set by Ikegai Ironwork Co., Ltd.) whose temperature was set to 120 ° C. Kneaded in company company). The obtained kneaded product is cooled, roughly crushed to 1 mm or less by a hammer mill, and made into a crushed product, and the obtained crushed product is crushed by a mechanical grinder T-250 (manufactured by Turbo Kogyo Co., Ltd.) Body fine particles were obtained. Subsequently, the obtained powder fine particles were classified by the Faculty F-300 (manufactured by Hosokawa Micron Corporation) to obtain powder particles.

Furthermore, the following materials are introduced into Henschel mixer FM-75 (manufactured by Nippon Coke Co., Ltd.), the peripheral speed of the rotating blade is 50.0 m / sec, and mixing is carried out for 3 minutes on the surface of powder particles. Toner powder particles to which silica and titanium oxide were attached were obtained.
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 a weight average particle diameter (D4) of 6.7 μm, particles having a particle diameter of 4.0 μm or less are 25.5 number%, and particles having a particle diameter of 10.0 μm or more are It was 2.5% 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 C for toner obtained at this time, the ratio of particles having a particle diameter of 4.0 μm or less, the ratio of particles having a particle diameter of 10.0 μm or more, and the average circularity are measured. It is summarized in Table 1.

Example 1
In this example, the powder particles A for toner were heat-treated using the heat treatment apparatus shown in FIG. 1 and FIG. At this time, the inner diameter of the device is 450 mm, and the outer diameter of the restricting means 5 which is a columnar member having a circular cross section is 330 mm.

  The number of the raw material supply means was eight, and they were arranged at 45 ° intervals on the same cross section orthogonal to the central axis of the processing chamber. Further, the angle α (°) formed by the cross section orthogonal to the central axis of the cylindrical processing chamber and the introduction direction of the powder particles introduced from the outlet of the powder particle supply means was 27 °.

Furthermore, 80 mm of length of the longitudinal feed supplies ducts, by lateral length and 10 mm, the cross-sectional area of the material supply means duct and 800 mm ^2, the total cross-sectional area of the material supply means duct was 6400Mm ² .

The flow rate of the carrier fluid supplied from the high pressure air supply nozzle was 0.45 m ³ / min.

  The angle of the substantially conical hot air distribution member 7 in FIG. 2 was 60 °.

Further, using the linear member of FIG. 3, the minimum gap G between the blades of the turning member is 9.5 mm, the height is 30 mm, the number of blades is 22, and the cross-sectional area of the outlet of the hot air supply means is 6270 mm ² .

  Cold air was supplied in three stages as shown in FIG. 1, and the number of first cold air and second cold air supply means was eight, and they were arranged at 45 ° intervals on the same cross section orthogonal to the central axis of the processing chamber . Further, an angle β (°) formed by a cross section orthogonal to the central axis of the cylindrical processing chamber and the introducing direction of the cold air introduced from the outlet of the cold air supply means was 27 °. The number of third cold air supply means was three, and was arranged at an interval of 90 ° on the same cross section orthogonal to the central axis of the processing chamber in combination with one discharge port.

  Further, the distance from the lower end of the powder supply means outlet to the upper end of the first cold air supply means was 230 mm.

By making the vertical length of the cold air supply means duct 80 mm and the lateral length 10 mm, the cross sectional area of the cold air supply means duct is 800 mm ² and the total cross sectional area of the first cold air supply means duct is 6400 mm ² . Further, the total cross-sectional area of the second cold air supply means duct was 6400 mm ² . The total cross-sectional area of the third cold air supply means duct was 2400 mm ² .

On the other hand, the cross-sectional area of the discharge port was 125 mm in length, 50 mm in width, and 6250 mm ² in cross-sectional area.

  The device configuration at this time is referred to as device configuration 1. Table 2 shows the basic conditions of the device configuration 1. Table 2 also shows the case apparatus configuration described later.

  Using the above apparatus configuration 1, the powder particle A for toner is heat-treated at a processing amount (kg / h) of the powder particle A for toner of 150 kg / h, and the heat-treated particles for toner having an average circularity of 0.965 Obtained.

The conditions at this time were a hot air temperature of 170 ° C. and a hot air flow rate of 28.0 m ³ / min. The flow rate of the first cold air was divided into eight parts of 8.0 m ³ / min, and 1.0 m ³ / min of cold air was supplied into the processing chamber. Similarly, the flow rate of the second cold air was divided into eight sections of 8.0 m ³ / min, and each 1.0 m ³ / min of cold air was supplied into the processing chamber. The third cold air was divided into three 4.5 m ³ / min, and each 1.5 m ³ / min cold air was supplied into the processing chamber.

  The above operating condition is referred to as operating condition 1.

  The surface-modified powder particles obtained at this time have a weight-average particle diameter (D4) of 6.8 μm, particles having a particle diameter of 4.0 μm or less are 24.4% by number, and particles having a particle diameter of 10.0 μm or more. Is 3.6% by volume, and there are very few coarse particles. This is a surface-modified powder particle for toner.

  Next, after the operation for 1 hour, the supply of the powder particle A for toner was stopped, and the fusion state was confirmed. As a result, no fusion was observed.

  Next, similarly, using the apparatus configuration 1, the powder particle A for toner is heat-treated, with the processing amount (kg / hr) of the powder particle A for toner being 220 kg / hr, for a toner having an average circularity of 0.965. Heat treated particles were obtained.

  In this case, the processing was performed under the operating condition 1 so that the hot air temperature was 200 ° C. so that a toner having an average circularity of 0.965 could be obtained even if the throughput was increased. The surface-modified powder particles obtained at this time have a weight-average particle diameter (D4) of 6.9 μm, particles having a particle diameter of 4.0 μm or less are 24.1% by number, and particles having a particle diameter of 10.0 μm or more. Was 3.9% by volume.

  In addition, the increase in volume percentage of particles with a particle diameter of 10.0 μm or more at a treatment of 220 kg / h is 0.3% as compared to that at a treatment of 150 kg / h, and the coarse Surface modified powder particles for toner.

  The evaluation for the obtained surface-modified powder particles for toner, the heat treatment apparatus and the heat treatment system was performed based on the following criteria.

<Evaluation of coarse powder amount>
The coarse powder amount of the obtained powder particles for toner after heat treatment is used as an index of coarse particles contained after heat treatment, and the ratio s (volume%) of particles of 10.0 μm or more in the surface modified particles is described below Judged on the basis of
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 amount of treatment is increased>
The difference of coarse powder at 220 kg / h treatment and difference Δs (vol%) of the coarse powder amount at 150 kg / h treatment are taken as an index of ease of increasing the amount of treatment in the heat treatment apparatus of the present invention. Judged on the basis of
A: 2.0 <Δs
B: 2.0 ≦ Δs <4.0
C: 4.0 ≦ Δs <6.0
D: 6.0 ≦ Δs <8.0
E: 8.0 ≦ Δs

<Evaluation of heat treatment equipment for fusion>
After one hour of operation under the conditions of each example, the supply of powder particles B for toner is stopped, and the scope portion of the industrial videoscope "IPLEX SA II R" (manufactured by OLYMPUS CO., LTD.) It inserted from the inspection port (not shown) of piping, the fusion state was checked, and it judged on the following standard.
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 is recognized, Unable to operate

  These results are summarized in Table 3.

Example 2
In the present embodiment, in the apparatus configuration 1 of the heat treatment apparatus shown in FIG. 1 and FIG. As a result, the toner processing amount (kg / hr) was 150 kg / hr, and heat-treated particles for toner having an average circularity of 0.965 were obtained. The powder particle B for toner had the amount of added wax increased to 6 parts by mass more than the powder particle A for toner, so the processing temperature for obtaining an average circularity of 0.965 became high.

  Next, similarly, using the apparatus configuration 1, the powder particle B for toner is heat-treated, with the processing amount (kg / hr) of the powder particle B for toner being 220 kg / hr, for a toner having an average circularity of 0.965. Heat treated particles were obtained.

  The condition at this time was operating condition 1 and the hot air temperature was set to 210 ° C. so that a toner having an average circularity of 0.965 could be obtained even if the throughput was increased.

  The processing temperature was higher than in Example 1, but the heat-treated heat-treated particles for toner did not stay at the bottom of the device, there was no fusion, there were no coalescence particles, and the coarseness was slightly inferior to Example 1. The powder amount was also very low, and the desired degree of circularity was obtained. For this reason, the increase in the coarse powder was very small even when the throughput was increased from 150 kg / h to 220 kg / hr.

  These results are summarized in Table 3.

[Example 3]
In the present embodiment, in the apparatus configuration 1 of the heat treatment apparatus shown in FIG. 1 and FIG. As a result, the toner processing amount (kg / hr) was 150 kg / hr, and heat-treated particles for toner having an average circularity of 0.965 were obtained. The powder particle C for toner has a wax addition amount more than that of the powder particle B for toner, which is 8 parts by mass, so that the processing temperature for obtaining an average circularity of 0.965 is compared with Example 1 and Example 2. It got higher.

  Next, similarly, using the apparatus configuration 1, the powder particle C for toner is heat-treated at a processing amount (kg / hr) of the powder particle C for toner of 220 kg / hr, for a toner having an average circularity of 0.965. Heat treated particles were obtained.

  The condition at this time was operating condition 1 and the hot air temperature was set to 220 ° C. so that a toner having an average circularity of 0.965 could be obtained even if the throughput was increased.

  The processing temperature was higher than in Examples 1 and 2. However, the heat-treated heat-treated particles for toner do not stay at the bottom of the apparatus, there is no fusion, and coalescence particles are suppressed. Although inferior to Example 2, the amount of coarse powder was also very small, and the desired degree of circularity was obtained. Therefore, the increase in the coarse powder was very small even when the treatment amount was increased from 150 kg / hr to 220 kg / hr.

  These results are summarized in Table 3.

Example 4
In this embodiment, using the powder particles C for toner, the inclination of the cold air supply means in the system configuration 1 is a cross section orthogonal to the central axis of the cylindrical processing chamber and the cold air introduced from the cold air supply means outlet. The angle β (°) formed by the introduction direction was 17 (°). This device configuration is referred to as device configuration 2.

  The operating conditions were heat treatment with a hot air temperature of 190 ° C. when the processing amount was 150 kg / hr under operating condition 1 and a hot air temperature of 220 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  Since the inclination of the cold air is shallower than the falling angle of the hot air, the flow in the apparatus is slightly disturbed compared to the third embodiment, and the ratio of the particles which collide and coalesce are roughly increased, but the rough The increase in the powder ratio was very small, and a large amount of toner could be processed. Also, there was no fusion within the device.

[Example 5]
In this embodiment, using the powder particles C for toner, the inclination of the cold air supply means in the system configuration 1 is a cross section orthogonal to the central axis of the cylindrical processing chamber and the cold air introduced from the cold air supply means outlet. The angle β (°) formed by the introduction direction was 37 (°). This device configuration is referred to as device configuration 3.

  The operating conditions were heat treatment with a hot air temperature of 190 ° C. when the processing amount was 150 kg / hr under operating condition 1 and a hot air temperature of 220 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  Since the inclination of the cold air is deeper than the falling angle of the hot air, the toner powder particles passing through the cold air portion in the cold air supply means and the toner powder particles not passing through the cold air portion have come out. The toner powder particles C which do not pass through the cold air portion in the latter case have a high probability of colliding with other particles in the molten state, which causes an increase in the ratio of coarsened particles. However, the amount of increase in the proportion of coarse powder was small, and a large amount of toner could be processed. Also, there was no fusion within the device.

[Example 6]
In this embodiment, the powder particle C for toner is used, and a cross section orthogonal to the central axis of the cylindrical processing chamber in the device configuration 3 and the introduction direction of the powder particle introduced from the powder particle supply means outlet and The angle α (°) formed by This device configuration is referred to as device configuration 4.

  The operating conditions were heat treatment with a hot air temperature of 190 ° C. when the processing amount was 150 kg / hr under operating condition 1 and a hot air temperature of 220 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  As the inclination of the powder particles for toner becomes shallower than the falling angle of the hot air, the flow in the apparatus is disturbed as compared with the fifth embodiment, and the ratio of the particles colliding and coalescing increases. As a result, although the amount of change in the ratio of coarse powder also increased, a large amount of toner could be processed. In addition, fusion within the device was slightly observed.

[Example 7]
In this embodiment, the powder particle C for toner is used, and in the apparatus configuration 4, a cross section orthogonal to the central axis of the cylindrical processing chamber, and the introducing direction of the powder particle introduced from the powder particle supply means outlet The angle α (°) formed by This device configuration is referred to as device configuration 5.

  The operating conditions were heat treatment with a hot air temperature of 210 ° C. when the processing amount was 150 kg / hr under operating condition 1 and a hot air temperature of 240 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  When the inclination of the powder particles for toner becomes deeper than the falling angle of the hot air, the distance between the powder particles introduced from the adjacent toner introduction port becomes wide, and the gap between the powder particles and the powder particles Since the hot air which does not mix with the powder particles is increased and the efficiency of heat transfer from the hot air to the powder particles is lowered, it is necessary to increase the temperature of the hot air to obtain a toner having an average circularity of 0.965. The For this reason, the ratio of the powder particle which collides and unites and coarsens increased. As a result, the amount of change in the proportion of coarse powder also increased, and fusion was slightly observed at the outlet of the powder particle supply means.

Example 8
In this embodiment, the powder particles C for toner are used, and the number of first cold air supply means and the number of second cold air supply means are set to four in the system configuration 5, and are orthogonal to the central axis of the processing chamber. They were arranged at 90 ° intervals on the same cross section. This device configuration is referred to as device configuration 6.

The operating conditions were heat treatment with a hot air temperature of 210 ° C. when the processing amount was 150 kg / hr under operating condition 1 and a hot air temperature of 240 ° C. when the processing amount was 220 kg / hr. The flow rate of the first cold air, divided into four 8.0 m ³ / min, was fed cold air 2.0 m ³ / min into the processing chamber, respectively. Similarly, the flow rate of the second cold air is divided into four 8.0 m ³ / min, was fed cold air 2.0 m ³ / min into the processing chamber, respectively. This operating condition is referred to as operating condition 2.

  These results are summarized in Table 3.

  Since the number of cold air supply means is smaller than the number of powder particle supply means, powder particles passing through the cold air portion and powder particles not passing through the cold air portion can be formed in the cold air supply means, and the flow velocity of cold air is fast. As a result, powder particles that have passed through the cold air portion fall faster than powder particles that do not pass through the cold air portion, causing separation of particle clusters, which disrupts the particle flow. . As a result, in the powder particles which did not pass through the cold air portion, the ratio of the particles which collided with other particles and was coarsened was increased. The amount of increase in the proportion of coarse powder was also large, and slight fusion was observed in the apparatus.

Comparative Example 1
In this comparative example, using toner powder particles C, in section 6, the section orthogonal to the central axis of the cylindrical processing chamber in the apparatus configuration 6, and the introduction direction of the powder particles introduced from the powder particle supply means outlet The angle α (°) formed by Also, the inclination of the cold air supply means is an angle β (°) of 16 (°) formed by a cross section orthogonal to the central axis of the cylindrical processing chamber and the introduction direction of the cold air introduced from the cold air supply means outlet. did. This device configuration is referred to as device configuration 7.

  The operating conditions were heat treatment with a hot air temperature of 190 ° C. when the processing amount was 150 kg / hr under operating condition 2 and a hot air temperature of 220 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  The flow of particles is caused by the introduction direction of powder particles for toner and the introduction direction of cold air being shallower than the falling angle of wind and the number of cold air supply means being smaller than the number of powder particle supply means And the increase in the proportion of particles with a long time to cooling increased the proportion of particles that collided with other particles and coarsened. In particular, as the throughput increased, the proportion of coarsened particles increased. Also, a slight fusion was seen in the device.

Comparative Example 2
In this comparative example, the powder particle C for toner is used, and in the device configuration 7, the cold air supplied from the cold air supply means outlet and the cross section orthogonal to the central axis of the cylindrical processing chamber. The angle .beta. (.Degree.) Formed by the introduction direction of and is 38 (.degree.). This device configuration is referred to as a device configuration 8.

  The operating conditions were heat treatment with a hot air temperature of 190 ° C. when the processing amount was 150 kg / hr under operating condition 2 and a hot air temperature of 220 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  As compared with Comparative Example 1, when the inclination of the cold air is deeper than the falling angle of the hot air, the toner powder particles passing through the cold air portion in the cold air supply means and the toner powder particles not passing through the cold air portion Come out. The latter powder particles for toner that do not pass through the cold air portion have a high probability of colliding with other particles in the molten state, which increases the ratio of coarsened particles, causing an increase in throughput. The proportion of coarsened particles increased. Also, a slight fusion was seen in the device.

Comparative Example 3
In this comparative example, using the powder particle C for toner, in the device configuration 7, the inclination of the powder particle supply means is introduced from the cross section orthogonal to the central axis of the cylindrical processing chamber and from the cold air supply means outlet The angle α (°) formed by the direction in which the cold air is introduced is 38 (°). This device configuration is referred to as a device configuration 9.

  The operating conditions were heat treatment with a hot air temperature of 220 ° C. when the processing amount was 150 kg / hr under operating condition 2 and a hot air temperature of 250 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  Since the inclination of the powder particles for toner is deeper than the falling angle of the hot air compared with Comparative Example 1, the distance between the powder particles introduced from the adjacent toner introduction port becomes wider, and the powder particles and In order to obtain a toner having an average circularity of 0.965, since the ratio of the hot air which descends without mixing the powder particles with the powder particles increases and the heat transfer efficiency from the hot air to the powder particles decreases. It was necessary to raise the hot air temperature. For this reason, the ratio of the powder particle which collides and unites and coarsens increased. As a result, the amount of change in the proportion of coarse powder also increased, and fusion was observed at the outlet of the powder particle supply means.

Comparative Example 4
In this comparative example, the powder particle C for toner is used, and in the device configuration 9, the cold air supplied from the cold air supply means outlet and the cross section orthogonal to the central axis of the cylindrical processing chamber. The angle .beta. (.Degree.) Formed by the introduction direction of and is 38 (.degree.). This device configuration is referred to as a device configuration 10.

  The operating conditions were heat treatment with a hot air temperature of 220 ° C. when the processing amount was 150 kg / hr under operating condition 2 and a hot air temperature of 250 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  As compared with Comparative Example 3, when the inclination of the cold air is deeper than the falling angle of the hot air, the toner powder particles passing through the cold air portion in the cold air supply means and the toner powder particles not passing through the cold air portion Come out. The latter powder particles for toner that do not pass through the cold air portion have a high probability of colliding with other particles in the molten state, which increases the ratio of coarsened particles, causing an increase in throughput. The proportion of coarsened particles increased. Also, fused material was seen in the device.

Comparative Example 5
In this comparative example, the powder particles for toner were made into powder particles C for toner, and heat treatment was carried out and evaluated by the heat treatment apparatus of the device configuration 11 shown in FIG.

  In this apparatus configuration, the exhaust port is a straight exhaust, the raw material supply port is one, the powder particles for toner and the hot air are swirled in the same direction and supplied into the apparatus. The cold air is provided with a first cold air which is introduced straight to the wall of the apparatus by providing a slit and a second cold air which is introduced from the tangential direction to cool the outlet.

  The results are summarized in Table 3.

In this device configuration, the flow rate of the carrier fluid supplied from the high-pressure air supply nozzle is 3.6 m ³ / min, the flow rate of the first cold air is 8.0 m ³ / min, and the second cold air is 4.0 m ³ / m. min was supplied into the processing chamber.

  As a result, the temperature for obtaining an average circularity of 0.965 was high, and the temperature reached 300 ° C. at 150 kg / hr and 350 ° C. at 220 kg / hr.

  When the treatment amount was increased from 150 kg / h to 220 kg / h because the treatment temperature became high, coarse powder increased significantly.

  The flows of the hot air, powder particles for toner, and cold air in the apparatus were disturbed and not uniform, and therefore, the number of coalescent particles increased, and the amount of coarse powder greatly increased. Furthermore, in the apparatus configuration, when the processing amount is large and the processing temperature is high, large fusion is observed in the apparatus.

Comparative Example 6
In this comparative example, the powder particles for toner were made into powder particles C for toner, and heat treatment was carried out and evaluated in the heat treatment apparatus of the apparatus configuration 12 shown in FIG.

  The present apparatus configuration 12 is configured such that the hot air supply unit and the raw material supply unit of the apparatus configuration 11 are remodeled so that the powder particles for toner and the hot air swirl in opposite directions and are supplied into the apparatus. Further, as shown in FIG. 8, the relationship between the hot air and the raw material supply unit is such that the hot air is supplied from the inside of the raw material supply unit.

  The results are summarized in Table 3.

  In this comparative example, using the apparatus configuration 12, the powder particles for toner having an added amount of wax of 8 parts by mass were heat-treated in the same manner as in Comparative example 3.

In this apparatus configuration, the flow rate of the injection air supplied from the high pressure air supply nozzle was 3.6 m ³ / min, and the toner powder particles C were supplied into the apparatus.

  As a result, the temperature for obtaining an average circularity of 0.965 was high, and 350 ° C. at 150 kg / h and 350 ° C. at 220 kg / h.

  In the 220 kg / hr treatment, it was not possible to obtain an average circularity of 0.965 even if the hot air temperature was raised to 400 ° C. Therefore, it was not possible to evaluate the amount of coarse powder at the time of 280 kg / hr treatment, evaluation of fusion and evaluation of Δs which is the difference between the amount of coarse powder at 150 kg / hr treatment.

  Further, since the flow of the hot air in the apparatus and the flow of the powder particles for toner are reversed, coalescent particles increase and the amount of coarse powder largely increases. Furthermore, in the apparatus configuration, large fusion was observed at the apparatus outlet under an operating condition where the processing amount was large and the processing temperature was high.

[Reference Example 1]
In this embodiment, the powder particle C for toner is used, and in section 6, the section perpendicular to the central axis of the cylindrical processing chamber in the apparatus configuration 6, and the introduction direction of the powder particle introduced from the powder particle supply means outlet The angle α (°) formed by In addition, the inclination of the cold air supply means is 0 (degrees), and the angle β (°) formed by the cross section orthogonal to the central axis of the cylindrical processing chamber and the introduction direction of the cold air introduced from the cold air supply means outlet did. This device configuration is referred to as a device configuration 13.

  The operating conditions were heat treatment with a hot air temperature of 190 ° C. when the processing amount was 150 kg / hr under operating condition 2 and a hot air temperature of 220 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  In this reference example, the powder particles for toner having an added amount of wax of 8 parts by mass were heat-treated at a processing amount of 150 kg / hr and 220 kg / hr.

  The flow of particles is disturbed by the fact that the direction of introduction of powder particles for toner and the direction of introduction of cold air are shallower than the falling angle of wind and the number of cold air supply means is smaller than the number of powder particle supply means. , The proportion of particles with a long time to cooling increased. As a result, compared to Comparative Example 1, the ratio of particles that collided with other particles and aggregated and coarsened was increased. In particular, as the throughput increased, the proportion of coarsened particles increased. Also, a slight fusion was seen in the device.

Reference Example 2
In this embodiment, the powder particle C for toner is used, and a cross section orthogonal to the central axis of the cylindrical processing chamber in the apparatus configuration 13 and the introduction direction of the powder particle introduced from the powder particle supply means outlet The angle α (°) formed by

  The operating conditions were heat treatment with a hot air temperature of 190 ° C. when the processing amount was 150 kg / hr under operating condition 2 and a hot air temperature of 220 ° C. when the processing amount was 220 kg / hr.

  These results are summarized in Table 3.

  In this reference example, the powder particles for toner having an added amount of wax of 8 parts by mass were heat-treated at a processing amount of 150 kg / hr and 220 kg / hr.

  The flow of particles is disturbed by the fact that the direction of introduction of powder particles for toner and the direction of introduction of cold air are shallower than the falling angle of wind and the number of cold air supply means is smaller than the number of powder particle supply means. , The proportion of particles with a long time to cooling increased. As a result, compared to Comparative Example 1, the ratio of particles that collided with other particles and aggregated and coarsened was increased. In particular, as the throughput increased, the proportion of coarsened particles increased. Also, a slight fusion was seen in the device.

  Compared with the reference example 1, the flow in the apparatus is disturbed by the inclination of the powder particles for toner becoming shallower than the falling angle of the hot air from the inclination of the reference example 1, and the collision and coalescence become coarse. The proportion of particles has increased. As a result, the amount of change in the proportion of coarse powder also increased, and fusion in the apparatus was slightly observed.

Reference Example 3
In the present embodiment, the toner powder particles A were heat-treated in the apparatus configuration 14. The operating condition is operating condition 1.

  Compared with Comparative Example 2, the temperature of the hot air was lowered and the ratio of coarse powder was lowered because the number of portions to which the powder particles for toner was added was 4 parts. Also, although slight fusion was observed inside the device, the amount of change in the ratio of coarse powder decreased, and 220 kg / hr could be processed.

  These results are summarized in Table 2.

  1: treatment chamber in which heat treatment of powder particles is performed, 2: powder particle supply means, 3: hot air supply means, 3-a: hot air supply means outlet, 4: cold air supply means, 4-1: first stage Cold air supply means, 4-2: second stage cold air supply means, 4-3: third stage cold air supply means, 5: control means which is a columnar member having a circular cross section, 6: outlet, 7: substantially Conical hot air distribution member, 7-a: an example of a substantially conical distribution member, 7-b: another example of a substantially conical distribution member, 7-c: yet another of a substantially conical distribution member Examples of 8: hot air swirling member, 9: blade of hot air swirling member, 10: installation place of substantially conical hot air distribution member, 11: cross section orthogonal to central axis of cylindrical processing chamber, 12: cylindrical Central axis of the processing chamber, 13: introduction direction of powder particles and the carrier fluid to the processing chamber 1, 14: central axis of the cylindrical processing chamber and Line cross-section, 15: center axis of the cylindrical processing chamber, 16: the direction of introduction of the cold air into the processing chamber 1, 17: heat treatment device of Comparative Example 5, 18: heat treatment device of Comparative Example 6

Claims (5)

A heat treatment apparatus for heat treating powder particles, wherein
The heat treatment apparatus
(1) A processing chamber having a cylindrical inner peripheral surface on which the heat treatment of the powder particles is performed,
(2) powder particle supply means for supplying the powder particles by a carrier gas for transporting 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 heat-treated powder particles;
(5) Control means provided in the processing chamber for controlling the flow of the hot air and the supplied powder particles;
(6) an outlet for discharging the heat-treated powder particles out of the processing chamber;
The hot air supply means comprises a turning member for adjusting the turning speed and the lowering speed of the hot air,
The restricting means is provided on the central axis of the cylindrical processing chamber so as to restrict the descending speed of the hot air or a mixed gas composed of the hot air and the powder particles and the carrier gas. And a columnar member having a circular cross section, which is disposed so as to protrude toward the end portion of the raw material supply means,
The outlet of the hot air supply means is provided opposite to the end of the regulation means on the side of the raw material supply means,
The powder particle supply means is provided at the outer peripheral portion of the processing chamber, and is introduced into the processing chamber from a cross section orthogonal to the central axis of the cylindrical processing chamber and the powder particle supply means outlet. When an angle formed by the introduction direction of the powder particles is α (°), the angle α (°) is
17 (°) ≦ α ≦ 37 (°)
Means for supplying the powder particles into the processing chamber so as to satisfy the condition and to rotate in the same direction as the hot air ,
The cold air supply means is provided on the outer periphery of the treatment chamber, and has a cross section orthogonal to the central axis of the cylindrical treatment room, and introduction of the cold air introduced into the treatment room from the cold air supply means outlet. When the angle formed by the direction is β (°), the angle β (°) is
17 (°) ≦ β ≦ 37 (°)
And a means for supplying the cold air so as to swirl in the same direction as the mixed gas . The angle α (°) is
22 (°) ≦ α ≦ 32 (°)
Satisfied
The angle β (°) is
22 (°) ≦ α ≦ 32 (°)
The heat treatment apparatus according to claim 1, characterized in that   The heat treatment apparatus according to claim 1 or 2, wherein a plurality of the powder particle supply means are provided, and the number of the cold air supply means is equal to or greater than the number of the powder particle supply means.   The heat treatment apparatus according to any one of claims 1 to 3, wherein the powder particles contain a binder resin, a colorant, and a wax.   A method for producing powder particles, comprising a heat treatment step of heat treating powder particles using a heat treatment apparatus, characterized in that the heat treatment apparatus is the heat treatment apparatus according to any one of claims 1 to 4. Method of producing powder particles.

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