JP4732276B2 - Cyclone classifier, airflow drying system and toner - Google Patents

Description

  The present invention relates to a cyclone apparatus for classifying and collecting powder, and more particularly to a cyclone classifier, an airflow drying system, and a toner for drying and producing toner as powder.

  In recent years, there has been a growing demand for higher functionality for powders, and there is a demand for particles having a small diameter and a narrow particle size distribution range. The state in which the particle size is distributed over a relatively wide range in the powder is the cause of variations in the various functions imparted to the powder particle, and having a more uniform particle size contributes to higher functionality of the powder. It is considered preferable. A toner used for electrophotography is one example, and a wide particle size distribution width is disadvantageous for necessary performance such as uniform charging and uniform melting.

  Many classification methods are known as means for aligning powders with a uniform particle size. As the known classification technique, there is a technique using a cyclone collector. Usually, cyclone collectors are used as solid-gas (solid-gas) separation devices. The powder particles that flow into the cyclone classifier in the air current are subjected to a centrifugal effect due to the swirling flow in the cyclone classifier, accumulate on the outer cylinder wall side of the cyclone classifier, and gradually fall down, and the cyclone classifier outer cylinder It is collected in a container installed underneath. A gas (generally air) that is much lighter than particles is discharged (exhausted) out of the cyclone classifier from the inner cylinder in the center of the cyclone classifier.

  There is also known a technique used as a classifier using the cyclone collector for solid-gas separation and used to discharge small particles together with gas. The cyclone collector itself is used for solid-gas separation, powder conveyance, etc. The classification process is incorporated separately by providing such equipment not only as a collector but also as a classifier. Since there is no need, the capital investment and the reduction of man-hours are significant advantages.

The powder handled by the cyclone collector has a particle size of 1 mm or less, and more specifically, it is generally intended for a range from several μm to several hundred μm.
For example, as such a technique, there is a technique in which a cylinder with a fine hole is installed between an outer cylinder and an inner cylinder of a cyclone collector and classified by a filter effect (see, for example, Patent Document 1). . In addition, a slide plate with variable opening width of the introduction part to the cyclone collector is installed, and the conical apex is opposed to the lower end of the outer cylinder. Is disclosed (for example, refer to Patent Document 2). Furthermore, an orifice-shaped baffle plate having an opening smaller than the opening opening area of the inner cylinder is installed at the central part on the concentric axis with the outer cylinder, and the powder-containing airflow is transferred to the center of the cylinder by this partition plate. A technique is disclosed in which the flow rates are increased and assembled (see, for example, Patent Document 3).
Japanese Patent Laid-Open No. 10-230223 JP-A-8-266938 JP 2004-283720 A

  However, when using a cyclone as a classifier, it is important to control the classification particle size by providing a function that can be finely adjusted as in the above technology. This is how the powder particle size is distributed in ascending order from the center of the outer cylinder of the cyclone classifier toward the outer periphery by the centrifugal force applied to the powder particles. As the classification (classification) by the particle diameter in the radial direction is more accurate and distributed in a wider range in the radial direction, the classification accuracy by exhaust suction from the inner cylinder increases. In addition, the recovered powder has a narrower particle size distribution width and can be collected better. On the contrary, if classification (classification) by the particle size in the radial direction is not performed, the yield is extremely deteriorated in order to obtain a desired narrow particle size distribution width, and further, the desired narrow particle size is obtained. Situations where it is not possible to have a distribution width can occur.

  The greater the mass of the powder particles, that is, the larger the particle size, the stronger centrifugal force is applied, and a greater force acts in the direction from the outer cylinder central axis toward the outer periphery. By effectively utilizing this force, small particles are distributed in the center of the outer cylinder of the cyclone classifier, that is, in the vicinity of the inner cylinder as the exhaust port, and large particles are distributed in the outer periphery. In an ideal state, the particles are distributed almost continuously in the order of particle diameter. Considering this point and adjusting the classification point using an adjustment mechanism on the equipment, it is possible to provide a classification device having a desired narrow particle size distribution width and good yield and a classification process. In other words, it is only necessary to have a prescribed distribution in the order of the particle diameter from the center of the outer cylinder to the outer periphery. Otherwise, no matter how much the classification point is adjusted using the adjustment mechanism on the equipment, classification is not possible. Is possible.

For example, in the technique described in Patent Document 2, it is possible to install a slide plate that can change the opening width of the introduction portion to the cyclone collector, and to narrow the introduction port width. Centrifugal force has already been received in a state where particles of all particle sizes are mixed and gathered in the vicinity of the wall surface, and classification from this state is difficult.
In fact, none of the above-mentioned known techniques is a mechanism that takes into consideration the distribution in the order of particle diameters.

The present invention has been made paying attention to the fact that the particles can be classified if they are arranged in the order of the particle diameters in the radial direction. In particular, the present invention is a raw material for electrophotographic toner as classified particles. When colored polymer particles are used, the cyclone collector of the present invention can efficiently obtain a powder having a desired particle size distribution width with a very high yield, for example, when polymerized toner is classified. In the process of drying the wet colored polymer particles, using a gas flow dryer, and the cyclone collector of the present invention when separating the powder after drying into a solid-gas separation, a classification process while performing the drying process Can be performed. Or it can also be set as the combination which performs a classification process using the apparatus of this invention as a classification process separately after a drying process.
In other words, an object of the present invention is to provide a cyclone classifier, an air flow drying system, and a toner that can separate powder particles having a narrow distribution width with a high yield in order to solve the above-described problems.

  In order to obtain a high-quality and high-quality toner, the present inventors dissolve or disperse a toner composition comprising at least a resin and a colorant in an organic solvent, and emulsify and wash the dissolved or dispersed material in an aqueous medium. In the step of classifying the colored polymer particles solid-gas separated in the cyclone classifier after drying the water-containing cake that has been solid-liquid separated using an air-flow dryer, classification is performed using a cyclone classifier. The present inventors have intensively studied conditions for obtaining colored polymer particles having a narrow particle size distribution with a high yield, and have achieved the present invention.

  According to the present invention, a cyclone classifier consisting of an outer cylinder and an inner cylinder can be used to accurately and widely distribute the radial alignment according to the particle size, so that a desired narrow particle size distribution width can be obtained with a high yield. A powder can be obtained.

That is, according to the present invention, the following (1) to (14) are provided.
(1) An outer cylinder composed of a cylindrical outer cylinder body and an outer cylinder bottom part that is an inverted conical shape connected vertically below the outer cylinder body, and an exhaust port configured in multiple layers by multiple tubes In the cyclone classifier formed of a cylinder, the cylinder has a reduced part made of a cylindrical or orifice-shaped baffle with an inner diameter reduced to an arbitrary height in the outer cylinder body part, and the lower end part of the inner cylinder has the above-mentioned It exists in a cylindrical space (cylindrical part) that is connected vertically below the reduction part, and a plurality of the cylindrical part and the reduction part exist in the outer cylinder body part, and are provided in the outer cylinder body part. The cyclone classifier according to claim 1, wherein a lower end portion of each tube of an inner cylinder composed of multiple tubes exists in each of the plurality of cylindrical portions in the cylindrical portion and the reduction portion .
(2) The cyclone classifier according to (1), wherein the position of the lower end portion of the inner cylinder is adjustable.
(3) The diameter De of the cylindrical portion is such that the diameter of the reduced portion (when the reduced portion is a cylinder with a reduced inner diameter) or the hole diameter (when the reduced portion is an orifice-shaped baffle plate) Dr> The cyclone classifier according to (1) or (2), wherein 1.2 × Dr is satisfied.

(4) The tip position of the inner cylinder is at a position that is not separated by 10 × ((De−Dr) / 2) or more vertically downward from the connection position between the cylindrical portion and the vertically reduced portion. The cyclone classifier according to any one of (1) to (3).
(5) the lower end position of each tube of the inner tube constituted by multi-tube are arranged independently, and, according to (4) in which the lower end position of the respective tube and which are located so as to be movable Cyclone classifier.

( 6 ) The cyclone classification according to any one of (1) to ( 5 ) above, further comprising a pocket portion for classifying large-diameter particles on an outer periphery of an outer cylinder body portion where the cylindrical portion exists. vessel.
( 7 ) The cyclone classifier according to ( 6 ), wherein a slide plate that is slidable in the vertical direction is provided at an inlet to the pocket portion.

( 8 ) The discharge port suction area is controlled by installing a plate-like or conical control plate below at least one inner cylinder lower end of the inner cylinder lower end existing in the cylinder. The cyclone classifier according to any one of (1) to ( 7 ).
( 9 ) The cyclone classifier according to ( 8 ), wherein the flat or conical control plate is movable in the vertical direction.
( 10 ) An airflow drying system comprising the cyclone classifier according to any one of (1) to ( 9 ).

  According to the present invention, it is possible to provide a cyclone classifier with good classification accuracy and high yield, and an air-flow drying function capable of performing drying and classification from a wet assembly (wet cake), and classification. It is possible to provide a cyclone classifier, an air flow drying system, and a toner that have functions simultaneously or continuously.

Hereinafter, the cyclone classifier of the present invention will be described in detail by embodiments.
In the following description, for convenience of explanation, an electrophotographic polymerization toner is mentioned. However, the present invention is not limited to the polymerization toner and the pulverization toner, and is an effective means for classifying any powder.
As shown in FIGS. 2 to 5, the cyclone classifier of the present invention has outer cylinder body portions 22 (22A, 22B), 32 (32A, 32B, 32C), 42 (42A, 42B), 52 (52A, 52B). And outer cylinder bottom part 5 and inner cylinders 24, 34 (34A, 34B), 44, 54. An inner cylinder tip (inner cylinder) which has a reduced portion 23, 33A, 33B, 43, 53 made of a cylinder having a reduced inner diameter or an orifice-shaped baffle plate at an arbitrary height in the outer cylinder body portion and which is an exhaust port. Are present in a cylindrical space (cylindrical portion) (22B, 32B, 32C, 42B, 52B) that is connected vertically below the contraction portion. Inside the cyclone, centrifugal force acts on the particles in the airflow in the radial direction of the swirling flow due to the swirling flow. Since the centrifugal force increases in proportion to the particle size, the small particle size particles gather near the swirling center, and the large particle size particles gather near the swirling outer periphery.

  In the present invention, the swirl flow swirls from the introduction parts 21, 31, 41, 51 in the upper cylinder outer part (22A, 32A, 42A, 52A) of the cyclone classifier while the arrow shown in the figure shows the lower part of the cyclone classifier outer cylinder. In this way, it falls downward and is sucked and exhausted from the tips of the inner cylinders 24, 34, 44, 54. The powder that has entered from the introduction parts 21, 31, 41, 51 in the upper part of the outer cylinder of the cyclone classifier is sufficiently subjected to centrifugal force by the outer cylinder upper parts 22A, 32A, 42A, 52A of the cyclone classifier, and the reduction part After the turning diameter is narrowed by 23, 33A, 33B, 43, 53, it enters the cylindrical portion (22B, 32B, 32C, 42B, 52B). The particles with various particle diameters that are strongly pressed against the upper wall surface of the outer cylinder by this centrifugal force are released from the wall surface that was the pressing surface immediately after entering the cylindrical portion, and the centrifugal force acting on each particle. Is dispersed in the radial direction in accordance with the centrifugal force given by the particle size of each particle in the cylindrical portion.

The centrifugal force F acting on each particle is represented by F = mV ² / R (where m represents the mass of the particle, V represents the turning speed, and R represents the turning radius). Since the diameter is proportional to the mass, a centrifugal force is applied in proportion to the particle diameter, whereby a particle size distribution is generated in the radial direction. Accordingly, each particle is ejected and diffused (dispersed) to the vicinity of the outer wall of the cylindrical portion, and the particles having a small particle diameter remain in the vicinity of the center of the cylindrical portion, while the particles having a large particle diameter are blown to the vicinity of the outer wall of the cylindrical portion, A distribution that is approximately in the order of particle sizes in the radial direction occurs.

By sucking the generated radial distribution in the order of particle size from the tip of the inner cylinder at a certain position, only particles having a desired particle size (particles having a desired distribution) are separated very efficiently. It becomes possible.
As a means of adjusting the powder particles distributed in order of particle size in the radial direction by the diffusion in the cylindrical portion to freely change the classification point to the desired particle size and particle size distribution, the inner cylinder vertical It is effective to form a device so that the directional position can be freely changed, and to appropriately incorporate the device thus formed. In this case, however, it is essential that the tip portion of the inner cylinder as the exhaust port is in the cylindrical portion.

  Moreover, it can also be set as the apparatus which gives a bigger centrifugal force by narrowing the diameter of the reduction part (part which consists of a cylinder with a reduced internal diameter, or an orifice-shaped baffle plate). By applying such a large centrifugal force, particles of all diameters gather in the reduced portion in the reduced portion, and as soon as they enter the cylindrical portion, a large swirl speed is given to the reduced portion to generate a large centrifugal force. When applied, it spreads over a wide area at once, and a distribution in the order of particle diameters can be made in the radial direction, enabling more efficient classification. However, if the reduced portion diameter becomes too small, the gap between the reduced portion diameter and the outer periphery of the inner cylinder becomes too narrow, and the swirling flow stays on the reduced portion. If the gap area is smaller than the cross-sectional area of the introduction portion, there is a possibility of stagnation, which is not preferable.

  In order to accelerate the swirl flow and enhance the centrifugal effect by inserting an orifice-shaped baffle plate, as in Patent Document 3, the tip of the inner cylinder, which is a suction port, is positioned above the orifice-shaped baffle plate However, in the embodiment according to the present invention, since the device is configured so as to obtain a diffusion effect by the cylindrical portion below the orifice-shaped baffle plate, the tip of the inner cylinder that is the suction port is It is essential to be located in the lower part of the orifice-shaped baffle, that is, in the cylindrical part.

In this cyclone classifier, it is preferable that the cylindrical part diameter De is in a range satisfying De> 1.2 × Dr with respect to the reduced part (diameter Dr) for the particle size alignment due to the centrifugal force diffusion effect. As for the cylindrical portion diameter De, if it becomes too large, the centrifugal force becomes weak, so the classification effect becomes small. As a possible value of De, it is desirable that a centrifugal force of at least 200 G or more is applied to the particles depending on the relationship with the wind speed at the inlet.
When the inner cylinder tip position existing in the cylindrical part is far from the cylindrical part inlet just below the reduction part, particles distributed in the order of the particle diameter in the radial direction by the centrifugal force applied by the cylindrical part will gather again. It will be. The inner cylinder tip position is preferably a position that is not separated by 10 × ((De−Dr) / 2) or more vertically downward from the connection position between the cylindrical portion and the vertically reduced portion.

  With respect to the inner cylinder, a single-tube configuration may be used, but it is preferable to configure the inner cylinder with a multi-tube, and with such a multi-tube, a cyclone classifier with a configuration that can classify more accurately can do. It is preferable that the tip of each inner cylinder at the time of adopting this configuration is in the cylindrical portion as described above. Also, when the inner cylinder is a multi-tube type, if the tip of each pipe of this inner cylinder is set to a different height, particles with a small particle diameter can be discharged from the exhaust port several times in small amounts, and classification accuracy is improved. be able to. By variably configuring the tip position of each layer of the multiple tube inner cylinder, the classification point can be adjusted with high accuracy.

  By providing a plurality of cylindrical portions of the present invention for one cyclone classifier, more precise classification is possible. For example, as shown in FIG. 3, it is possible to adopt a configuration in which the cylindrical portion has two stages and a configuration in which the inner cylinder is a double tube. In this case, it is preferable that the tip of the outer suction port of the double-pipe inner cylinder is configured in the first-stage cylindrical portion from the top, and the tip of the inner suction port is configured in the second-stage cylindrical portion from the top. Such a plurality of cylindrical portions can also be achieved by installing a plurality of orifice-shaped baffle plates.

  The cyclone classifier mechanism adopting this baffle structure can perform a plurality of classification steps, can exhibit a similar multi-stage (for example, two-stage) classification effect, or a multiple tube (for example, a double tube) ) Type inner cylinder inner layer, outer layer, and classified powder from the lower part of the cyclone classifier are separated and recovered to obtain a three-separation classification effect (multi-separation simultaneous recovery effect), and more precise classification Alternatively, it is possible to adjust the distribution and particle size as appropriate, such as multi-separation (simultaneous recovery of other distributions), and the like so that adjustment can be performed.

  Further, since particles having a large particle size jump out in the vicinity of the outer wall near the entrance of the cylindrical portion, if a collection pocket 45 is provided in the vicinity of the outer wall as shown in FIG. 4, it is possible to classify only large particles. By adjusting the inlet position to the large particle size particle collection pocket by the slide plate 46 that can be moved up and down, the classification point (classification position) of the large particle size particle can also be adjusted. Regarding the appropriate size of the pocket, for example, if the vertical width of the pocket is too large, particles having a desired particle size other than the large particle size are discharged into the pocket. Preferably, the lower limit position of the pocket (bottom side position of the pocket square hole) is a position not farther than 2 × ((De−Dr) / 2) from the lower end of the reduced portion. Further, the lateral width of the pocket is preferably in the range of 45 ° to 90 ° of the arc of the cylindrical portion wall.

  Further, in the embodiment of the cyclone classifier according to the present invention, as shown in FIG. 5, the control for adjusting the outlet suction area calculated by the product of the circumference of the inner cylinder tip diameter and the distance to the control plate By adopting the configuration in which the plate 55 is installed, it is possible to adjust the flow rate of the airflow into the inner cylinder and to stabilize the flow of the airflow flowing into the inner cylinder. By configuring in this way, the cyclone classifier of the present invention can further improve the classification accuracy.

  Such a control plate may be a flat plate, but preferably has a conical shape, and by adopting such a configuration, a configuration in which airflow is sucked into the inner cylinder without causing turbulence along the conical slope. This is preferable. When the control plate is installed, the airflow inflow area into the inner cylinder is constituted by a gap between the tip of the inner cylinder and the control plate surface. At this time, within the range of the height of the cylindrical portion, if the inner cylinder tip is arranged by adjusting for a predetermined classification point, the air flow rate can be appropriately changed by moving the control plate up and down, The flow of the inflow airflow is stabilized, and thus the cyclone classifier can be configured to further improve the classification accuracy.

As described above, the classifiers shown in FIGS. 2 to 5 have been described using the standard classifier as an example. However, in the present invention, a reduced cylindrical classifier can be used instead of the standard classifier.
FIG. 6 shows a configuration example of a cyclone classifier (a) of a standard type (the outer cylinder body portion has the same diameter) and a cyclone classifier (b) in which the reduced portion according to the present invention, which is a modified example thereof, is formed of a reduced cylinder. Show.
The cyclone classifiers shown in FIGS. 2 to 5 are all described with reference to an example of a standard type, but can be used in place of the reduced cylindrical cyclone classifier of the modified example shown in FIG. 6B. . In the reduced cylindrical classifier, the cyclone classifier includes an introduction part (inlet part) 1, an outer cylinder body part including a reduction part 2 A and a cylindrical part 2 B, an outer cylinder bottom part 5, and an inner cylinder 4. It has the composition which becomes.
In the standard cyclone classifier (a), as shown in FIGS. 2 to 5, a reduced portion is formed by an orifice-shaped baffle plate. Also in the cyclone classifier (b) in which the reducing portion is formed of a reducing cylinder, the cylindrical portion 2B may have a configuration having an orifice-shaped baffle plate and a plurality of cylindrical portions, and the reducing portion 2A and the cylinder The part 2B may be connected via an orifice-shaped baffle plate.

Next, an airflow drying system having a cyclone classifier shown in FIGS.
Another embodiment of the airflow drying system according to the present invention is configured to include a cyclone classifier.
For example, FIG. 7 shows a configuration example of the airflow drying system of the present invention. An air dryer 73 is installed on the upstream side of the cyclone classifier 75, and the powder is sent to the cyclone classifier. On the downstream side, a bag filter 77 for collecting classified small particle diameter particles and a desired particle diameter particle collecting container 76 for collecting desired particle diameter particles are provided. Supply of powder before drying to the air dryer is controlled by a powder feeder 74 and air in the system is controlled by an exhaust fan 78 and an air supply fan 71. The heat exchanger 72 is a device that heats air for airflow drying.
FIG. 1 shows a study system of the present invention that assumes the airflow drying system of FIG. The air flow drying system of the present invention simulated in FIG. 1 includes a supply means for supplying powder (for example, toner) to be classified from the upstream side of the cyclone classifier 14, a cyclone collector 16 on the downstream side, and an exhaust fan. 18.
As a supply means, for example, it has a powder feeding means (for example, powder feeding air 12) for introducing powder into a cyclone classifier and a powder feeder 11, and these are provided with a receiving tray 13. good.

Further, a feedback means may be provided between the cyclone collector 16 and the cyclone classifier 14, and at least a part of the classified powder can be fed back to the introduction part of the cyclone classifier.
The feedback means is preferably a means having a suction mechanism and an exhaust mechanism. For example, a configuration in which the valve body and the exhaust fan 18 are combined, or a configuration having only the exhaust fan can be employed.
Furthermore, in the airflow drying system of the present invention, the cyclone collector 16 can be omitted, and the above-described feedback means can be provided to use the cyclone classifier in multiple stages. The powdered toner fed back by such a feedback means is classified in the cyclone classifier 14 by an arbitrary number of stages, or is dried while being classified, so that the classified toner having a desired particle size distribution is obtained. It will be easily obtained.

Further, the use of the cyclone classifier of the present invention can sufficiently exert its labor saving effect by combination with equipment used in other processes. For example, in the drying process when polymerized toner is produced, when the wet colored polymer particles are dried with an airflow dryer, the colored polymer particles discharged together with the airflow after drying can be separated into a solid and gas with a cyclone classifier. is there. At that time, by using the cyclone classifier of the present invention together with the classification, the cost of the entire equipment can be reduced, and at the same time, it can exert a great effect on drastically reducing man-hours. For this, a great effect is brought about.
As described above, the present inventors have provided an invention of a cyclone classifier, an airflow drying system, and a toner that can produce a polymer toner having a narrow distribution width without newly using a classification process.
Examples and comparative examples are shown below.
In addition, what was shown as Examples 1-4 and 6-9 below is a reference example and is a thing outside this invention, and what was shown as Example 5 is an Example of this invention.

Examples according to the present invention will be described below. The production process of colored polymer particles as an example of the present invention will be described in more detail. However, the present example is not limited to the invention used only for the colored polymer particles described below and the invention of the toner production method. The present invention is also effective for particles of various other types and particle sizes.
Therefore, the present invention should not be construed as being limited to the following examples and the like, and it goes without saying that the present invention is construed according to the contents disclosed in the specification and the drawings. Note that “parts” used below indicates “parts by weight”.

(Raw material adjustment)
In a reaction vessel in which a stir bar and a thermometer are set, 683 parts of water, 11 parts of a sodium salt of ethylene oxide methacrylate adduct sulfate (Eleminol RS-30: manufactured by Sanyo Chemical Industries, Ltd.), 138 parts of styrene, When 138 parts of methacrylic acid and 1 part of ammonium persulfate were charged and stirred for 15 minutes at 400 rpm, a white emulsion was obtained.
The system temperature was raised to 75 ° C. by heating to react for 5 hours. Further, 30 parts of a 1% ammonium persulfate aqueous solution was added, and the mixture was aged at 75 ° C. for 5 hours, and an aqueous dispersion of vinyl resin (styrene salt copolymer of styrene-methacrylic acid-methacrylic acid ethylene oxide adduct sulfate) [ Fine particle dispersion].
Further, 83 parts of [fine particle dispersion] were mixed with 990 parts of water, 37 parts of a 48.5% aqueous solution of sodium dodecyl diphenyl ether disulfonate (Eleminol MON-7) manufactured by Sanyo Chemical Industries, Ltd., and 90 parts of ethyl acetate. Agitation gave a milky white liquid. This is referred to as [aqueous phase].

  In a reaction vessel equipped with a condenser, a stirrer and a nitrogen inlet tube, 229 parts of bisphenol A ethylene oxide 2 mol adduct, 529 parts of bisphenol A propylene oxide 3 mol adduct, 208 parts terephthalic acid, 46 adipic acid 46 And 2 parts of dibutyltin oxide were added, reacted at 230 ° C. under normal pressure for 8 hours, and further reacted under reduced pressure of 10 to 15 mmHg (10 to 15 Torr) for 5 hours. Then, 44 parts of trimellitic anhydride was added to the reaction vessel. The mixture was reacted at 180 ° C. for 2 hours at normal pressure to obtain [Low molecular weight polyester].

In a reaction vessel equipped with a cooling pipe, a stirrer and a nitrogen introduction pipe, 682 parts of bisphenol A ethylene oxide 2-mole adduct, 81 parts of bisphenol A propylene oxide 2-mole adduct, 283 parts of terephthalic acid, trimellitic anhydride 22 And 2 parts of dibutyltin oxide were added, reacted at 230 ° C. for 8 hours under normal pressure, and further reacted for 5 hours at a reduced pressure of 10 to 15 mmHg to obtain an [intermediate polyester].
Next, 410 parts of [intermediate polyester], 89 parts of isophorone diisocyanate, and 500 parts of ethyl acetate were placed in a reaction vessel equipped with a cooling pipe, a stirrer, and a nitrogen introduction pipe, and reacted at 100 ° C. for 5 hours. Phase].

  170 parts of isophoronediamine and 75 parts of methyl ethyl ketone were charged into a reaction vessel equipped with a stirrer and a thermometer, and reacted at 50 ° C. for 5 hours to obtain a [ketimine compound].

  1200 parts of water, 540 parts of carbon black (manufactured by Printex 35 Dexa) [DBP oil absorption (JIS K6221 DBP: dibutyl phthalate) = 42 ml / 100 mg, pH = 9.5] and 1200 parts of polyester resin were added, and a Henschel mixer (Mitsui) (Mine Co., Ltd.) and the mixture was kneaded at 150 ° C. for 30 minutes using two rolls, rolled and cooled, and pulverized with a pulverizer to obtain [Masterbatch].

In a container in which a stir bar and a thermometer are set, 378 parts of the above-mentioned [low molecular polyester], 110 parts of carnauba wax, 22 parts of CCA (salicylic acid metal complex E-84: Orient Chemical Industry), and 947 parts of ethyl acetate Were heated to 80 ° C. with stirring, held at 80 ° C. for 5 hours, and then cooled to 30 ° C. over 1 hour. Next, 500 parts of [Masterbatch] and 500 parts of ethyl acetate were charged in a container and mixed for 1 hour to obtain [Raw material solution].
1324 parts of this [raw material solution] was transferred to a container, and using a bead mill (Ultra Visco Mill, manufactured by Imex Co., Ltd.), a liquid feeding speed of 1 kg / hr, a disk peripheral speed of 6 m / sec, and 0.5 mm zirconia beads were 80% by volume. Filling was performed, and carbon black and wax were dispersed under conditions of 3 passes.
Next, 1324 parts of a 65% ethyl acetate solution of the above [low molecular polyester] was added, followed by one pass with a bead mill under the above conditions to obtain [Pigment / WAX Dispersion].
664 parts of [Pigment / WAX Dispersion] and 5.9 parts of [Ketimine Compound] were put in a container and mixed well with a disper to obtain [B Oil Phase].

(Emulsification process)
The [A oil phase] and the [B oil phase] were fed with a feed pump and mixed through a static mixer (manufactured by Noritake Company). The amount of liquid fed was adjusted so that [B oil phase] was 60.4 parts with respect to [A oil phase] 74 parts. Here, the [oil phase], which is sufficiently mixed and uniform, is joined with 101.6 parts of the above [water phase] sent out separately by a liquid feed pump, and a continuous emulsifier pipeline homomixer (Special Machine Industries) (Made by Co., Ltd.) and emulsified by applying a large shear force at 8400 rpm. At this time, it became [Slurry liquid A] in which minute [oil phase] liquid droplets serving as colored polymer particles were present in the [aqueous phase] medium.

(Solvent removal process, aging process)
[Slurry liquid A] containing an organic solvent is put into a container in which a stirrer and a thermometer are set, and after removing the solvent at 40 ° C. for 8 hours, aging is performed at 60 ° C. for 8 hours, and then [slurry liquid B] Got.

(Washing process, solid-liquid separation process)
100 parts of [Slurry liquid B] were solid-liquid separated with a filter press and dehydrated with a pressing pressure of 0.4 MPa to obtain [Hydrate cake A].
To 100 parts of this [hydrated cake A], 200 parts of ion-exchanged water was added and dispersed uniformly with a TK homomixer (rotation speed: 6,000 rpm for 30 minutes) to obtain [Dispersed slurry liquid A].
100 parts of the [dispersed slurry liquid A] was subjected to solid-liquid separation with a siphon pillar type centrifugation with a centrifugal effect of 1000 G to obtain [hydrous cake B].

(Drying process)
The [hydrated cake B] was dried with a flash dryer. [Water-containing cake B] had a water content of 25% by weight.
The drying conditions in the air dryer were set to an air volume of 10 m ³ / min, an inlet temperature of 65 ° C., and an outlet temperature of 33 ° C. As a result of airflow drying under these conditions, the drying treatment speed was 0.5 kg / min. Moreover, the water content after airflow drying was 0.9% by weight.

  The colored polymer particles that had undergone the drying step were classified using an experimental cyclone classifier. FIG. 1 shows a schematic diagram of an attached facility of the cyclone classifier used and a simulated airflow drying system including the same. Since air is sucked by the exhaust fan 18, a swirling flow is generated in the cyclone collector 16 and the cyclone classifier 14. First, the colored polymer particles are quantitatively and continuously discharged into the receiving tray 13 by the powder feeder 11. The colored polymer particles discharged into the tray 13 ride on the air flow from the suction and powder feed air 12 of the exhaust fan 18 and are sent into the cyclone classifier 14. The colored polymer particles classified into the desired particle size and the particle size distribution width by the swirling flow in the cyclone classifier 14 are dropped and collected in the desired particle size particle collecting container 15. Colored polymer particles having a particle size smaller than the desired particle size are discharged from the inner cylinder of the cyclone classifier 14 and enter the cyclone collector 16. All colored polymer particles having a particle diameter smaller than the desired particle diameter are collected by the swirling flow of the cyclone collector 16 and fall into the small particle collection container 17.

A schematic diagram of the cyclone classifier used in Example 1 is shown in FIG.
The circles of various sizes in the cylinder in FIG. 2 are schematically represented in consideration of the size of the colored polymer particles. The colored polymer particle group having a wide particle size distribution width flowing from the cyclone introduction part 21 is subjected to centrifugal force in the upper part 22A of the cyclone outer cylinder due to the swirling flow in the cyclone and gradually descends along the cyclone outer cylinder. . In the vicinity of the upper surface of the orifice-shaped baffle plate 23, the flow area is narrowed by the holes of the orifice-shaped baffle plate 23, so that the swirl flow rate increases rapidly, and the centrifugal force applied to the colored polymer particles also increases.
The airflow that has passed through the holes in the orifice-shaped baffle plate 23 is released from the holes in the orifice-shaped baffle plate 23 that was the pressing surface, and the radial force is accumulated in the cylinder of the cyclone cylindrical portion 22B by the centrifugal force accumulated in each particle. Spread. The colored polymer particles having a large particle size are released from the accumulated large centrifugal force, expelled to the vicinity of the outer wall of the cylindrical portion, diffused, and dropped along the wall surface in the cyclone cylindrical portion 22B to collect the desired particle size particles. To be collected. The colored polymer particles having a small particle diameter remain in the vicinity of the center of the cylindrical portion because the accumulated centrifugal force is small, and are discharged from the cyclone classifier together with the exhaust flow from the cyclone inner cylinder 24.

In the present example and comparative example, the same colored polymer particles were used.
The colored polymer particles used had a volume average particle diameter Dv of 5.8 μm, Dv / Dn obtained by dividing the volume average particle diameter by the number average particle diameter Dn represents the particle size distribution width of the powder, and the color weight used The combined particles had a Dv / Dn of 1.18. The content of particles having a particle size of 4.0 μm or less was 14.6% by number, and the content of particles having a particle size of 12.7 μm or more was 1.3% by volume. Yield used in this example and comparative example is (weight of powder collected in desired particle size collection container [kg]) / (weight of powder charged into system from powder feeder [kg]) Calculated.
The experimental conditions in Example 1 were a cyclone outer cylinder body diameter of 155 mm, a cyclone outer cylinder body length of 450 mm, a cyclone outer cylinder bottom part length (vertical direction length) of 300 mm, and an exhaust fan air volume of 270 m ³ / h. The feed amount of the colored polymer particles was 8.7 kg / h, and the ratio De / Dr of the diameter De of the cyclone cylindrical portion 22B and the baffle hole diameter Dr of the orifice shape was 1.6. The tip position of the cyclone inner cylinder was 1 × ((De−Dr) / 2)) (position 30 mm from the bottom surface of the orifice-shaped baffle plate) from the bottom surface of the orifice-shaped baffle plate.

Using the same equipment as in Example 1, the exhaust fan air flow rate 270 m ³ / h, the colored polymer particle feed rate 8.7 kg / h, the ratio De of the cyclone cylindrical portion 22B diameter De and the orifice-shaped baffle plate hole diameter Dr / Dr is 1.6, and the tip position of the cyclone inner cylinder is 9 × ((De-Dr) / 2) from the bottom surface of the orifice-shaped baffle plate (position 270 mm from the bottom surface of the orifice-shaped baffle plate). It was carried out under the set conditions.

Using the same equipment as in Example 1, the ratio De of the exhaust fan air flow rate 270 m ³ / h, the colored polymer particle feed rate 8.7 kg / h, the diameter De of the cyclone cylindrical portion 22B, and the baffle plate hole diameter Dr of the orifice shape / Dr is 1.3, and the tip position of the cyclone inner cylinder is 5 × ((De−Dr) / 2) from the bottom surface of the orifice-shaped baffle plate (position 90 mm from the bottom surface of the orifice-shaped baffle plate). It was carried out under the set conditions.

Using the same equipment as in Example 1, the ratio De of the exhaust fan air flow rate 270 m ³ / h, the colored polymer particle feed rate 8.7 kg / h, the diameter De of the cyclone cylindrical portion 22B, and the baffle plate hole diameter Dr of the orifice shape / Dr is 1.3, and the position of the tip of the cyclone inner cylinder is 9 × ((De−Dr) / 2) from the bottom surface of the orifice-shaped baffle plate (position 150 mm from the bottom surface of the orifice-shaped baffle plate) It carried out on the conditions set to.

The cyclone classifier shown in FIG. 3 is a cyclone classifier (a cyclone classifier having a mechanism having a double cylindrical portion composed of two orifice-shaped baffle plates 33A and 33B and a double pipe inner cylinder: outside of the double pipe inner cylinder. Except that the colored polymer particles having a small particle size conveyed from the suction layer 34A and the inner suction layer 34B are mixed together and conveyed to the cyclone collector 16 and changed to the cyclone classifier 14) of the two-stage classification mode, the example 1, the exhaust fan air flow rate 270 m ³ / h, the colored polymer particle feed rate 8.7 kg / h, the diameter De of the cyclone cylindrical portion 32B, and the hole diameter of the orifice-shaped baffle plate (in this embodiment) The ratio De / Dr with respect to Dr is 1.6, and the position of the cyclone inner cylinder tip 34 is such that the outer suction tube 34A and the inner suction tube 34B are respectively in the orifice-shaped baffle plate 3 Was carried out under the conditions set on the lower surface than 1 × A and 33B ((De-Dr) / 2) of the position (baffle lower surface than 30mm position of the orifice shape).

The cyclone classifier shown in FIG. 4 is a cyclone classifier having a large particle size particle collection pocket 45 (vertical 50 mm, horizontal [arc angle 45 °]). Except for changing to the collection pocket inlet adjustment slide plate 46), the same incidental equipment as in Example 1 was used, the exhaust fan air flow rate was 270 m ³ / h, and the colored polymer particle feed rate was 8.7 kg. / H, the ratio De / Dr of the diameter De of the cyclone cylindrical portion 42B and the orifice-shaped baffle plate hole diameter Dr is 1.6, and the tip position of the cyclone inner cylinder 44 is the lower surface of the orifice-shaped baffle plate 43 Thus, the measurement was performed under the conditions set at a position of 1 × ((De−Dr) / 2) (position 30 mm from the bottom surface of the baffle plate having an orifice shape).

The cyclone classifier shown in FIG. 4 is a cyclone classifier having a large particle size particle collection pocket 45, and the height width of the inlet to the large particle size particle collection pocket 45 can be increased or decreased. Except for being reduced to 1/2 by the slide plate 46), using the same incidental equipment as in Example 1, the exhaust fan air flow rate was 270 m ³ / h, the colored polymer particle feed rate was 8.7 kg / h, the cyclone The ratio of the diameter [De] of the cylindrical portion 42B to the orifice-shaped baffle plate hole diameter [Dr] is De / Dr = 1.6, and the tip position of the cyclone inner cylinder is 1 × ((De− Dr) / 2) was carried out under the conditions set at the position (position 30 mm from the lower surface of the baffle plate of the orifice shape).

The cyclone classifier shown in FIG. 5 is a cyclone classifier having a mechanism having a control plate (conical type) 55 at the tip of the inner cylinder. The positions of the conical control plates are the tip of the inner cylinder 54 and the control plate 55. The area of the airflow inflow constituted by the gap with the surface was set to be 2/3 of the inner cylinder tip area.) Except for the change, the same incidental equipment as in Example 1 was used, and the exhaust fan air volume was 270 m ^3. / H, the feed amount of the colored polymer particles 8.7 kg / h, the ratio of the diameter [De] of the cyclone cylindrical portion 52B to the baffle hole diameter [Dr] of the orifice shape is De / Dr = 1.6, and the cyclone inner cylinder The tip position was carried out under the condition set at a position of 9 × ((De−Dr) / 2) from the bottom surface of the orifice-shaped baffle plate (position 270 mm from the bottom surface of the orifice-shaped baffle plate).

Using the same equipment as in Example 1, the exhaust fan air flow rate was 270 m ³ / h, the colored polymer particle feed rate was 8.7 kg / h, the diameter [De] of the cyclone cylindrical portion 22B and the baffle plate hole diameter [Dr] of the orifice shape. The ratio is De / Dr = 1.1, and the tip position of the cyclone inner cylinder is 12 × ((De−Dr) / 2) from the bottom surface of the orifice-shaped baffle plate (90 mm from the bottom surface of the orifice-shaped baffle plate) ).

[Comparative Example 1]
Using the same equipment as in Example 1, the exhaust fan air flow rate was 270 m ³ / h, the colored polymer particle feed rate was 8.7 kg / h, the diameter [De] of the cyclone cylindrical portion 22B and the baffle plate hole diameter [Dr] of the orifice shape. The ratio is De / Dr = 1.1, and the tip position of the cyclone inner cylinder is 1 × ((De−Dr) / 2) above the upper surface of the orifice-shaped baffle plate (10 mm from the upper and lower surfaces of the orifice-shaped baffle plate) Was carried out under the conditions set in

[Comparative Example 2]
A cyclone classifier comprising a standard-type outer cylinder body, an outer cylinder bottom, and an inner cylinder without a reduction part and a cylinder part was used.
The experimental conditions in Comparative Example 2 were as follows: the exhaust fan air flow rate was 270 m ³ / h, the colored polymer particle feed rate was 8.7 kg / h, and the tip position of the cyclone inner cylinder was set to the inner cylinder length of 515 mm. Carried out.

[Comparative Example 3]
A cyclone classifier comprising a standard-type outer cylinder body, an outer cylinder bottom, and an inner cylinder without a reduction part and a cylinder part was used.
The experimental conditions in this Comparative Example 3 were as follows: the exhaust fan air flow rate was 270 m ³ / h, the colored polymer particle feed amount was 8.7 kg / h, and the tip position of the cyclone inner cylinder was set to be 305 mm of the inner cylinder length. Carried out.

[Comparative Example 4]
Using a cyclone classifier consisting of a standard outer cylinder body, outer cylinder bottom, and inner cylinder, which does not have a reduction part and a cylinder part, an exhaust fan air flow rate of 270 m ³ / h, a colored polymer particle feed rate of 8.7 kg / h, The cyclone inner cylinder tip position was carried out under the conditions set so that the inner cylinder length was 85 mm.

[Evaluation methods]
<Particle size>
The particle diameters of the colored polymer particles in the above Examples and Comparative Examples were measured using a Coulter Counter Multisizer (manufactured by Coulter). Specifically, it measured by the following method. First, 0.1 to 5 ml of a surfactant (preferably alkylbenzene sulfonate) is added as a dispersant to 100 to 150 ml of an aqueous electrolytic solution. Here, an about 1% NaCl aqueous solution is prepared using first grade sodium chloride as an electrolytic solution. For example, ISOTON-II (manufactured by Coulter) can be used. Further, 2 to 20 mg of a measurement sample is added. The electrolytic solution in which the sample is suspended is subjected to a dispersion treatment with an ultrasonic disperser for about 1 to 3 minutes, and the measurement device is used to measure the volume and number of toner particles or toner using a 100 μm aperture as an aperture. Volume distribution and number distribution are calculated. From the obtained distribution, the toner has a volume average particle diameter (Dv), a number average particle diameter (Dn), a content having a particle diameter of 4.0 μm or less (number%), and a content (volume%) having a particle diameter of 12.7 μm or more. )
As channels, 2.00 to less than 2.52 μm; 2.52 to less than 3.17 μm; 3.17 to less than 4.00 μm; 4.00 to less than 5.04 μm; 5.04 to less than 6.35 μm; 6 Less than 35 to 8.00 μm; less than 8.00 to less than 10.08 μm; less than 10.08 to less than 12.70 μm; less than 12.70 to less than 16.00 μm; less than 16.00 to less than 20.20 μm; Using particles of less than 40 μm; 25.40 to less than 32.00 μm; 32.00 to less than 40.30 μm, particles having a particle diameter of 2.00 μm to less than 40.30 μm were targeted.
Table 1 shows the results of evaluating examples and comparative examples using the above evaluation methods.

  As shown in Table 1, when Examples 1 to 5 using the present invention are compared with a comparative example, the content is 4.0 μm or less in particle size, and particles having a desired particle size or less are well classified. It has been shown that Further, in the embodiment, these classifications are performed with good yield. In Examples 6 and 7, it was confirmed that the large particle size particles were classified, and that the amount of large particle size classification could be controlled by adjusting the large particle size pocket inlet width. In Example 8 where the air flow inflow area at the tip of the inner cylinder was adjusted with the control plate, the inflow speed was increased and stabilized. As a result, the exhaust gas flow from the inner cylinder could reliably capture small particle size particles, and high yield. It was confirmed that high-precision classification was performed.

  The present invention is not limited to the production of colored polymer particles that are the raw materials of electrophotographic toners that are usually handled, and can be used from the drying process to the classification process of powders of all kinds and particle sizes, so that a very wide range is possible. It can be used for the production of powders and the like, and can be used over a wide range when using the cyclone classifier of the present invention.

It is the schematic which shows the arrangement structure of the whole invention examination system which imitated the airflow drying system using the cyclone classifier of this invention. It is a schematic block diagram of the cyclone classifier of this invention. It is a schematic block diagram of the cyclone classifier (two-stage classification style) of this invention. It is a schematic block diagram of the cyclone classifier (with a large particle size particle collection pocket) of this invention. It is a schematic block diagram of the cyclone classifier (with a conical control board) of this invention. It is a figure which shows the example of the cyclone classifier of this invention, (a) is a structural example of a standard cyclone classifier, (b) is a structural example of a reduction | decrease cylindrical cyclone classifier. It is the schematic which shows the arrangement structure of the whole airflow drying system using the cyclone classifier of this invention.

Explanation of symbols

1 Introduction (entrance)
2 Outer cylinder body 2A Reduced part (reduced cylindrical shape)
2B Cylindrical part 4 Inner cylinder 5 Outer cylinder bottom part 11 Powder feeder 12 Feeding air 13 Receptacle 14 Cyclone classifier 15 Desired particle size collection container 16 Cyclone collector 17 Small particle diameter particle collection container 18 Exhaust fan 21 Cyclone introduction Part 22 Cyclone outer cylinder body 22A Outer cylinder upper part 22B Cylindrical part 23 Orifice-shaped baffle plate 24 Cyclone inner cylinder 31 Cyclone introduction part 32 Cyclone outer cylinder body part 32A Outer cylinder upper part 32B, 32C Cylindrical part 33A, 33B Orifice-shaped baffle Plate 34A, 34B Cyclone inner cylinder (outer suction layer, inner suction layer)
DESCRIPTION OF SYMBOLS 41 Cyclone introduction part 42 Cyclone outer cylinder trunk | drum 42A Outer cylinder upper part 42B Cylindrical part 43 Orifice-shaped baffle plate 44 Cyclone inner cylinder 45 Large particle size particle collection pocket 46 Large particle size particle collection pocket inlet adjustment slide plate 51 Cyclone Introduction part 52 Cyclone outer cylinder body 52A Outer cylinder upper part 52B Cylindrical part 53 Orifice-shaped baffle plate 54 Cyclone inner cylinder 55 Control plate (conical type)
71 Air Supply Fan 72 Heat Exchanger 73 Air Dryer 74 Powder Feeder 75 Cyclone Classifier 76 Desired Particle Size Collection Container 77 Bag Filter 78 Exhaust Fan

Claims (10)

Formed with an outer cylinder consisting of a cylindrical outer cylinder body, an outer cylinder bottom part that is an inverted conical shape connected vertically below the outer cylinder body part, and an inner cylinder that is a multi-layered exhaust port The cyclone classifier has a reduced portion made of a cylindrical or orifice-shaped baffle plate whose inner diameter is reduced to an arbitrary height in the outer cylinder body, and a lower end portion of the inner cylinder is formed of the reduced portion. Present in a cylindrical space (cylindrical part) that is connected vertically below , a plurality of the cylindrical part and the reduction part exist in the outer cylinder body part, and a plurality of cylindrical parts provided in the outer cylinder body part and The cyclone classifier according to claim 1, wherein a lower end portion of each tube of an inner cylinder configured by multiple tubes is present in each of the plurality of cylindrical portions in the reduction portion .   The cyclone classifier according to claim 1, wherein a position of a lower end portion of the inner cylinder is adjustable.   The diameter De of the cylindrical portion is such that De> 1.2 with respect to the diameter of the reduced portion (when the reduced portion is a cylinder with a reduced inner diameter) or the hole diameter (when the reduced portion is an orifice-shaped baffle plate) Dr. The cyclone classifier according to claim 1 or 2, wherein xDr is satisfied.   The tip position of the inner cylinder is at a position that is not separated by 10 × ((De−Dr) / 2) or more vertically downward from the connection position between the cylindrical portion and the vertically reduced portion. Item 4. A cyclone classifier according to any one of Items 1 to 3. 5. The cyclone classifier according to claim 4 , wherein a lower end position of each tube of the inner cylinder constituted by the multiple tubes is independently arranged, and a lower end position of each tube is provided movably. . The cyclone classifier according to any one of claims 1 to 5 , further comprising a pocket portion for classifying large-diameter particles on an outer periphery of an outer cylinder body portion where the cylindrical portion exists. The cyclone classifier according to claim 6 , wherein a slide plate that is slidable in a vertical direction is provided at an inlet to the pocket portion. The discharge port suction area is controlled by installing a plate-like or conical control plate below at least one inner cylinder lower end of the inner cylinder lower end existing in the cylinder. Item 8. A cyclone classifier according to any one of Items 1 to 7 . The cyclone classifier according to claim 8 , wherein the flat or conical control plate is movable in the vertical direction. An airflow drying system comprising the cyclone classifier according to any one of claims 1 to 9 .

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