JP2010091647A - Toner manufacturing device and method for manufacturing toner - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a toner manufacturing device which can obtain stable toner even in the case of start/stop thereof is repeated. <P>SOLUTION: The device comprises: a carrying means carrying raw materials to a raw material feeding means; the raw material feeding means for feeding the raw materials into a heat treating apparatus. The heat treating apparatus comprises a hot air feeding means feeding hot air for heat-treating the fed raw materials. The hot air feeding means is annularly provided at a position at intervals to the adjacent or horizontal direction of the outer circumferential face of the raw material feeding means. The raw material feeding means is composed in such a manner that the raw materials exhausted from the outlet of the raw material feeding means are exhausted toward the hot air fed from the hot air feeding means. The carrying means comprises: a first compressed gas feeding means continuously introducing compressed gas; and a second compressed gas feeding means intermittently introducing compressed gas. <P>COPYRIGHT: (C)2010,JPO&amp;INPIT

Description

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

  In image forming methods such as electrophotography, electrostatic photography, and electrostatic printing, toner for developing an electrostatic charge image is used.

  In general, the toner production method uses as a raw material a binder resin for fixing to a transfer material, various colorants for producing a color as a toner, and a charge control agent for imparting electric charges to particles. Accordingly, for example, other additives such as a release agent and a fluidity-imparting agent are added and dry-mixed. Then, after melt-kneading with a general-purpose kneader such as a roll mill, an extruder, etc., cooling and solidifying, the kneaded product is coarsely pulverized with a coarse pulverizer such as a hammer mill, a pin mill, a speed mill, etc. Toner particles are obtained by fine pulverization by various pulverization apparatuses such as a jet airflow pulverizer and a mechanical collision pulverizer. The obtained toner particles are a method of obtaining toner particles having a desired particle diameter using various air classifiers as required.

  Alternatively, the toner composition dissolved in a solvent is suspended in water, and then the solvent is distilled off to obtain toner particles. The emulsion obtained by emulsion polymerization is added with other materials such as a colorant, and the emulsion A method of agglomerating and associating toner particles to obtain toner particles, vinyl monomers such as styrene and n-butyl acrylate, colorants, and waxes (if necessary, polar resins, crosslinking agents, charge control agents, chain transfer agents) , Other additives) are uniformly dissolved or dispersed into a polymerizable monomer composition, and then the polymerizable monomer composition is mixed with an aqueous medium (for example, an aqueous phase) containing a dispersion stabilizer such as calcium phosphate. ) In a suitable high-speed stirrer, complete the suspension polymerization reaction using a polymerization initiator in a nitrogen atmosphere, and filter, wash, and dry the toner particles. It can be employed a variety of methods, such as that way.

  Furthermore, the obtained toner particles are added with a fluidizing agent, a lubricant, an abrasive or the like as necessary, and are dry-mixed to obtain a toner for image formation. In the case of a toner used in the two-component development method, various magnetic carriers and the above toner are mixed and then used for image formation.

  However, in recent years, with high image quality and high definition of copying machines, printers, etc., the performance required for toner as a developer has become more severe. Then, the particle diameter of the toner is reduced, and the toner particle size distribution is demanded to be sharp with no coarse particles and few ultrafine particles.

  In addition to the widespread use of color machines, as transfer materials, there are various materials such as plain paper and overhead projector films that have been used in the past, as well as thick paper such as glossy paper, cards, and small-size paper such as postcards. It has come to be used. As a countermeasure, the case where a transfer system using an intermediate transfer body is adopted on the main body side is increasing.

  Usually, in the transfer system using an intermediate transfer member, a visualized toner image is transferred from the image carrier to the intermediate transfer member, and then transferred from the intermediate transfer member to the transfer material. For toner, improvement in transfer efficiency is required.

  As a method for improving the toner transfer efficiency, studies have been made to make the toner spherical. Known methods for spheroidizing toner include, for example, polymerizing toner such as suspension polymerization and emulsion polymerization, and spheroidizing a pulverized toner.

  However, in the case of having an existing pulverization toner plant, a new toner plant is required to produce the polymerized toner. Furthermore, problems such as fixability and developability other than transferability may occur due to restrictions on material selection due to the polymerization method and the inclusion state of the additive material in the manufacturing process.

  In addition, in the method of spheroidizing by mechanical impact treatment, it is difficult to improve the spheroidization of the toner itself, although it is easy to add a processing device to an existing line, and there is a problem in terms of productivity. May occur.

  Under such circumstances, an apparatus and method for spheroidizing toner with hot air have been proposed (Patent Document 1). In this apparatus, fusion due to heating of particles is suppressed by installing a dispersion target for the purpose of dispersing the toner in the vicinity of the outlet of the toner supply unit. However, since the toner supply unit and the dispersion target are provided in the center of the hot air, the scale-up for the purpose of improving the toner productivity is more uniform in the heat treatment, and further against the start / stop / restart of the device. As a result, there may be a problem in that the toner adhering to the dispersion target exposed to hot air is fixed or mixed into the treated toner.

  As described above, various proposals have been made as to the method of spheroidizing the toner. In particular, the method and apparatus using hot air for the purpose of spheroidizing the toner produced by the pulverization method are versatile depending on the purpose. There is room for improvement.

The coarse particles, fine particles, and ultrafine particles in the toner particles described in the present specification are as follows.
Coarse particles: Particle group fine particles of about twice or more of the toner weight average diameter (D4): Particle group ultrafine particles of about ½ times or less of the toner weight average diameter (D4): measured by a flow type particle image analyzer 2 μm or less particles

JP 2004-276016 A

  An object of the present invention is to provide a toner heat treatment apparatus that can solve the above-described problems and obtain toner with higher definition and higher image quality.

  An object of the present invention is to provide a toner heat treatment apparatus capable of obtaining stable toner even when the apparatus is repeatedly started and stopped.

  An object of the present invention is to provide a toner heat treatment apparatus capable of performing processing in accordance with performance required for toner.

  An object of the present invention is to provide a heat treatment apparatus capable of stably producing a large amount of spherical toner.

  An object of the present invention is to provide a toner heat treatment apparatus that does not require a significant layout change in an existing manufacturing plant.

In order to achieve the above object, the present invention provides a toner production apparatus having a heat treatment apparatus for heat treating a toner,
The production apparatus includes a conveying means for conveying the raw material discharged from the raw material quantitative supply means to the raw material supply means, a raw material supply means for supplying the raw material into the heat treatment apparatus, and a heat treatment apparatus,
The heat treatment apparatus includes hot air supply means for supplying hot air for heat treating the supplied raw material, and the hot air supply means is adjacent to the outer peripheral surface of the raw material supply means or spaced apart from the horizontal direction. Provided in a ring at the position,
The raw material supply means is configured such that the raw material discharged from the outlet of the raw material supply means is discharged toward the hot air supplied from the hot air supply means,
The transport unit includes at least a first compressed gas supply unit that continuously introduces compressed gas, and a second compressed gas supply unit that intermittently introduces compressed gas. .

The present invention also relates to a method for producing a toner having a weight average diameter (D4) of 4 μm or more and 12 μm or less, comprising at least a heat treatment step.
The heat treatment step has at least a conveyance step of conveying the raw material discharged from the raw material quantitative supply step to the raw material supply step, a raw material supply step for supplying the raw material into the heat treatment apparatus, and a heat treatment step,
The heat treatment step includes a hot air supply step for supplying hot air for heat-treating the supplied raw material, and the hot air supply step is adjacent to the outer peripheral surface of the raw material supply step or spaced apart from the horizontal direction. The raw material supply step is configured such that the raw material that is annularly provided at the position and discharged from the outlet of the raw material supply step is discharged toward the hot air supplied from the hot air supply step,
The transport process includes at least a first compressed gas supply process that continuously introduces compressed gas and a second compressed gas supply process that intermittently introduces compressed gas.

  According to the present invention, it is possible to maintain a uniform processing state and obtain a desired sphericity without depending on the processing amount and the operation mode of the apparatus even when the toner is spheroidized by the heat treatment method. it can.

  In the past, as a result of research on heat treatment equipment for the purpose of controlling the sphericity of the toner, in order to increase the productivity of the heat treatment equipment, a unity called adhesion or fusion that occurs between toner particles. It is important to suppress the phenomenon. Further, an optimum apparatus configuration has been proposed on the assumption that it is important for the heat treatment apparatus to uniformly disperse the toner itself before processing and to control the temperature distribution in the apparatus.

  This time, we assumed the operation status when the device was actually installed on the toner production line, and focused on the actual operation and the quality when repeated stoppages occurred, and the stability of the device, the following results were obtained. Obtained.

The heat treatment system includes a conveying means for conveying the raw material discharged from the raw material quantitative supply means to the raw material supply means, a raw material supply means for supplying the raw material into the heat treatment apparatus, and a heat treatment apparatus,
The heat treatment apparatus includes hot air supply means for supplying hot air for heat treating the supplied raw material, and the hot air supply means is adjacent to the outer peripheral surface of the raw material supply means or spaced apart from the horizontal direction. Provided in a ring at the position,
The raw material supply means is configured such that the raw material discharged from the outlet of the raw material supply means is discharged toward the hot air supplied from the hot air supply means,
It is important that the transport means includes at least a first compressed gas supply means for continuously introducing a compressed gas and a second compressed gas supply means for intermittently introducing the compressed gas.

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

  First, the flow when this apparatus is introduced will be described. FIG. 1 is a flow chart showing one example when a heat treatment apparatus according to the present invention is introduced.

  Depending on the purpose of the processing, the raw material stocker (1) is filled with toner particles or toners produced by various manufacturing methods, and is supplied by a quantitative feeder (2) through a transport system (3) to a heat treatment device (4). To be introduced into the powder introduction tube. At this time, the compressed air introduced from the air flow feeder (5) is continuously supplied from the ejector (6) to the transport system (3) and is intermittently supplied from the ejector (7). The toner particles or toner accelerated by the compressed air is dispersed into the apparatus from the powder introduction tube outlet. 2 and 3 are diagrams schematically showing the arrangement of the ejector (6) and the ejector (7). The ejector (6) and the ejector (7) may be arranged close to the quantitative feeder (2) as shown in FIG. 2, but preferably close to the quantitative feeder (2) as shown in FIG. It is preferable to arrange the ejector (6) and arrange the ejector (7) in the middle of the transfer pipe of the transport system. In particular, when the transfer distance is long, or when the transfer pipe is raised or lowered due to equipment layout, or when the direction is changed, the effect of flowing the powder to be transferred smoothly by placing it in that part is also produced. .

  The temperature of the compressed air introduced is not more than the toner Tg, preferably Tg minus 10 ° C. or less, more preferably Tg minus 20 ° C. or less. When the temperature of the compressed air is higher than the Tg of the toner, aggregation or fusion due to heat occurs in the powder introduction tube and the outlet, the inside of the apparatus, and the like, which may cause a problem in the stability of the apparatus.

Furthermore, if necessary, the compressed air can be changed to an inert gas such as N ₂ gas.

  The dispersed toner particles or toner is heat-treated with hot air supplied from the air flow feeder (8).

  The temperature of the hot air introduced can be adjusted to 100 ° C. or higher and 450 ° C. or lower, and can be changed as needed according to the toner prescription. Although it is possible in terms of apparatus to set the temperature of the hot air to less than 100 ° C., problems may occur in terms of uniformity of heat treatment and productivity. Further, when the temperature of the hot air exceeds 450 ° C., it is difficult to increase the size of the hot air generator itself and to adjust the thermal energy received by the toner particles or toner during processing. Similarly, the temperature inside the apparatus cannot be sufficiently controlled, and a fusing phenomenon may occur.

  The toner or toner particles heated by the hot air is adjusted so as to receive arbitrary heat energy by the cold air supplied from the air flow supply device (9), and then sucked and transported to the recovery device (10).

At this time, the cold air is supplied in an annular shape around the outer periphery of the hot air. Further, if necessary, the second cold air may be supplied from the circumferential direction of the central portion of the toner manufacturing apparatus. At this time, compressed air or N ₂ gas dehumidified can be used as the cold air. In addition, the temperature of the cold air is preferably −100 ° C. or more and 60 ° C. or less, and more preferably −for the purpose of constructing an optimum temperature distribution in the device by interaction with the air flow introduced into the device. It is 20 degreeC or more and 20 degrees C or less. If the temperature itself is too high or too low, excessive energy may be required for the heat treatment, and further, the treatment itself may be non-uniform.

  In the recovery device (9), the target powder is recovered to the product stocker (10) via a pipe provided at the lower portion of the recovery device (9) and / or a damper, a double damper, a rotary valve, or the like. The powder that has not been collected by the collection device is collected by a filter cloth or the like provided on the bag (11) and collected in the bag stocker (12). The collected bug powder can be reused.

Furthermore, for the purpose of improving the dispersion state in the apparatus, compressed air or N ₂ gas can be supplied to the powder introduction pipe from the air flow supply machine (8) or the air flow supply machine (15) to the powder supply pipe.

  Next, the heat treatment apparatus used in the present invention will be described. FIG. 4 is a sectional view showing an example of a heat treatment apparatus according to the present invention. The outer periphery of the apparatus is designed with a maximum diameter of 500 mm, a height from the bottom of the lower transfer pipe to the top plate (powder introduction pipe outlet) of about 1500 mm, and a cone angle of 70 ° toward the discharge pipe at the lower part of the apparatus.

  The outer periphery of the main body and the powder introduction tube are provided with a cooling jacket (104). FIGS. 5 and 6 are examples of the powder introduction tube. The powder introduction tube of FIG. 5 is designed with a receiving side opening diameter of Φ45 mm, an outlet side (injection side in the apparatus) opening diameter of Φ15 mm, and a length of 450 mm for receiving toner particles or toner sent from the transport system. The powder introduction tube of FIG. 6 is designed with a receiving side opening diameter of Φ45 mm, an outlet side (injection side in the apparatus) opening diameter of Φ45 mm, and a length of 450 mm. It has a diffusion air introduction tube of Φ18 mm inside, and a hole of Φ1 mm at the bottom. Multiple conical plates are attached. The powder introduction tube including the cooling jacket is designed with an outer diameter of Φ100 mm. The powder introduction tube is inserted from above into a folder having a heat insulation layer provided on the main body top plate, and is fixed at a predetermined position by packing such as an O-ring or a screw.

  The toner particles or toner supplied to the powder introduction pipe (100) is continuously fed from the ejector (6) to be introduced into the heat treatment apparatus (4) via the transport system (3) by the fixed quantity feeder (2). The air is accelerated by the compressed air supplied and intermittently supplied from the ejector (7), and is dispersed into the apparatus from the outlet of the powder introduction pipe (100).

  Thereafter, heat treatment is performed by hot air supplied from a hot air introducing portion (101) provided annularly at a position adjacent to the outer peripheral surface of the outlet of the powder introduction tube (100) or at a distance from the horizontal direction.

  As can be seen from FIG. 4, in this apparatus, a distance is provided by providing a cooling jacket (104) and a heat insulating material (105) between the outlet of the powder introduction pipe (100) and the hot air introduction part (101). This increases the amount of treatment and increases the concentration of the powder to be treated in the vicinity of the outlet, which is effective for coalescence (increase in coarse particles) and non-uniformity of the heat treatment itself.

  That is, this is because it is easy to balance the distance required for the particles to be dispersed in the apparatus from the outlet and the energy (heat amount) required for the heat treatment. When the processing amount is small, the amount of compressed air given for dispersion is small, and the hot air necessary for the processing can be controlled to a desired circularity at a low temperature and in a small amount. For this reason, the positional relationship of the introduction part does not matter so much.

  However, when the processing amount is increased, the dust concentration in the vicinity of the outlet increases under the same conditions, which causes inconvenience for the processing. As a countermeasure for this, when the amount of compressed air is increased and the dust concentration is lowered, when a hot air introduction part is provided near the outlet, the hot air itself is affected by the compressed air, and the spheroidizing process at the assumed processing position and temperature is performed. It will not be done.

  As a countermeasure, in this apparatus, an interval of at least 20 mm, preferably 50 mm or more is provided between the supply unit outlet (100) and the hot air introduction unit (101). By doing so, the toner particles or toner ejected from the outlet of the supply unit is dispersed from the high speed state of the outlet to follow the flow of the air current in the apparatus, and then subjected to treatment with hot air.

  The heat-treated toner particles or toner has a cold air introduction part (102) provided in an annular shape on the outer periphery of the hot air introduction part (101) and a second cold air introduction part (102 provided in the circumferential direction of the central part as necessary. ) Is cooled by cold air introduced into the apparatus.

  When toner particles or toner is spheroidized by this apparatus, the flow rate and temperature of each airflow (compressed air, hot air, cold air, etc.) are controlled according to the desired sphericity. Specifically, for example, when the circularity is desired to be relatively low, the compressed air is increased. Alternatively, the temperature of the hot air is lowered. Or it can be adjusted by lowering the temperature of the cold air or increasing the flow rate. Conversely, when it is desired to obtain a high degree of circularity, for example, 0.975 or more in the FPIA 3000 measurement value, the compressed air is decreased. Or, increase the temperature of the hot air. Alternatively, it can be adjusted by increasing the temperature of the cold air or decreasing the flow rate.

Next, a transport system (3) that is a feature of the present apparatus will be described. The original purpose of this system is to achieve stable heat treatment even when the device is repeatedly operated and stopped when transferring toner particles or toner discharged from the metering feeder (2) into the heat treatment device. It is. As for conveyance, toner particles or toner and compressed air (in some cases N ₂ gas) move while being mixed in the transfer pipe. At this time, the pipe diameter is designed to be small to some extent in consideration of the powder velocity at the outlet of the apparatus. Specifically, it is equivalent to the supply part outlet diameter or the supply part inlet diameter.

  In addition, for normal operation of the apparatus, the apparatus is operated from the exhaust side apparatus (in this case, the blower), and the other auxiliary facilities are sequentially operated, and then the toner particle or toner quantitative supply device is operated.

  Further, at the time of stoppage, after stopping the toner particle or toner fixed quantity supply machine, the other incidental equipment is sequentially stopped, and finally the exhaust side device (blower in this case) is stopped.

  As described above, when considering the order of operation and stoppage of the quantitative feeder, toner particles or toner drawn from the piping to the outlet side by blower suction may be accumulated during re-operation. Further, when the stop time becomes long, it is considered that the apparatus is affected by the temperature in the apparatus and is thermally agglomerated or fused. As a countermeasure, a method of forcibly discharging the toner particles or toner remaining in the pipe by delaying the compressed air interruption at the time of stop until immediately before the stop of the blower can be considered. However, in this method, during operation, the amount of toner particles or toner supplied in the initial stage adheres to the inside of the pipe, thereby reducing the amount supplied into the apparatus. For this reason, excessive spheronization processing is performed under the assumed processing conditions. The same applies to the case where toner particles or toner remaining in the pipe forcibly after stopping is supplied into the apparatus.

  Therefore, in the present conveyance system (3), the compressed air continuously introduced from the air flow feeder (5) for the purpose of conveying and dispersing toner particles or toner, and the toner remaining in the pipe and in the vicinity of the outlet of the supply unit. It is provided with intermittently supplied compressed air for the purpose of discharging particles or toner into the apparatus during operation.

  The compressed air that is intermittently supplied is arbitrarily set to ON / OFF by a solenoid valve or the like. An effective setting for discharging residual toner particles or toner into the operating device is, for example, device scale such as ON for 0.1 second OFF for 0.1 second and ON for 1 second OFF for 1 second. And adjust according to the processing amount.

At this time, it is preferable that the gas flow rate A (m ³ / min) supplied intermittently and the gas flow rate B (m ³ / min) supplied continuously have the relationship of the following formula (1).
Formula (1) 0.1B <= A <= 0.9B

  When the intermittently supplied gas flow rate (compressed air amount) A is less than 0.1B, the discharge of the residue that is the original purpose may be insufficient. In addition, when the amount of compressed air A that is intermittently supplied exceeds 0.9B, there is no problem with the discharge of the residue, which is the original purpose, but the fluctuation in the dust concentration at the outlet is increased. In some cases, the process becomes non-uniform and it is difficult to adjust the circularity.

  Next, an outline of a heat treatment apparatus that easily exhibits the effect of the present invention will be described with reference to FIG.

  The toner particles or toner supplied to the powder introduction tube (201) is accelerated by compressed air, and is provided at the outlet of the powder introduction tube (201), the first nozzle (202) and the second nozzle ( 203) and is injected in a ring shape toward the radially outer side in the apparatus. Further, a tubular member 1 (204) and a tubular member 2 (205) are provided inside the powder introduction pipe (201), and compressed air is also supplied to the inside of each. The compressed air that has passed through the tubular member 1 (204) passes through a space formed by the first nozzle (202) and the second nozzle (203). The tubular member 2 (205) penetrates the second nozzle (203), and compressed air is jetted from the outlet of the tubular member 2 (205) toward the inner surface of the second nozzle (203) inside the second nozzle (203). Is done.

  In this apparatus, a hot air introduction part (206) is provided in an annular shape outside the powder introduction pipe (201), and further, the heat-treated toner particles or toner is cooled on the outside and downstream side. Cold air introduction portions 1 (207), 2 (208), and 3 (209) are provided for preventing toner particles from coalescing and fusing due to the temperature rise.

  Furthermore, it is preferable that the cold air introducing portions 1 (207), 2 (208) and 3 (209) are individually divided into a plurality of parts. In this apparatus (FIG. 7), each is divided into four parts to introduce cold air into the apparatus. By doing so, it is possible to finely adjust the amount of air flow in the apparatus and the deviation of the temperature distribution by adjusting each introduction amount.

  The hot air introduction part (206) is provided in an annular shape at a position spaced apart from the outer peripheral part of the powder introduction pipe (201) in the horizontal direction. This is because the outlet portions of the first and second nozzles are heated by the supplied hot air to prevent the toner particles ejected from the outlet portions from melting and adhering.

  In the apparatus of the present invention, the downstream end of the first nozzle (202) provided at the outlet portion of the powder introduction pipe (201) is more preferably located below or at the same position as the downstream end of the hot air introduction portion (206).

  This is a flow in which the toner particles or toner injected into the apparatus generate turbulent flow at the outlets of the first nozzle (202) and the second nozzle (203) and wind up to the upper part of the apparatus. This is because when the toner particles are melted by the supplied heat, the toner particles are liable to stay in the upper part of the apparatus, and the heat-treated toner particles exist for a long time, thereby creating a state where they are easily united. In addition, there is a concern that when melted toner particles in the flow of winding adhere to the upper surface of the apparatus, it may lead to fusion.

  In addition, the downstream end of the first nozzle (202) and the downstream end of the second nozzle (203) are preferably the same in the vertical direction, or the second nozzle (203) is more preferably located downstream. .

  This is because when the first nozzle (202) is positioned upstream, the toner particles or toner conveyed by the compressed air pass through the space formed by the first nozzle (202) and the second nozzle (203). In this case, the state of being annularly sprayed toward the hot air is small, and the toner particles passing through the supplied hot air are reduced. Conversely, when the second nozzle (203) is positioned below the first nozzle (202), the exit portion of the space formed by the first nozzle (202) and the second nozzle (203) faces the outside of the apparatus. Since the toner particles are more easily ejected toward the hot air, the heat treatment is sufficiently performed and the circularity tends to increase.

  The toner particles or toner ejected into the apparatus is made spherical by being ejected and heat-treated toward the hot air supplied from the hot air supply unit (206).

  In addition, the powder introduction pipe (201) and the first nozzle (202) are integrally configured, and the cooling efficiency can be improved by forming a jacket. In the path from the upstream side of the powder introduction pipe (201) to the first nozzle (202), the diameter of the portion connected to the first nozzle (202) is smaller than the diameter of the upstream end of the powder introduction pipe (201). Has been. A so-called tapered shape is more preferable. This is because the supplied toner particles or toner once accelerates the flow velocity at the entrance of the first nozzle (202), so that it becomes possible to further assist the dispersion of the toner particles or toner.

  The heat-treated toner particles or toner is cooled by cold air introduced from the cold air supply unit 1 (207). At this time, cold air may be introduced from the cold air supply unit 2 (208) provided on the side surface of the main body of the apparatus for the purpose of controlling the temperature in the apparatus and controlling the surface state of the toner particles. The exit part of the cool air supply means 2 (208) can use a slit shape, louver shape, perforated plate shape, mesh shape, etc., and the introduction direction is selected from the horizontal direction along the center direction and the direction along the device wall surface according to the purpose. Is possible.

  The apparatus of the present invention is provided with an air flow introduction part (209) for assisting the cooled toner particles or toner to be transferred to the recovery means (210) and for cooling the recovery means.

  A blower (not shown) is provided on the downstream side of the collecting means (210) and is sucked and conveyed by the blower.

  Next, the powder introduction tube will be described with reference to FIG.

  FIG. 8 is a partial cross-sectional perspective view showing an example of the powder introduction part (201) and each nozzle (202, 203) according to the present invention.

  As shown in FIG. 8, the powder introduction part (201) is cylindrical, and has a structure having a first nozzle (202) at the outlet. The path from the upstream side of the powder introduction part (201) to the first nozzle (202) has a tapered shape from upstream to downstream in the raw material supply direction. Furthermore, the powder introduction part (201) is entirely jacketed and has a cooling mechanism.

  A second nozzle (203) is provided inside the first nozzle (202).

  A tubular member 1 (204) is provided at the axial center of the powder introduction part (201), and the lower end of the tubular member 1 (204) is provided above the upper end of the second nozzle (203). Compressed air is introduced into the tubular member 1 (204), and the compressed air is jetted toward the outer surface of the second nozzle (203). The injected compressed air causes the toner particles that have passed through the space formed by the first nozzle (202) and the second nozzle (203) to be accelerated and further dispersed and injected into the apparatus.

  Further, a tubular member 2 (205) is provided inside the tubular member 1 (204), and the tubular member 2 (205) is connected to the second nozzle (203). The tubular member 2 (205) passes through the second nozzle (203) and reaches the inner surface, and a nozzle (211) for injecting compressed air toward the inner surface of the second nozzle (203) is provided at the downstream end. . Compressed air is applied to the flow of toner particles or toner ejected from the space composed of the first nozzle (202) and the second nozzle (203) toward the inner surface of the second nozzle (203) at the outlet. By ejecting, there is an effect of promoting the flow of toner particles or toner to the outside. As the nozzle, a spinning nozzle, spray nose (both manufactured by Spraying System Japan Co., Ltd.) and the like are used.

  In the case of the above-described apparatus configuration, it is excellent to disperse and inject toner particles or toner into the apparatus, but in order to exert the effect of compressed air amount, processing amount, and dispersion, the first nozzle ( 202) and the second nozzle (203) may be better narrowed. In this case, as pointed out in the present invention, the effect of increasing the stability at the time of restarting from the operation and stop of the apparatus is exhibited.

  As a method for producing a toner having a weight average diameter (D4) of 4 μm or more and 12 μm or less according to the present invention, finely pulverized or classified toner particles or toner added using a general production apparatus are used in this heat treatment system. If it processes and a desired circularity and a particle diameter are obtained, it will not specifically limit. When processing toner particles or toner having a weight average diameter (D4) of less than 4 μm, it may be difficult to balance the processing amount and the apparatus operating conditions. The same applies to processing of toner particles or toner having a weight average diameter (D4) exceeding 12 μm.

  Specifically, a binder resin, a colorant, a charge control agent, or a release agent as another additive is added, and a double-con mixer, V-type mixer, drum-type mixer, super mixer, Henschel mixer, Nauter Dry mixing with a mixer, pressure kneader, Banbury mixer, KTK type twin screw extruder manufactured by Kobe Steel, TEM type twin screw extruder manufactured by Toshiba Machine Co., Ltd. After being melt-kneaded using a bus-made co-kneader or the like, it is cooled through a cooling step of cooling by water cooling or the like. The cooled solidified product is coarsely pulverized with a crusher, hammer mill, feather mill, etc., and the resulting coarsely pulverized product is subjected to a collision-type airflow crusher such as a jet mill, micron jet, IDS type mill, kryptron, turbo mill, inomizer, etc. After finely pulverizing using a mechanical pulverizer, and obtaining a toner particle having a desired particle size distribution using an airflow classifier, etc., fine powder such as a fluidizing agent and an abrasive The toner of the present invention can be obtained by externally mixing the body.

  The spheronization process using the thermal spheronization apparatus of the present invention may be after the pulverization or classification, or after external addition. However, after the amount of fine powder is adjusted by classification treatment, the treatment can be made more uniform by treatment with a heat treatment apparatus. Therefore, preferably, classification is performed for the purpose of removing fine powder before treatment by the heat treatment apparatus, and rough treatment is performed after treatment. It is better to perform classification for the purpose of grain removal (corresponding to sieving is also possible).

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

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

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

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

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

  As the binder resin, the following polyester resins are also preferable.

  In the polyester resin, 45 to 55 mol% of all components is an alcohol component, and 55 to 45 mol% is an acid component.

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

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

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

Specifically, examples of magnetic materials include triiron tetroxide (Fe ₃ O ₄ ), iron sesquioxide (γ-Fe ₂ O ₃ ), iron oxide zinc (ZnFe ₂ O ₄ ), and iron yttrium oxide (Y ₃ Fe). ₅ O ₁₂ ), iron cadmium oxide (CdFe ₂ O ₄ ), iron gadolinium oxide (Gd ₃ Fe ₅ O ₁₂ ), copper iron oxide (CuFe ₂ O ₄ ), lead iron oxide (PbFe ₁₂ O ₁₉ ), nickel iron oxide (NiFe ₂ O ₄ ), neodymium iron oxide (NdFe ₂ O ₃ ), barium iron oxide (BaFe ₁₂ O ₁₉ ), magnesium iron oxide (MgFe ₂ O ₄ ), manganese iron oxide (MnFe ₂ O ₄ ), iron lanthanum oxide (LaFeO ₃ ), iron powder (Fe), cobalt powder (Co), nickel powder (Ni) and the like. The magnetic materials described above are used alone or in combination of two or more. A particularly suitable magnetic material is a fine powder of triiron tetroxide or γ-iron sesquioxide.

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

  The following are mentioned as a nonmagnetic coloring agent used by this invention.

  Examples of the black colorant include carbon black; those adjusted to black using a yellow colorant, a magenta colorant, and a cyan colorant.

  Examples of the color pigment for magenta toner include the following. Examples 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, 23, 30, 31, 32, 37, 38, 39, 40, 41, 48: 2, 48: 3, 48: 4, 49, 50, 51, 52, 53, 54, 55, 57: 1, 58, 60, 63, 64, 68, 81: 1, 83, 87, 88, 89, 90, 112, 114, 122, 123, 144, 146, 150, 163, 166, 169, 177, 184, 185, 202, 206, 207, 209, 220, 221, 238, 254, 269; I. Pigment violet 19, C.I. I. Bat red 1, 2, 10, 13, 15, 23, 29, 35 are mentioned.

  The colorant may be used alone as a pigment, but it is preferable from the viewpoint of the image quality of a full-color image to improve the sharpness by using a dye and a pigment together.

  Examples of the magenta toner dye include the following. C. I solvent red 1, 3, 8, 23, 24, 25, 27, 30, 49, 81, 82, 83, 84, 100, 109, 121, C.I. I. Disper thread 9, C.I. I. Solvent Violet 8, 13, 14, 21, 27, C.I. I. Oil-soluble dyes such as Disper 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.

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

  Examples of the color pigment for yellow include the following. 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, and 20 are mentioned. In addition, 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.

  Further, in the toner, it is preferable to use a toner obtained by mixing a colorant with a binder resin in advance to form a master batch. Then, the colorant can be favorably 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 to make a master batch, 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. Further, a toner having a large covering power on the transfer material can be obtained. Further, since the dispersibility of the colorant is improved, it is possible to obtain an image having excellent durability stability of toner chargeability and maintaining high image quality.

  The amount of the colorant used is preferably 0.1 to 30 parts by mass, more preferably 0.5 to 20 parts by mass, and most preferably 3 to 15 parts by mass with respect to 100 parts by mass of the binder resin. is there.

  In the toner of the present invention, a charge control agent can be used as necessary in order to further stabilize the chargeability. The charge control agent is preferably used in an amount of 0.5 to 10 parts by mass per 100 parts by mass of the binder resin. When the amount is less than 0.5 parts by mass, sufficient charging characteristics may not be obtained, which is not preferable. When the amount exceeds 10 parts by mass, compatibility with other materials is deteriorated or charging is performed under low humidity. It may be excessive, which is not preferable.

  Examples of the charge control agent include the following.

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

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

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

  Aliphatic hydrocarbon waxes such as low molecular weight polyethylene, low molecular weight polypropylene, microcrystalline wax, paraffin wax, and the like, or oxides of aliphatic hydrocarbon waxes such as oxidized polyethylene wax, or block copolymers thereof; And waxes mainly composed of fatty acid esters such as wax, sazol wax and montanic acid ester wax; and those obtained by partially or fully deoxidizing fatty acid esters such as deoxidized carnauba wax. In addition, saturated linear fatty acids such as palmitic acid, stearic acid, and montanic acid; unsaturated fatty acids such as brassic acid, eleostearic acid, and valinalic acid; stearyl alcohol, aralkyl alcohol, behenyl alcohol, carnauvir alcohol, and seryl alcohol Saturated alcohols such as melyl alcohol; long-chain alkyl alcohols; polyhydric alcohols such as sorbitol; fatty acid amides such as linoleic acid amide, oleic acid amide, and lauric acid amide; methylene bis stearic acid amide, ethylene biscaprin Saturated fatty acid bisamides such as acid amide, ethylene bislauric acid amide, hexamethylene bis stearic acid amide; ethylene bis oleic acid amide, hexamethylene bis oleic acid amide, N, N′-dioleyl Unsaturated fatty acid amides such as dipinamide, N, N-dioleyl sebacic acid amide; aromatic bisamides such as m-xylenebisstearic acid amide, N, N-distearylisophthalic acid amide; calcium stearate, laur Grafted with fatty acid metal salts such as calcium phosphate, zinc stearate, magnesium stearate (generally called metal soaps), and aliphatic hydrocarbon waxes with vinyl monomers such as styrene and acrylic acid. Examples of waxes include partially esterified products of fatty acids such as behenic acid monoglyceride and polyhydric alcohols, and methyl ester compounds having a hydroxyl group obtained by hydrogenation of vegetable oils and the like.

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

  The melting point of the releasing agent defined by the maximum endothermic peak temperature at the time of temperature rise measured by a differential scanning calorimeter (DSC) is preferably 65 to 130 ° C. More preferably, it is 80 to 125 ° C. If the melting point is less than 65 ° C., the viscosity of the toner decreases and toner adhesion to the photoreceptor is likely to occur. If the melting point exceeds 130 ° C., the low-temperature fixability may deteriorate, which is not preferable. .

  In the toner of the present invention, a fine powder that can be increased by adding the toner particles externally before and after the addition may be used as a fluidity improver. For example, fluorine resin powders such as vinylidene fluoride fine powder and polytetrafluoroethylene fine powder; wet production silica, fine powder silica such as dry production silica, fine powder titanium oxide, fine powder alumina, etc., silane coupling agent, titanium It is particularly preferable that the surface treatment is performed with a coupling agent and silicone oil, and the surface is hydrophobized, and the surface is hydrophobized as measured by a methanol titration test so as to show a value in the range of 30 to 80.

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

  In addition to the polishing effect, the toner of the present invention may contain inorganic fine powders other than those described above as chargeability and fluidity imparting and cleaning aids. By adding the inorganic fine powder externally to the toner particles, the effect can be increased more than before and after the addition. Examples of the inorganic fine powder used in the present invention include titanates and / or silicates such as magnesium, zinc, cobalt, manganese, strontium, cerium, calcium, and barium.

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

  The toner of the present invention can be used as a magnetic one component, a non-magnetic one component, or a two-component mixed with a carrier, but in order to achieve the effect of the present invention, it can be mixed with a magnetic carrier and used as a two-component. It is preferably used as a system developer.

  Examples of the magnetic carrier include iron powder whose surface is oxidized, non-oxidized iron powder, metal particles such as iron, lithium, calcium, magnesium, nickel, copper, zinc, cobalt, manganese, chromium, rare earth, and the like Magnetic material-dispersed resin carriers (so-called resin carriers) containing magnetic materials such as alloy particles, oxide particles, and ferrite, and magnetic materials and binder resins that hold the magnetic materials in a dispersed state Can be used.

  When the toner of the present invention is mixed with a magnetic carrier and used as a two-component developer, the carrier mixing ratio at that time is 2% by mass to 15% by mass, preferably 4% as the toner concentration in the developer. When the content is from 13% by weight to 13% by weight, good results are usually obtained. If the toner concentration is less than 2% by mass, the image density tends to decrease, and if it exceeds 15% by mass, fogging or in-machine scattering tends to occur.

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

(1) Measurement of particle size distribution The particle size distribution can be measured by various methods. In the present invention, the particle size distribution was measured using a multisizer of a Coulter counter.

<Measuring method of weight average particle diameter (D4) and number average particle diameter (D1)>
The weight average particle diameter (D4) and number average particle diameter (D1) of the toner are measured by a fine particle size distribution measuring apparatus “Coulter Counter Multisizer 3” (registered trademark, Beckman 2) Effective measurement channel number 25,000 using “Beckman Coulter Multisizer 3 Version 3.51” (manufactured by Beckman Coulter, Inc.) and attached dedicated software “Beckman Coulter Multisizer 3 Version 3.51” for measurement condition setting and measurement data analysis Measurement was performed on the channel, and the measurement data was analyzed and calculated.

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

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

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

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

  The specific measurement method is as follows.

  (1) About 200 ml of the electrolytic aqueous solution is put in a glass 250 ml round bottom beaker exclusively for Multisizer 3, set on a sample stand, and the stirrer rod is stirred counterclockwise at 24 rotations / second. Then, dirt and bubbles in the aperture tube are removed by the “aperture flush” function of the analysis software.

  (2) About 30 ml of the electrolytic aqueous solution is put in a glass 100 ml flat bottom beaker, and "Contaminone N" (nonionic surfactant, anionic surfactant, organic builder pH 7 precision measurement is used as a dispersant therein. About 0.3 ml of a diluted solution obtained by diluting a 10% by weight aqueous solution of a neutral detergent for washing a vessel (made by Wako Pure Chemical Industries, Ltd.) 3 times with ion exchange water is added.

  (3) Two oscillators with an oscillation frequency of 50 kHz are incorporated in a state where the phase is shifted by 180 degrees, and placed in a water tank of an ultrasonic dispersion device “Ultrasonic Dissipation System Tetora 150” (manufactured by Nikki Bios Co., Ltd.) having an electrical output of 120 W. A fixed amount of ion-exchanged water is added, and about 2 ml of the above-mentioned Contaminone N is added to this water tank.

  (4) The beaker of (2) is set in the beaker fixing hole of the ultrasonic disperser, and the ultrasonic disperser is operated. And the height position of a beaker is adjusted so that the resonance state of the liquid level of the electrolyte solution in a beaker may become the maximum.

  (5) In a state where the electrolytic aqueous solution in the beaker of (4) is irradiated with ultrasonic waves, about 10 mg of toner is added to the electrolytic aqueous solution little by little and dispersed. Then, the ultrasonic dispersion process is continued for another 60 seconds. In the ultrasonic dispersion, the temperature of the water tank is appropriately adjusted so as to be 10 ° C. or higher and 40 ° C. or lower.

  (6) To the round bottom beaker of (1) installed in the sample stand, the electrolyte solution of (5) in which the toner is dispersed is dropped using a pipette, and the measurement concentration is adjusted to about 5%. . The measurement is performed until the number of measured particles reaches 50,000.

  (7) The measurement data is analyzed with the dedicated software attached to the apparatus, and the weight average particle diameter (D4) and the number average particle diameter (D1) are calculated. When the graph / volume% is set with the dedicated software, the “average diameter” on the analysis / volume statistics (arithmetic average) screen is the weight average particle size (D4), and the graph / number% is set with the dedicated software. The “average diameter” on the analysis / number statistic (arithmetic average) screen is the number average particle diameter (D1).

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

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

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

For example, the volume% of particles of 10.0 μm or more in the toner is determined by performing the above-mentioned Multisizer 3 measurement.
(1) Graph / Volume% is set with dedicated software, and the measurement result chart is displayed as volume%. (2) Check “>” in the particle size setting part on the Format / Particle Size / Particle Size Statistics screen, Enter “10” in the particle size input section. (3) When the analysis / volume statistics (arithmetic average) screen is displayed, the numerical value of the “> 10 μm” display portion is the volume% of particles of 10.0 μm or more in the toner.
(2) Measurement of Average Circularity of Toner Particles The average circularity of toner particles was measured with a flow type particle image analyzer “FPIA-3000 type” (manufactured by Sysmex Corporation) under the measurement and analysis conditions during calibration work.

  As a specific measurement method, 0.05 ml of a surfactant, preferably alkylbenzene sulfonate, is added to 20 ml of ion-exchanged water, and then 0.02 g of a measurement sample is added, and the oscillation frequency is 50 kHz, electrical output. Dispersion treatment was carried out for 2 minutes using a 150 W tabletop type ultrasonic cleaner / disperser (for example, “VS-150” (manufactured by VervoCrea Co., Ltd.)) to obtain a dispersion for measurement. It cools suitably so that temperature may become 10 to 40 degreeC.

  The flow type particle image analyzer equipped with a standard objective lens (10 ×) was used for the measurement, and a particle sheath “PSE-900A” (manufactured by Sysmex Corporation) was used as the sheath liquid. The dispersion prepared in accordance with the above procedure is introduced into the flow type particle image analyzer, 3000 toner particles are measured in the total count mode in the HPF measurement mode, and the binarization threshold at the time of particle analysis is 85%. The analysis particle diameter was limited to a circle equivalent diameter of 2.00 μm or more and 200.00 μm or less, and the average circularity of the toner particles was determined.

  In the measurement, automatic focus adjustment is performed using standard latex particles (for example, Duke Scientific 5200A diluted with ion-exchanged water) before the measurement is started. Thereafter, it is preferable to perform focus adjustment every two hours from the start of measurement.

  In this embodiment, a flow type particle image analyzer which has been issued a calibration certificate issued by Sysmex Corporation, which has been calibrated by Sysmex Corporation, has an analysis particle diameter of 2.00 μm in equivalent circle diameter. The measurement was performed under the measurement and analysis conditions when the calibration certificate was received, except that it was limited to 200.00 μm or less.

(3) Melting | fusing point measurement of wax It measures using a differential thermal analysis measuring device (DSC measuring device) and DSC-7 (made by Perkin Elmer). The measurement is performed according to ASTM D3418-82. Precisely weigh 2 to 10 mg of the measurement sample and place it in an aluminum pan. Using an empty aluminum pan as a reference, measure it at a temperature rise rate of 10 ° C / min and normal temperature and humidity at a measurement temperature range of 30 to 200 ° C. I do. In this temperature raising process, an endothermic peak of a main peak in a temperature range of 30 to 200 ° C. is obtained. The temperature of this endothermic main peak is taken as the melting point of the wax.

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

  The sample to be measured is precisely weighed from 5 to 20 mg, preferably 10 mg. This is put into an aluminum pan, and an empty aluminum pan is used as a reference, and measurement is performed at a temperature rise rate of 10 ° C./min and normal temperature and humidity in a measurement temperature range of 30 to 200 ° C. In this temperature raising process, an endothermic peak of a main peak in a temperature range of 40 to 100 ° C. is obtained. At this time, the point of intersection between the base line midpoint before and after the endothermic peak and the differential heat curve is defined as the glass transition temperature Tg in the present invention.

(5) Measurement of molecular weight distribution of binder resin and molecular weight of chromatogram by GPC is measured under the following conditions.

The column is stabilized in a heat chamber at 40 ° C., and tetrahydrofuran (THF) as a solvent is allowed to flow through the column at this temperature at a flow rate of 1 ml / min. The sample is dissolved in THF, filtered through a 0.2 μm filter, and the filtrate is used as a sample. Measurement is performed by injecting 50 to 200 μl of a THF sample solution of a resin adjusted to a sample concentration of 0.05 to 0.6 mass%. In measuring the molecular weight of a sample, the molecular weight distribution of the sample is calculated from the relationship between the logarithmic value of a calibration curve prepared from several types of monodisperse polystyrene standard samples and the number of counts. As a standard polystyrene sample for preparing a calibration curve, for example, Pressure Chemical Co. Manufactured by Toyo Soda Kogyo Co., Ltd. and having molecular weights of 6 × 10 ² , 2.1 × 10 ³ , 4 × 10 ³ , 1.75 × 10 ⁴ , 5.1 × 10 ⁴ , 1.1 × 10 ⁵ , 3 .9 × 10 ⁵ , 8.6 × 10 ⁵ , 2 × 10 ⁶ , 4.48 × 10 ⁶ are used, and it is appropriate to use at least about 10 standard polystyrene samples. An RI (refractive index) detector is used as the detector.

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

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

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

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

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

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

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

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

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

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

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

(2) Operation 0.5 to 2.0 g of a sample is correctly weighed in a round bottom flask, and 5 ml of an acetylating reagent is correctly added thereto. A small funnel is put on the mouth of the flask, and the bottom is immersed in a glycerin bath at 95 to 100 ° C. to heat the bottom. At this time, in order to prevent the temperature of the neck of the flask from rising due to the heat of the bath, a cardboard disc with a round hole in it is put on the base of the neck of the flask. After 1 hour, the flask is removed from the bath, and after cooling, 1 ml of water is added from the funnel and shaken to decompose acetic anhydride. In order to further complete the decomposition, the flask was again heated in a glycerin bath for 10 minutes, allowed to cool, and then the funnel and the wall of the flask were washed with 5 ml of ethyl alcohol, and N / 2 potassium hydroxide ethyl alcohol using a phenolphthalein solution as an indicator. Titrate with solution. A blank test is performed in parallel with the main test. In some cases, a KOH-THF solution may be used as an indicator.

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

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

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

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

(Example of toner production: T-1)
Binder resin (polyester resin): 100 parts by mass (Tg 55 ° C., acid value 20 mgKOH / g, hydroxyl value 16 mgKOH / g, molecular weight: Mp4 500, Mn2300, Mw38000)
・ C. I. Pigment Blue 15: 3: 5 parts by mass, 1,4-di-t-butylsalicylic acid aluminum compound: 0.5 parts by mass, paraffin wax (maximum endothermic peak temperature 78 ° C.): 5 parts by mass After mixing well with a Henschel mixer (FM-75J type, manufactured by Mitsui Mining Co., Ltd.), 60 kg / hr at a biaxial kneader (PCM-45 type, manufactured by Ikekai Steel Co., Ltd.) set at a temperature of 130 ° C. It knead | mixed with the amount of Feed (the kneaded material temperature at the time of discharge is about 150 degreeC). The obtained kneaded product was cooled and coarsely crushed with a hammer mill, and then finely pulverized with a mechanical pulverizer (T-250: manufactured by Turbo Kogyo Co., Ltd.) at a Feed amount of 20 kg / hr.

  Further, the obtained toner finely pulverized product was classified by a multi-division classifier using the Coanda effect, to obtain test toner particles (T-1).

  The obtained toner particles (T-1) have a weight average particle size (D4) of 6.2 μm, 30.2% by number of particles having a particle size of 4.0 μm or less, and particles having a particle size of 10.1 μm or more. It was 0.6% by volume.

  Further, the average circularity measured by FPIA3000 was 0.936, and the particle content of 2 μm or less was 15.1%.

<Example 1>
Next, the compressed air introduced from the air flow feeder (5) is ejected from the toner particles (T-1) in the flow shown in FIG. (6) is continuously supplied at 1.5 m ³ / min, and the ejector (7) attached in the middle of the transfer pipe is repeatedly turned on for 0.5 seconds and turned off for 1.0 seconds. It was set to supply 0.5 m ³ / min. The compressed air at this time was 22 degreeC.

  The first nozzle ridge line angle α = 50 °, the second nozzle ridge line angle β = 70 °, the outermost diameter of the lower end of the first nozzle is Φ77 mm, the outermost diameter of the lower end of the second nozzle is Φ71 mm, The vertical distance H1 between the lower end and the lower end of the second nozzle was set to 5 mm, and the distance between the lower end of the first nozzle and the lower end of the hot air introducing portion was set to 10 mm. Furthermore, a spinning nozzle was installed on the inner surface of the second nozzle.

  The outermost diameter of the tubular member 1 was Φ15 mm, the outermost diameter of the tubular member 2 was Φ8 mm, and the lower end position of the tubular member was H3 = 5 mm with respect to the upper part of the second nozzle.

The operating conditions of the apparatus are as follows: hot air temperature 240 ° C, hot air flow rate 4.5m ³ / min, cold air 1, 2, 3 temperature 3 ° C, cold air 1 flow rate 3.0m ³ / min, cold air 2 flow rate 1.5m ³ / min, cold air 3 flow 3.0 m ³ / min, blower volume 20.0 m ³ / min, the tubular member 1 flow rate 0.4 m ³ / min, the tubular member 2 in a flow rate 0.2 m ³ / min, the cooling of 7 ° C. in the apparatus jacket I let water through.

  Under the above conditions, the metering feeder was adjusted so that the amount of toner particles fed was 15 kg / hr and then operated for 12 minutes, and then the feeder was stopped.

  The processed product collected from the product stocker is 2.6 kg, the weight average particle diameter (D4) is 6.3 μm, the particle diameter is 4.0 μm or less is 28.7% by number, and the particle diameter is 10.1 μm or more. The particles were 3.6% by volume.

  Further, the average circularity measured by FPIA3000 was 0.976, and the particle content of 2 μm or less was 3.1%.

  Furthermore, after 6 minutes of idle operation after stopping the feeder, the processed product recovered from the product stocker is 0.3 kg, the weight average particle size (D4) is 6.3 μm, and the particle size is 4.0 μm. The following particles were 28.4% by number, and particles having a particle size of 10.1 μm or more were 3.8% by volume.

  Moreover, the average circularity measured by FPIA3000 was 0.976, and the particle content of 2 μm or less was 2.9%.

  Next, the feeder was turned on again and after running for 3 minutes, the feeder was stopped.

  The processed product recovered from the product stocker is 0.7 kg, the weight average particle size (D4) is 6.3 μm, the particle size of 4.0 μm or less is 28.9% by number, and the particle size is 10.1 μm or more. The particles were 3.5% by volume.

  The average circularity measured by FPIA3000 was 0.976, and the particle content of 2 μm or less was 3.0%.

  Furthermore, as a result of carrying out the idle operation for 6 minutes after stopping the feeder, the processed product recovered from the product stocker is 0.1 kg, the weight average particle diameter (D4) is 6.3 μm, and the particle diameter is 4.0 μm. The following particles were 28.3% by number, and particles having a particle size of 10.1 μm or more were 3.9% by volume.

  The average circularity measured by FPIA3000 was 0.976, and the particle content of 2 μm or less was 3.0%.

  As a result, by intermittently introducing the compressed air into the supply system, the toner particles remaining in the supply pipe and the like are reduced, and the shake of the processed product itself before and after the operation of the apparatus is suppressed.

Incidentally, in this test, about 12% of the processed products were collected in stocker during operation and the processed products collected in stocker after stopping. In the present invention, in the present invention, the residual rate in the apparatus is calculated from the following formula.
Residual rate in equipment (%) = Total recovery during idle operation / (Recovery during 12-minute operation + Recovery during 3-minute operation)
(The total recovery amount during idle operation is the total recovery amount after 6 minutes after 12 minutes of operation and 6 minutes after operation of 3 minutes)

  This is because the processed product is recovered from the stocker immediately after the supply machine is stopped, so the toner in the transport path to the stocker includes unrecovered parts. It is thought that there is not.

<Comparative Example 1>
Compressed air introduced from the air flow feeder (5) is continuously supplied from the ejector (6) at 2.0 m ³ / min, and the supply from the ejector (7) attached in the middle of the transfer pipe is stopped. In the same manner as in Example 1, the toner particles (T-1) were processed with the configuration of FIGS. 3 and 7 in the flow of FIG. 1 which is a toner manufacturing apparatus.

  The metering feeder was adjusted so that the toner particle feed rate would be 15 kg / hr and then operated for 12 minutes, and then the feeder was stopped.

  The processed product recovered from the product stocker is 2.4 kg, the weight average particle size (D4) is 6.3 μm, the particle size is 4.0 μm or less 29.3% by number, and the particle size is 10.1 μm or more. The particles were 3.4% by volume.

  The average circularity measured by FPIA3000 was 0.976, and the particle content of 2 μm or less was 2.7%.

  Furthermore, after 6 minutes of idle operation after stopping the feeder, the processed product recovered from the product stocker is 0.5 kg, the weight average particle size (D4) is 6.4 μm, and the particle size is 4.0 μm. The following particles were 27.4% by number, and particles having a particle size of 10.1 μm or more were 4.2% by volume.

  The average circularity measured by FPIA3000 was 0.974, and the particle content of 2 μm or less was 2.9%.

  Next, the feeder was turned on again and after running for 3 minutes, the feeder was stopped.

  The processed product collected from the product stocker is 0.5 kg, the weight average particle size (D4) is 6.3 μm, 29.9% by number of particles having a particle size of 4.0 μm or less, and a particle size of 10.1 μm or more. The particles were 3.5% by volume.

  The average circularity measured by FPIA3000 was 0.977, the particle content of 2 μm or less was 2.5%.

  Furthermore, after 6 minutes of idle operation after stopping the feeder, the processed product recovered from the product stocker is 0.3 kg, the weight average particle size (D4) is 6.3 μm, and the particle size is 4.0 μm. The following particles were 29.3% by number, and particles having a particle size of 10.1 μm or more were 4.3% by volume.

  The average circularity measured by FPIA3000 was 0.976, and the particle content of 2 μm or less was 2.3%.

  From the results, it can be seen that when compressed air is not intermittently introduced into the supply system, there is a difference in the processed product before and after the operation of the apparatus due to the presence of toner particles remaining in the supply pipe or the like. Incidentally, in this test, the residual rate in the apparatus was about 30%.

  Furthermore, in this test, the supply amount is 15 kg / hr, but if the processing amount increases, the remaining amount is expected to increase.

<Examples 2 to 8 and Comparative Examples 2 and 3>
The toner particles (T-1) were prepared in the same manner as in Example 1 except that each configuration and compressed air conditions were changed as shown in Table 1 in the flow of FIG. The result was obtained. Examples 2 and 5 are examples in which A in Formula (1) exceeds 0.9B.

  In Example 2, the residual rate in the apparatus was reduced by making the continuous and intermittent compressed air amounts the same, but the airflow in the apparatus was slightly disturbed, so the coarse particles increased.

  In the third embodiment, testing is performed by changing the device configuration. Since the dispersion state of the toner particles in the apparatus was changed, changes in the circularity and the amount of coarse particles were observed, but the remaining ratio in the apparatus was in a range where there was no problem.

  In Example 4, the amount of air introduced intermittently was reduced in the amount of continuous and intermittent compressed air. As a result, the residual rate in the apparatus increased to the allowable range limit.

  In Example 5, the amount of air introduced intermittently was larger than the amount of air introduced continuously. As a result, the residual rate in the apparatus decreased, but the amount of air that was always dispersed decreased, resulting in an increase in circularity and an increase in the amount of coarse particles.

  In Example 6, in order to confirm the influence of the processing amount, the supply amount was set to 10 kg / hr. Since the processing amount is small, the residual rate in the apparatus is low, and the circularity is very high by the processing under the same conditions.

  In Examples 7 and 8, the intermittent air ON and OFF times were changed. When the ON time is short, the remaining rate without the apparatus increases, and when the ON time is long, the remaining rate decreases.

  In the present embodiment, since all the processing conditions are the same and tested, there is a difference in the degree of circularity of the state of processed goods depending on the state. As described above, the degree of circularity can be adjusted by adjusting hot air and cold air to be introduced, and in that case, the amount of coarse particles is considered to change.

  In Comparative Example 2, the supply rate was 10 kg / hr compared to Comparative Example 1. As a result, the residual rate in the apparatus was within the allowable range limit. This can be said to be a result that supports the improvement in stability when the processing amount is increased, which is the gist of the present invention.

  In Comparative Example 3, the device configuration is changed and tested. Since the dispersion state of the toner particles in the apparatus was changed, changes in the circularity and the amount of coarse particles were observed, but the residual ratio in the apparatus was as high as in Comparative Example 1.

It is the flowchart which showed one example of the heat processing apparatus of this invention. It is the schematic of the supply system of this invention. It is the schematic of the supply system of this invention. It is the schematic of the heat processing apparatus of this invention. It is the schematic of the supply part used for the apparatus of FIG. It is the schematic of the supply part used for the apparatus of FIG. It is the schematic of the heat processing apparatus of this invention. It is the schematic of the supply part used for the apparatus of FIG.

Explanation of symbols

1 Raw material stocker 2 Constant supply machine 3 Supply system 4 Heat treatment device (thermal spheronization device)
5 Airflow supply machine 1
6 Ejector (Compressed air supply machine 1)
7 Ejector (Compressed air supply machine 2)
8 Hot Air Supply Machine 9 Cold Air Supply Machine 10 Collection Device 11 Processed Product Stocker 12 Bug 13 Bug Collection Stocker 14 Blower 15 Airflow Supply Machine 2
100 Powder / Air Flow Supply Unit 101 Hot Air Supply Unit 102 Cold Air Supply Unit 103 Transport Air Flow Supply Unit 104 Cooling Jacket 105 Insulating Material 106 Cooling Jacket 107 Diffusion Air Introduction Unit 201 Powder / Air Flow Supply Unit 202 First Nozzle 203 Second Nozzle 204 Tubular member 1
205 Tubular member 2
206 Hot air introduction part 207 Cold air introduction part 1
208 Cold air introduction part 2
209 Cold air introduction part 3
210 Collection line

Claims (6)

A toner manufacturing apparatus having a heat treatment apparatus for heat treating toner,
The production apparatus includes a conveying means for conveying the raw material discharged from the raw material quantitative supply means to the raw material supply means, a raw material supply means for supplying the raw material into the heat treatment apparatus, and a heat treatment apparatus,
The heat treatment apparatus includes hot air supply means for supplying hot air for heat treating the supplied raw material, and the hot air supply means is adjacent to the outer peripheral surface of the raw material supply means or spaced apart from the horizontal direction. Provided in a ring at the position,
The raw material supply means is configured such that the raw material discharged from the outlet of the raw material supply means is discharged toward the hot air supplied from the hot air supply means,
An apparatus for producing toner, wherein the conveying means comprises at least first compressed gas supply means for continuously introducing compressed gas and second compressed gas supply means for intermittently introducing compressed gas. The gas flow rate A (m ³ / min) intermittently supplied from the second compressed gas supply means and the gas flow rate B (m ³ / min) continuously supplied from the first compressed gas supply means are expressed by the following equation (1): The toner manufacturing apparatus according to claim 1, wherein
Formula (1) 0.1B <= A <= 0.9B   The raw material supply means has a first nozzle and a second nozzle that expand in a tapered shape from the upstream to the downstream in the raw material supply direction at the outlet, and the second nozzle is the first nozzle. 3. The toner manufacturing method according to claim 1, wherein the supplied raw material passes through a space formed by the first nozzle and the second nozzle. apparatus. In a method for producing a toner having a weight average diameter (D4) of 4 μm or more and 12 μm or less, comprising at least a heat treatment step,
The heat treatment step has at least a conveyance step of conveying the raw material discharged from the raw material quantitative supply step to the raw material supply step, a raw material supply step for supplying the raw material into the heat treatment apparatus, and a heat treatment step,
The heat treatment step includes a hot air supply step for supplying hot air for heat-treating the supplied raw material, and the hot air supply step is adjacent to the outer peripheral surface of the raw material supply step or spaced apart from the horizontal direction. The raw material supply step is configured such that the raw material that is annularly provided at the position and discharged from the outlet of the raw material supply step is discharged toward the hot air supplied from the hot air supply step,
The method for producing toner, wherein the conveying step includes at least a first compressed gas supply step for continuously introducing compressed gas and a second compressed gas supply step for intermittently introducing compressed gas. The gas flow rate A (m ³ / min) intermittently supplied in the second compressed gas supply step and the gas flow rate B (m ³ / min) continuously supplied in the first compressed gas supply step are expressed by the following formula ( The toner production method according to claim 4, wherein the relationship is 1).
Formula (1) 0.1B <= A <= 0.9B   The raw material supply step has a first nozzle and a second nozzle that expand in a tapered shape from the upstream to the downstream in the raw material supply direction at the outlet portion, and the second nozzle includes the first nozzle 6. The toner production according to claim 4, wherein the supplied raw material passes through a space formed by the first nozzle and the second nozzle. Method.

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