JP6519840B2 - Particle production apparatus and particle production method - Google Patents

Description

  The present invention relates to a particle manufacturing apparatus such as a toner manufacturing apparatus provided with a droplet discharge apparatus which discharges liquid from discharge holes to form droplets, and a particle manufacturing method.

  As a method of manufacturing toner for electrostatic charge image development used in image forming apparatuses such as copiers, printers, facsimiles and composite machines thereof based on the electrophotographic recording method, the pulverization method has conventionally been mainstream. In recent years, the polymerization method has been increasingly adopted. The polymerization method is a method of forming toner particles in an aqueous medium, and is referred to as such because it involves the polymerization reaction of toner raw materials at the time of or during the formation of toner particles. As the polymerization method, various polymerization methods are put to practical use, and those utilizing suspension polymerization, emulsion aggregation, polymer suspension (polymer aggregation), ester elongation reaction and the like are known. The toner produced by the polymerization method is called a polymerization toner or a chemical toner.

  Generally, the toner obtained by the polymerization method is characterized in that the particle diameter is easy to obtain, the particle diameter distribution is narrow, and the shape is nearly spherical compared to the toner obtained by the pulverization method. These features bring about the effect that it is easy to obtain high image quality as an image formed by the electrophotographic method. However, it takes a long time for the polymerization process, and after the completion of solidification, it is necessary to separate the solvent and the toner particles, and then to repeat washing and drying, requiring a large amount of water and a large amount of energy. There is a problem such as

  In addition, a liquid (toner component liquid) in which raw material components of toner are dissolved or dispersed in an organic solvent is discharged into fine droplets using a sprayer (atomizer) or the like, and dried to obtain fine particle toner. There is known a toner production method called an injection granulation method to obtain (Patent Documents 1 to 4). According to this toner manufacturing method, since it is not necessary to use water, the time and energy required for washing and drying can be greatly reduced, and the problems of the polymerization method can be avoided.

  When fine particles such as toner are produced by the injection granulation method, the fine particle-containing liquid such as toner component liquid (the raw material component of fine particles is a solvent from the plurality of discharge holes opened in the discharge hole surface of the droplet discharge device The discharge operation of discharging the liquid droplets of the liquid dissolved or dispersed in The particles are manufactured by solidifying the droplets discharged by the solidifying means.

  For example, in the particle manufacturing apparatus of Patent Documents 5 and 6, vibration generating means for applying vibration to the liquid chamber is provided, vibration is applied to the liquid in the liquid chamber, and a standing wave is generated by liquid column resonance in the liquid chamber. Form. The liquid is discharged from the discharge hole formed in the area which becomes the antinode of the standing wave into the air flow path in which the high temperature carrier air flow is flowing, and the droplet formed into droplets is dried in the carrier air and solidified Do. The particles are produced by collecting the solidified particles by the collection means.

  However, in the particle manufacturing apparatus of Patent Documents 5 and 6, the discharge holes are exposed to the high temperature carrier air flow. For this reason, there is a possibility that the fine particle-containing liquid is dried in the discharge hole and the discharge hole is clogged to cause discharge failure, which makes it difficult to secure a target production amount. As the number of clogged discharge holes increases with time and the discharge amount of droplets decreases, the amount of latent heat of vaporization at the time of particle formation also decreases, and the decrease in temperature of the carrier air flow decreases. As the dried particles are carried along the carrier stream, the temperature of the particles is approximately the same as the temperature of the carrier stream, and the temperature of the dried particles is higher than the target. As a result, the particles become soft, particles adhere to each other, and particles having a narrow particle size distribution can not be obtained.

  The present invention has been made in view of the above problems, and an object thereof is a particle manufacturing apparatus capable of manufacturing particles having a narrow particle size distribution while suppressing the temperature rise of the discharge hole surface in contact with the carrier air flow, It is an object of the present invention to provide a particle production method.

In order to achieve the above object, the invention according to claim 1 has an air flow path forming means and a plurality of discharge holes on a plane, and a resin composition liquid containing a resin and a solvent from the discharge holes into the air flow path. Droplet forming means for forming droplets by discharging, air flow supplying means for supplying high temperature carrier air flow into the air flow path so as to flow in a direction parallel to the surface direction of the discharge hole surface, and high temperature carrier air flow In the particle manufacturing apparatus, further comprising: a collection means for collecting particles solidified by drying in the air, the air flow supply means supplying a first carrier air flow so as to flow while contacting the discharge hole surface; The second carrier air stream having a temperature higher than that of the first carrier air stream supplied so as to flow on the opposite side to the discharge hole surface across the first carrier air stream, the first carrier air stream, and the second carrier air stream A member forming the air flow path on the opposite side to the discharge hole surface And a third conveying gas stream from the second transport stream supplied to flow while being in contact with a low temperature on the inner wall surface is supplied to the air flow path, the temperature of the third conveying airflow adjustable in response to variations in ambient temperature der is, on the upstream side of the discharge port to the flow direction of the transport stream of the high temperature, the pore size to arrange a plurality of transport stream so as to be parallel airflow discharge holes face 0.1 [mm] ~10 [ the Rukoto provided rectifying means honeycomb shape mm] are those characterized.

  ADVANTAGE OF THE INVENTION According to this invention, the specific effect that the particle | grains which have narrow particle size distribution can be manufactured is acquired, suppressing the temperature rise of the discharge hole surface which conveyance air flow contacts.

It is the schematic diagram which expanded and showed a part of droplet formation means of the droplet discharge apparatus of a liquid column resonance type used in this embodiment. It is sectional drawing which showed typically a part of liquid column resonance droplet formation unit which is the same droplet discharge apparatus. It is a schematic diagram which shows an example of the cross-sectional shape of a discharge hole. (A)-(d) is a schematic diagram which shows the shape (resonance mode) of the standing wave of the speed | velocity and the pressure fluctuation in the case of N = 1, 2, 3. FIG. (A)-(e) is a schematic diagram explaining the mode of the liquid column resonance phenomenon which arises in the liquid column resonance liquid chamber in the droplet discharge head in a droplet formation means. It is the schematic explaining the structure of the particle manufacturing apparatus of this embodiment. It is the schematic explaining another structure of the particle manufacturing apparatus of this embodiment. It is a figure which shows the mode which the basic particle | grains couple | bonded. It is the schematic which shows the appearance of the particle | grains which adhered. It is the schematic which shows the appearance of the particle | grains which adhered. FIG. 6 is a view showing a particle size distribution of toner collected when coalescence of droplets occurs. FIG. 6 is a view showing a particle size distribution of the toner collected when no coalescence of droplets occurs. It is a figure explaining the droplet formation phenomenon of a Rayleigh breakup type liquid column. FIG. 6 is a schematic view showing an enlarged part of a droplet discharge portion of a Rayleigh breakup type droplet discharge device.

Hereinafter, an embodiment in which a particle manufacturing apparatus according to the present invention is applied to the manufacture of toner will be described with reference to the drawings.
In the toner manufacturing apparatus of this embodiment, the toner component liquid (liquid containing fine particle component), which becomes toner particles (fine particles) when liquid droplets are solidified, is replenished to the liquid droplet discharge device while the toner component is discharged from the discharge hole of the liquid droplet discharge device. The discharge operation for discharging liquid droplets is continued. Thereafter, the discharged droplets are solidified to obtain toner particles.

  Although it is preferable that the droplet discharge device of the present embodiment has a narrow particle diameter distribution of the droplets to be discharged, there is no particular limitation, and a known device can be used. The droplet discharge apparatus includes: 1 fluid nozzle, 2 fluid nozzle, droplet discharge means of film vibration type, droplet discharge means of Rayleigh split type, droplet discharge means of liquid vibration type, droplet discharge of liquid column resonance type Means etc. The film vibration type droplet discharge means is disclosed, for example, in Japanese Patent Application Laid-Open No. 2008-292976. Further, as a Rayleigh split type droplet discharge means, there is one disclosed in Japanese Patent No. 4647506. Further, as a liquid vibration type droplet discharge means, there is one disclosed in Japanese Patent Application Laid-Open No. 2010-102195.

  In order to secure the productivity of the toner, the particle size distribution of the droplets is narrow, vibration is applied to the liquid in the liquid column resonance liquid chamber in which a plurality of discharge holes are formed, and a standing wave is formed by the liquid column resonance. Do. A liquid column resonance type droplet discharge device which discharges a liquid from the discharge hole formed in the region which becomes the antinode of the standing wave is preferable. In this embodiment, an example of manufacturing toner using a liquid column resonance type droplet discharge device will be described.

  The particle production apparatus of the present invention comprises at least an air flow path forming unit, a droplet forming unit, an air flow supplying unit, and a collecting unit, and further has other units as required. The particle production method of the present invention at least includes an air flow path forming step, a droplet forming step, an air flow supplying step, and a collecting step, and further includes other steps as necessary.

  The particle production method can be suitably carried out by the particle production apparatus, the air flow passage forming step can be suitably carried out by the gas flow passage forming means, the droplet formation step can be suitably carried out by the droplet formation means, and the air flow supply step is The present invention can be suitably carried out by means of air flow supplying means, the collecting step can be suitably carried out by the collecting means, and the other steps can be suitably carried out by other means.

  In the production of particles in which a resin composition liquid containing a resin and a solvent is discharged to form droplets, and the droplets are dried in a carrier air stream to form particles, the solvent in the resin composition liquid is The particles obtained by volatilization are collected.

  When the discharged droplets are discharged into the carrier air stream, the temperature of the droplets once reaches the wet bulb temperature due to the relationship between the vapor pressure around the droplets and the temperature, but the amount of solvent in the droplets is small. Then, the temperature of the droplets rises to the temperature of the carrier air stream. Thus, the temperature of the particles obtained by drying the droplets is about the same as the temperature of the air stream.

  When the solvent evaporates from the droplets in the carrier gas stream, the temperature of the carrier gas stream drops because the latent heat of vaporization is deprived from the carrier gas stream. That is, it is necessary to set the temperature of the air flow to a high temperature in advance in anticipation of the temperature taken away by the latent heat of vaporization. Then, when the discharge amount of the resin composition liquid fluctuates, the amount of latent heat of vaporization when the particles are formed changes, so the temperature of the carrier air flow fluctuates depending on the discharge amount of the resin composition liquid. Therefore, if the discharge holes are clogged and the discharge amount of the resin composition liquid is reduced, the decrease in temperature of the carrier air flow is reduced. Then, since the temperature of the particles dried in the particle forming step becomes substantially the same as the temperature of the carrier air stream, the temperature of the dried particles becomes high when the discharge amount of the resin composition liquid decreases.

  Then, when the dried particles are collected, the particles adhere to each other, and particles having a narrow particle size distribution can not be obtained. Some particles produced have a low softening temperature, but the tendency is remarkable for particles having a low softening temperature. For example, toners tend to be designed at lower softening temperatures to reduce power consumption during operation of the electrophotographic system. If the particles are collected in a state where the temperature of the particles is higher than the softening temperature of the particles, the particles will be solidified in a state in which the particles adhere to each other, even if particles with a particle size distribution close to monodispersion were generated just before the collection. The particle size distribution in the collecting section is significantly broadened. The cause of the deterioration of the particle size distribution is caused by the instability of the droplet forming means, and by improving it, not only the productivity is improved but also the particles are always in a stable dry state, The quality can be stabilized.

  Therefore, the present inventors diligently studied. As a result, in the particle manufacturing apparatus, a droplet forming unit that has a plurality of discharge holes on at least a flat surface and discharges a resin composition liquid containing a resin and a solvent from the discharge holes to form droplets; It has an air flow path forming means for forming a path, an air flow supply means for supplying a carrier air flow to the air flow path, and a collection means. As a result, the temperature rise of the droplet forming means can be suppressed, the clogging due to the drying of the nozzle can be suppressed, and not only the droplet discharge amount can be greatly improved, but also particle collection can be performed stably. It has been found that coalescence can be prevented and particles with a narrow particle size distribution can be produced over a long period of time.

  As a droplet forming means, it is a means having a plurality of discharge holes on a flat surface and discharging a resin composition liquid containing a resin and a solvent from the discharge holes to form droplets of uniform particle diameter. There is no particular limitation, and it can be selected appropriately according to the purpose, and may be membrane vibration type, Rayleigh split type, liquid vibration type, liquid column resonance type and the like. As a film | membrane vibration type, the thing etc. which were described in Unexamined-Japanese-Patent No. 2008-292976 are mentioned, for example. As the Rayleigh split type, for example, those described in Japanese Patent No. 4647506 and the like can be mentioned. As a liquid vibration type, the thing etc. which were described in Unexamined-Japanese-Patent No. 2010-102195 are mentioned, for example. Among them, the droplet forming means is preferably a liquid column resonance type in that the particle size distribution of droplets is narrow and the productivity of particles can be secured.

  The droplet forming process is not particularly limited as long as it is a process of forming a droplet by discharging a resin composition liquid containing a resin and a solvent from a plurality of discharge holes on a plane, and it is appropriately selected according to the purpose. It is preferable to use droplet forming means.

Next, a liquid column resonance type droplet forming unit as an example of the droplet forming unit will be described.
The liquid column resonance type droplet forming means forms a pressure standing wave by liquid column resonance by applying vibration to the resin composition liquid inside the liquid column resonance liquid chamber having at least one discharge hole, and pressure standing It is a means for discharging a resin composition liquid from at least one discharge hole arranged in a region which becomes an antinode of a wave to form a droplet.

  The liquid column resonance type droplet forming means has a liquid column resonance liquid chamber having at least one discharge hole, and a vibration generating portion for applying vibration to the resin composition liquid in the liquid column resonance liquid chamber, and a plurality of these are arranged. Preferably, a plurality of nozzle holes are arranged on a plane. The vibration generating section applies vibration to the resin composition liquid in the liquid column resonance liquid chamber to form a pressure standing wave by liquid column resonance, and the resin composition is formed from the discharge hole formed in the area which becomes the pressure standing wave The liquid can be discharged in the form of droplets.

  The “region that becomes the antinode of the pressure standing wave” is a region where the amplitude is large and the pressure fluctuation is large in the pressure wave of the liquid column resonance standing wave, and the pressure is large enough to eject the droplet. It is an area with fluctuations. There is no restriction | limiting in particular as an area | region used as the antinode of such a pressure standing wave, Although it can select suitably according to the objective, The position where the amplitude of a pressure standing wave becomes maximum (as a velocity standing wave From the clause (1), ± 1/3 wavelength is preferable, and ± 1/4 wavelength is more preferable toward the position where the local minimum is obtained. It is preferable that the discharge holes are formed in the area that becomes the antinode of the pressure standing wave, so that substantially uniform droplets can be formed from the respective discharge holes even when the plurality of discharge holes are opened. .

  The liquid column resonance liquid chamber is a liquid chamber capable of forming a pressure standing wave by the vibration applied by the vibration generating unit according to the principle of liquid column resonance phenomenon described later. Examples of the material forming the liquid column resonance liquid chamber include metals, ceramics, plastics, silicone and the like. Among these, those which do not dissolve in the resin composition liquid and do not cause denaturation of the resin composition liquid are preferable.

FIG. 1 is a schematic view showing an enlarged part of droplet forming means of a droplet discharge apparatus of a liquid column resonance type used in the present embodiment.
As shown in FIG. 1, the droplet forming means 11 of the present embodiment is provided with a liquid column resonance liquid chamber 18, and the liquid column resonance liquid chamber 18 has both ends in the longitudinal direction (left and right direction in FIG. 1). Among the side wall portions, the liquid common supply path 17 is in communication via a communication path provided in one side wall portion (opening side wall portion). Further, the liquid column resonance liquid chamber 18 has a plurality of discharges for discharging the droplets 21 to one wall (bottom wall in FIG. 1) of the walls connecting the side walls at both ends in the longitudinal direction. A hole 19 is provided. The carrier air flow 41 is made to flow in a direction parallel to the surface direction of the discharge hole surface. As a result, the droplets 21 discharged from the discharge holes 19 receive the carrier air flow from the direction orthogonal to the discharge direction, and are conveyed in the oblique direction. Thereby, the interval of the droplets 21 is enlarged, and the coalescence of the droplets 21 is suppressed. Further, on the upper wall side facing the discharge hole 19 in the liquid column resonance liquid chamber 18, a vibration generating means 20 for generating high frequency vibration to form a liquid column resonance standing wave through the diaphragm 22 is provided. It is provided. The vibration generating means 20 is connected to a high frequency power supply (not shown).

  As shown in FIG. 1, the liquid column resonance liquid chamber 18 discharges the resin composition liquid 14 in the liquid column resonance liquid chamber 18 in which liquid column resonance standing waves are generated as a droplet 21 from the discharge holes 19 by a mechanism described later. Do. The droplet forming means 11 constitutes a droplet forming unit in which a plurality of liquid column resonance liquid chambers are arranged.

  The length L between the wall surfaces at both ends in the longitudinal direction of the liquid column resonance liquid chamber 18 as shown in FIG. 1 is not particularly limited and may be appropriately selected according to the purpose. Preferably, it is determined based on the pillar resonance principle. Further, as shown in FIG. 2, the width W of the liquid column resonance liquid chamber 18 is not particularly limited and may be appropriately selected according to the purpose, but it is preferable not to give an extra frequency to the liquid column resonance. Preferably, the length is smaller than one half of the length L of the liquid column resonance liquid chamber 18.

  The number of liquid column resonance liquid chambers in the droplet forming means is not particularly limited, and can be appropriately selected according to the purpose. In order to dramatically improve the productivity of droplets, it is preferable that a plurality of droplets be arranged for one droplet forming means, and in the point that operability and productivity are compatible, 100 to 2,000 are More preferably, 200 to 1,000 are more preferable, and 300 to 700 are particularly preferable.

  There is no restriction | limiting in particular as a discharge hole, Although it can select suitably according to the objective, It is preferable that at least 1 discharge hole is arrange | positioned in at least 1 area | region of the area | region which becomes an antinode of a pressure standing wave Also, it is preferable that a plurality of the liquid column resonance liquid chambers are disposed.

  There is no restriction | limiting in particular as the number of objects of a discharge hole, According to the objective, it can select suitably. When the droplet forming means is a liquid column resonance type, the number of discharge holes formed in one liquid column resonance liquid chamber may be one, but it is preferable from the viewpoint of productivity to arrange a plurality of discharge holes. 2 to 100 are preferable, 4 to 60 are more preferable, and 4 to 20 are particularly preferable. When the number of discharge holes formed in one liquid column resonance liquid chamber exceeds 100, the voltage applied to the vibration generating means is set high when forming droplets of the desired resin composition liquid from the discharge holes. This may cause the behavior of the vibration generating means to become unstable. On the other hand, in the case of 4 to 20, the pressure standing wave is stabilized and productivity is maintained. The productivity increases as the number of ejection holes increases, but if the number exceeds 20, the ejection holes may become too dense, and the ejected droplets may coalesce to become coarse particles and adversely affect the image quality. .

  There is no restriction | limiting in particular as an opening diameter of a discharge hole, Although it can select suitably according to the objective, 1 [μm]-40 [μm] is preferable, 2 [μm]-15 [μm] is more preferable, 6 [μm] to 12 [μm] is particularly preferred. If the opening diameter is less than 1 μm, the formed droplets may be so small that particles (for example, toner) can not be obtained. When the opening diameter exceeds 40 [μm], the diameter of the droplets of the resin composition liquid is large, and when drying and solidifying this to obtain a desired particle size of 3 [μm] to 6 [μm], an organic solvent It is necessary to dilute the resin composition liquid (for example, toner composition liquid) to a very dilute liquid. In this case, a large amount of drying energy is required to obtain a certain amount of particles (for example, toner), and the time required for drying may be extended. On the other hand, when manufacturing the member in which the discharge hole is open when the diameter of the opening is 6 [μm] to 12 [μm], the variation in the hole diameter of many discharge holes can be kept small, and the discharge holes are densely packed. Is advantageous in that the productivity can be kept high. The opening diameter of the discharge hole is the diameter of the opening located on the side of the discharge hole from which the liquid droplets are discharged. If it is a perfect circle, it means the diameter and it is an ellipse, or a quadrangle, a hexagon, an octagon If it is a polygon or regular polygon such as, it means the mean diameter.

There is no restriction | limiting in particular as a cross-sectional shape of a discharge hole, According to the objective, it can select suitably.
FIGS. 3A to 3D show an example of the sectional shape of the discharge hole. The discharge hole 19 shown in FIG. 3A has a shape in which the opening diameter is narrowed while having a round shape from the liquid contact surface of the discharge hole 19 toward the discharge port. Therefore, the pressure applied to the liquid becomes maximum near the outlet of the discharge hole 19 when the thin film 42 in which the discharge hole of the liquid column resonance liquid chamber is formed vibrates, and therefore, the shape is the most preferable for the discharge stabilization.
The discharge hole 19 shown in FIG. 3B has a tapered shape having a taper angle A such that the opening diameter is narrowed at a constant angle from the liquid contact surface of the discharge hole 19 toward the discharge port. Here, the taper angle is a cross-section in the thickness direction of the surface (opening axis) perpendicular to the opening surface of the discharge hole 19 (surface perpendicular to the thickness direction of the formation surface of the discharge hole 19) and the formation surface of the discharge hole 19 Of the cross-sectional shape of the discharge hole 19 in the The taper angle A can be changed as appropriate. Similar to FIG. 3A, the pressure applied to the liquid can be increased near the outlet of the discharge hole 19 when the thin film 42 vibrates due to the taper angle A, but the range of the taper angle A is 60 °. -90 [°] is preferable. When the taper angle A is less than 60 °, pressure may not be applied to the resin composition liquid, and processing of the thin film 42 may be difficult. When the taper angle A is 90 [°], FIG. 3C corresponds. In this case, pressure may not easily be applied to the outlet of the discharge hole 19. If the taper angle exceeds 90 °, pressure may not be applied to the outlet of the discharge hole 19, and droplet discharge may be extremely destabilized. FIG. 3 (d) shows a shape obtained by combining FIG. 3 (a) and FIG. 3 (b). Thus, the shape may be changed stepwise.

  In addition, when a plurality of discharge holes are formed, the pitch between discharge holes (the shortest distance between the center portions of adjacent discharge holes) in one of the regions which become antinodes of the pressure standing wave is not particularly limited. Can be selected appropriately according to the purpose. 20 μm or more and the length L or less of the liquid column resonance liquid chamber are preferable, 20 μm to 200 μm is more preferable, 40 μm to 135 μm is further preferable, and 40 μm to 80 [μm] is particularly preferred. If the pitch between the discharge holes is less than 20 μm, the probability that the droplets discharged from the adjacent discharge holes collide with each other and become large drops increases, leading to the deterioration of the particle size distribution of the particles. There is. The pitch between the discharge holes may be all equally spaced between the discharge holes, or at least one pitch may be different, but it is necessary to obtain particles of uniform particle diameter that all are equally spaced. Is preferable in that

The vibration generating means is not particularly limited as long as it can be driven at a predetermined frequency and can impart vibration to the resin composition liquid in the liquid column resonance liquid chamber, and can be appropriately selected according to the purpose. A piezoelectric body, an ultrasonic vibration generation part, etc. are mentioned. There is no restriction | limiting in particular as a piezoelectric material, According to the objective, it can select suitably. For example, a piezoelectric body formed of piezoelectric ceramics such as lead zirconate titanate (PZT), piezoelectric polymers such as polyvinylidene fluoride (PVDF), single crystals such as quartz, LiNbO ₃ , LiTaO ₃ , KNbO ₃ or the like Etc. There is no restriction | limiting in particular as an ultrasonic vibration generation part, According to the objective, it can select suitably, For example, a magnetostriction element etc. are mentioned. Among these, a piezoelectric body is preferable. In general, the piezoelectric body is often used in lamination because the amount of displacement is small. It is preferable that the piezoelectric body be bonded to an elastic plate. The elastic plate forms a part of the wall of the liquid column resonance liquid chamber so that the piezoelectric body does not contact the liquid.

  The arrangement of the vibration generating means is not particularly limited and may be appropriately selected according to the purpose. However, with one wall (surface in the longitudinal direction) of the liquid column resonance liquid chamber in which at least one discharge hole is formed Preferably, it is formed on the facing wall. The vibration generating means is preferably bonded to an elastic plate, and the elastic plate preferably forms a part of the wall of the liquid column resonance liquid chamber so that the vibration generating means does not contact the liquid. . Furthermore, it is preferable that the vibration generating means be disposed so as to be individually controllable for each liquid column resonance liquid chamber. Further, it is preferable to dispose vibration generating means such as a block-like piezoelectric body via an elastic plate in accordance with the arrangement of the liquid column resonance liquid chambers from the viewpoint of individually controlling each liquid column resonance liquid chamber.

Next, the mechanism of droplet formation by the liquid column resonance type droplet formation means will be described.
The principle of the liquid column resonance phenomenon that occurs in the liquid column resonance liquid chamber (for example, the liquid column resonance liquid chamber 18 in the droplet forming means 11 of FIG. 1) will be described below. Assuming that the sound velocity of the resin composition liquid in the liquid column resonance liquid chamber is c, and the driving frequency given to the resin composition liquid as the medium from the vibration generating hand (for example, the vibration generating means 20 in FIG. 1) is f. The wavelength λ at which the resonance of the composition liquid occurs is in the relationship of the following formula (1).
λ = c / f formula (1)

Here, in the case where the liquid column resonance liquid chamber is both fixed ends or equivalent to both fixed ends, the length between the reflecting wall surfaces at both ends in the longitudinal direction of the liquid column resonance liquid chamber is the liquid column resonance liquid chamber Length L in the longitudinal direction. In this case, the resonance is most efficiently formed when the length L coincides with an even multiple of one quarter of the wavelength λ. That is, it is represented by the following formula (2).
L = (N / 4) λ formula (2)
However, N is an even number.
In addition, "when it is equivalent to a both-sides fixed end" is a case where it can be regarded that there is no pressure relief portion at a certain end. For example, if the height of the reflecting wall at one end is twice or more the height of the communication port for supplying the resin composition liquid, and the area of the reflecting wall at one end is the communication for supplying the resin composition liquid It refers to the case where the area of the opening of the mouth is twice or more. In FIG. 1, the length from the end of the frame at the fixed end of the liquid column resonance liquid chamber 18 to the end at the liquid common supply path 17 corresponds to the length L in FIG. In addition, the height h1 (= about 80 [μm]) of the end of the frame on the common liquid supply path 17 side is about twice the height h2 (= about 40 [μm]) of the communication port, and the end is It can be considered equivalent to a closed fixed end.

  Furthermore, the above equation (2) holds also in the case of both open ends where both ends are completely open. Similarly, if one side is equivalent to an open end with a pressure relief and the other side is closed (fixed end), that is, one fixed end or one open end, the length L Is most efficiently formed when it corresponds to an odd multiple of one quarter of the wavelength λ. That is, this corresponds to the case where N in the above equation (2) is represented by an odd number. In the case of open ends on both sides, L corresponds to an even multiple of a quarter of the wavelength, and in the case of fixed end on one side, L corresponds to an odd multiple of a quarter of the wavelength.

The following equation (3) is derived from the above equation (1) and the above equation (2) for the driving frequency f with the highest efficiency.
f = N × c / (4 L) formula (3)
Here, L represents the length of the liquid column resonance liquid chamber in the longitudinal direction, c represents the velocity of the sound wave of the resin composition liquid, and N represents an integer.

  Therefore, in the particle manufacturing apparatus and the particle manufacturing method of the present invention, it is preferable to apply vibration of the frequency f in which the above equation (3) holds, to the resin composition liquid. However, in practice, the resin composition liquid does not amplify vibrations infinitely because it has a viscosity that attenuates resonance, but has a Q value, as shown in formulas (4) and (5) described later. In addition, resonance occurs even at a frequency near the most efficient drive frequency f shown in the above equation (3).

  The shape (resonance mode) of the standing wave of the speed | velocity and pressure fluctuation in the case of N = 1, 2, 3 is shown in FIG. 4 (a)-(d). Although it is originally compression wave (longitudinal wave), it is generally described as shown in FIGS. 4 (a) to 4 (d). The solid line is the velocity standing wave (velocity distribution), and the dotted line is the pressure standing wave (pressure distribution).

  For example, as can be seen from FIG. 4A showing the case of N = 1 one-side fixed end, in the case of a velocity standing wave, the amplitude of the velocity standing wave becomes zero at the closed end and the amplitude is maximum at the aperture end. Become. When the length between both ends in the longitudinal direction of the liquid column resonance liquid chamber is L, the wavelength at which the liquid undergoes liquid column resonance is λ, and the integer N is 1 to 5 (N = 4 and 5 are not shown) Standing waves occur most efficiently. In addition, since the standing wave pattern differs depending on the open / close state of both ends, they are also described. As described later, the condition of the end portion is determined by the state of the opening of the discharge hole and the opening on the supply side.

  In acoustics, the open end is an end at which the moving speed of the medium (liquid) in the longitudinal direction becomes zero, and conversely, the pressure becomes maximum. At the closed end, conversely, it is defined as an end where the moving speed of the medium becomes zero. The closed end is considered as an acoustically hard wall, and wave reflections occur. In the case of ideally completely closed or open, superposition of waves produces a resonant standing wave having a form as shown in FIGS. 4 (a) to 4 (d). However, the standing wave pattern fluctuates depending on the number of discharge holes and the opening position of the discharge holes, and a resonance frequency appears at a position deviated from the position obtained from the above equation (3). In that case, stable discharge conditions can be created by appropriately adjusting the drive frequency.

  For example, the sound velocity c of the liquid is 1,200 m / s, the length L of the liquid column resonance liquid chamber is 1.85 mm, wall surfaces exist at both ends, and both ends are completely equivalent From the above equation (3), when the N = 2 resonance mode of is used, the most efficient resonance frequency is derived as 324 [kHz]. In another example, using the same conditions as described above, the sound velocity c of the liquid is 1200 m / s, the length L of the liquid column resonance liquid chamber is 1.85 mm, and there are wall surfaces at both ends, When N = 4 resonance modes equivalent to the fixed ends on both sides are used, the highest efficient resonance frequency is derived as 648 [kHz] from the above equation (3), and even in the liquid column resonance liquid chamber having the same configuration, Higher order resonances can be used.

  The liquid column resonance liquid chamber 18 in the droplet forming means 11 shown in FIG. 1 is an end portion which can be described as an acoustically soft wall under the influence of the opening of the discharge hole or both ends being equivalent to the closed end state. Although it is preferable to increase the frequency, it is not limited to this and may be an open end. Here, the influence of the opening of the discharge hole means that the acoustic impedance becomes smaller, and in particular, the compliance component becomes larger. Therefore, in the configuration in which wall surfaces are formed at both ends in the longitudinal direction of the liquid column resonance liquid chamber as shown in FIG. 4B, resonance modes at both fixed ends and all resonance modes at one open end where the discharge hole side is regarded as an opening Is a preferred configuration because it is available.

  Further, the numerical aperture of the discharge hole, the arrangement position of the opening, and the cross-sectional shape of the discharge hole also become factors to determine the drive frequency, and the drive frequency can be appropriately determined accordingly. For example, when the number of discharge holes is increased, the restraint of the tip of the liquid column resonance liquid chamber, which has been a fixed end, is loosened gradually, a resonant standing wave near the open end is generated, and the drive frequency is increased. In addition, the restriction condition is relaxed starting from the opening position of the discharge hole located closest to the liquid supply path, and the cross-sectional shape of the discharge hole is round or the volume of the discharge hole varies depending on the thickness of the frame. The upper standing wave has a short wavelength and is higher than the drive frequency. When a voltage is applied to the vibration generating unit at the driving frequency determined in this manner, the vibration generating unit is deformed to generate the resonant standing wave most efficiently at the driving frequency. The liquid column resonant standing wave is also generated at a frequency near the driving frequency at which the resonant standing wave is most efficiently generated. That is, the length between both ends in the longitudinal direction of the liquid column resonance liquid chamber is L, and the distance to the discharge hole closest to the liquid supply side end is Le. At this time, the vibration generating unit is vibrated using a drive waveform whose main component is the drive frequency f in the range determined by the following equation (4) and the following equation (5) using both the lengths L and Le. It is possible to eject liquid droplets from the ejection holes by inducing liquid column resonance.

N × c / (4 L) ≦ f ≦ N × c / (4 Le) Formula (4)
N × c / (4 L) ≦ f ≦ (N + 1) × c / (4 Le) (5)
Here, L represents the length of the liquid column resonance liquid chamber in the longitudinal direction, Le represents the distance to the discharge hole closest to the end on the liquid supply path side, c represents the velocity of the sound wave of the resin composition liquid, and N Represents an integer.
Preferably, the ratio of the length L between both ends in the longitudinal direction of the liquid column resonance liquid chamber and the distance Le to the discharge hole closest to the end on the liquid supply side is Le / L> 0.6.

  By using the principle of the liquid column resonance phenomenon described above, the liquid column resonance pressure standing wave is formed in the liquid column resonance liquid chamber 18 of FIG. 1 and the discharge holes 19 disposed in a part of the liquid column resonance liquid chamber 18. Discharge of the droplets 21 occurs continuously. It is preferable to dispose the discharge hole 19 at the position where the pressure of the standing wave fluctuates the most, since the discharge efficiency becomes high and the drive can be performed with a low voltage.

Next, the state of the liquid column resonance phenomenon generated in the liquid column resonance liquid chamber in the droplet discharge head in the droplet forming means will be described with reference to FIGS. 5 (a) to 5 (e). 5 (a) to 5 (e), the solid lines in the liquid column resonance liquid chamber indicate arbitrary measurement positions from the fixed end side in the liquid column resonance liquid chamber to the end on the common liquid supply path side. The velocity distribution is shown by plotting the velocity at the position of (1), the direction from the common fluid supply channel side to the liquid column resonance liquid chamber is "+", and the opposite direction is "-". Further, dotted lines in the liquid column resonance liquid chamber indicate pressure distributions obtained by plotting pressure values at arbitrary measurement positions from the fixed end side in the liquid column resonance liquid chamber to the end on the liquid common supply path side, The positive pressure is "+" and the negative pressure is "-" with respect to the atmospheric pressure. Further, if the pressure is positive, the pressure is applied downward in the drawing, and if the pressure is negative, the pressure is applied upward in the drawing.
Furthermore, in FIGS. 5 (a) to 5 (e), as described above, the liquid common supply passage side is opened, but the height at which the liquid common supply passage 17 and the liquid column resonance liquid chamber 18 communicate with each other (FIG. The height (height h1 shown in FIG. 1) of the frame which is the fixed end is about twice or more than the height h2) shown in FIG. Therefore, the liquid column resonance liquid chamber 18 shows temporal changes in velocity distribution and pressure distribution under the approximate condition that the both ends are both fixed ends.

  FIG. 5A shows a pressure waveform (pressure distribution) and a velocity waveform (velocity distribution) in the liquid column resonance liquid chamber 18 at the time of droplet discharge. Further, FIG. 5B shows that the meniscus pressure increases again after the liquid is drawn in immediately after the droplet discharge. As shown in FIGS. 5A and 5B, the pressure in the flow channel in which the discharge hole 19 is provided in the liquid column resonance liquid chamber 18 is a maximum. After that, as shown in FIG. 5C, the positive pressure in the vicinity of the discharge hole 19 becomes smaller, and the negative pressure is shifted to discharge the droplet 21. And as shown in FIG.5 (d), the pressure of the discharge hole 19 vicinity becomes the minimum. From this time, the filling of the resin composition liquid 14 into the liquid column resonance liquid chamber 18 starts. Thereafter, as shown in FIG. 5E, the negative pressure in the vicinity of the discharge hole 19 decreases and shifts in the direction of the positive pressure. At this point, the filling of the resin composition liquid 14 is completed. Then, as shown in FIG. 5A again, the positive pressure in the droplet discharge area of the liquid column resonance liquid chamber 18 is maximized, and the droplet 21 is discharged from the discharge hole 19. As described above, a standing wave is generated in the liquid column resonance liquid chamber by the high frequency driving of the vibration generating unit due to the liquid column resonance. In addition, since the discharge hole 19 is disposed in the droplet discharge area corresponding to the antinode of the standing wave by the liquid column resonance where the pressure fluctuates the most, the droplet 21 corresponds to the antinode cycle. The ink is discharged continuously from the discharge hole 19.

Next, the configuration of the particle production apparatus of the present embodiment will be described.
FIG. 6 is a schematic view illustrating the configuration of a particle production apparatus according to the present embodiment. As shown in FIG. 6, the droplets 21 discharged by the droplet forming means 11 are conveyed by the carrier air flow which is supplied by the air flow supply means 30 and whose temperature is adjusted. Then, the droplets are transported to the particle forming unit 60, and the droplets are dried and solidified, transported to the particle capturing unit 70 as a capturing unit, and collected as solid particles. The droplets discharged from the droplet forming means 11 can be formed continuously. It is desirable that the air flow supply means 30 supply a carrier air flow from the lateral direction to the air flow path in the droplet discharge direction, and carry the droplets by the carrier air flow. This is because the distance between droplets can be effectively separated. In the case of the same direction as the droplet discharge direction, the air flow stagnates in the vicinity of the discharge holes arranged on a plane, so that the droplets can not be separated, and the droplets are likely to be in contact with each other.

  As shown in FIG. 6, an example of a liquid transfer form of the resin composition liquid 14 to the droplet forming means 11 (droplet forming unit) will be described. In the particle manufacturing apparatus 1, the resin composition liquid 14 contained in the raw material container 13 is pressure-fed by the liquid circulation pump 15 through the liquid supply pipe 16 and supplied to the droplet forming means 11. Furthermore, the resin composition liquid 14 returns from the droplet forming means 11 to the raw material container 13 through the liquid return pipe 23.

  The resin composition liquid 14 contained in the raw material container 13 shown in FIG. 6 flows into the common liquid supply path 17 through the liquid supply pipe 16 by the liquid circulation pump 15 for circulating the resin composition liquid 14. , And is supplied to the liquid column resonance liquid chamber 18. Then, in the liquid column resonance liquid chamber 18 filled with the resin composition liquid 14, a pressure distribution is formed by the liquid column resonance standing wave generated by the vibration generating means 20. Then, in the liquid column resonance standing wave, the droplet 21 is discharged from the discharge hole 19 which is a portion having a large amplitude and having a large pressure fluctuation and which is an antinode of the pressure standing wave.

  The liquid transfer pressure to the droplet forming means 11 and the pressure in the particle forming means 60 are controlled by a liquid pressure gauge P1 and a pressure gauge P2 in the particle forming means 60. At this time, if P1> P2, the resin composition liquid 14 may exude from the discharge hole, and if P1 <P2, gas may enter the droplet forming means 11 and the discharge may be stopped. Therefore, it is desirable to have P1 ≒ P2.

  The resin composition liquid 14 having passed through the common liquid supply path 17 flows through the liquid return pipe 23 shown in FIG. 6 and is returned to the raw material container 13. By discharging the droplets 21, the amount of the resin composition liquid 14 in the liquid column resonance liquid chamber 18 decreases. Then, the suction force by the action of the liquid column resonance standing wave in the liquid column resonance liquid chamber 18 acts, and the flow rate of the resin composition liquid 14 supplied from the liquid common supply path 17 increases, and the liquid column resonance liquid chamber 18 The resin composition liquid 14 is replenished inside. Then, when the resin composition liquid 14 is replenished in the liquid column resonance liquid chamber 18, the flow rate of the resin composition liquid 14 passing through the common liquid supply path 17 returns to the original, and the liquid supply pipe 16 and the liquid return pipe 23 The flow of the resin composition liquid 14 circulating in the apparatus is again formed.

  As shown in FIG. 1, the droplets 21 of the resin composition liquid 14 discharged from the droplet forming means 11 in the droplet forming step are transported by the transport air flow generating means (not shown) into the air flow passage 12. As the air flow 41 passes, it flows out to the particle forming means 60 side shown in FIG.

  As shown in FIG. 6, the droplets 21 formed by the droplet forming unit (droplet forming unit 11) fall within the chamber 61 of the particle forming unit 60. At that time, the droplets 21 fall on the air flow sent from the transfer air flow inlet 64 at the top of the chamber 61 and are dried in the air flow until reaching the transfer air flow outlet 65. The solidified particles collected by the particle collection unit 71 are stored in the particle storage unit 72. If necessary, it is additionally dried by a secondary drying means not shown.

  In the particle manufacturing apparatus 1 shown in FIG. 6, the droplets 21 discharged in the right direction of FIG. 6 from the droplet forming means 11 are conveyed by the carrier air flow 41 flowing from the upper side of FIG. When the jetted droplets come in contact with each other before drying, the droplets coalesce and become one particle (hereinafter, this phenomenon may be referred to as "cohesion"). In order to obtain solidified particles having a uniform particle size distribution, it is necessary to maintain the distance between the jetted droplets. However, the ejected droplets have a constant initial velocity, but eventually stall due to air resistance. The stalled particles catch up with droplets ejected later, resulting in coalescence. Since this phenomenon occurs constantly, the particle size distribution will be greatly deteriorated when the particles are collected. In order to prevent coalescence, it is preferable to transport while solidifying the droplets while preventing coalescence by lowering the droplet speed and preventing coalescence between the droplets. Therefore, it is preferable to transport the solidified particles to the particle collection means 70 by the air flow, in terms of high production efficiency.

  As shown in FIG. 6, as long as it is a means capable of adjusting the temperature of the carrier air flow 41 supplied by the air supply means 30 and supplying the carrier air flow 41 into the air flow path, there is no particular limitation, and it is suitable according to the purpose. It can be selected. The temperature adjustment step is not particularly limited as long as it is a step capable of adjusting the temperature of the carrier air flow 41 by the droplet conveyance means, and can be appropriately selected according to the purpose, but using the air flow supply means 30 preferable. Although not shown in FIG. 6 as the air flow supply means 30, it is preferable that the air flow adjustment means have a control mechanism that measures the air flow temperature and stabilizes the air flow temperature. Although this embodiment has a plurality of air flow supply means, it has a mechanism capable of adjusting the temperature of each air flow supply means.

  As shown in FIG. 6, as the particle forming means 60, there is no particular limitation as long as it is a means for drying and solidifying the droplets 21 in a gas flow to form the particles, which may be appropriately selected according to the purpose. it can. The particle forming step is not particularly limited as long as it is a step of forming the particles by drying and solidifying the droplets 21 in a gas flow, and can be appropriately selected according to the purpose, but using the particle forming means Is preferred.

  There is no restriction | limiting in particular as a method to dry and solidify the droplet 21 in air flow (Hereafter, it distinguishes from the above-mentioned "conveyance air flow", and it calls it simply air flow.), According to the objective, it can select suitably. After discharging the droplets 21 out of the discharge holes by the droplet forming means 11, the droplets 21 are dried while being transported by air flow, that is, while the droplets 21 are being transported by air flow, the solvent in the droplets is in the air stream And the like. There is no restriction | limiting in particular as an air flow velocity, Although it can select suitably according to the objective, It is preferable that a droplet and the particle | grain which dried the droplet have a faster free fall speed. There is no restriction | limiting in particular as atmosphere (temperature, vapor pressure, the kind of gas, etc.) of the gas used for airflow, According to the objective, it can select suitably. Examples of the type of gas include air and nonflammable gases such as nitrogen. These may be used alone or in combination of two or more.

  The particles obtained by drying the droplets may not be completely dried as long as the solid state can be maintained. In order to improve the productivity, the particle drying time can be suppressed by collecting in a minimum collectable dry state and further drying in a separated state from the carrier air flow having a large amount of solvent vapor.

  As shown in FIG. 6, the particle collecting means 70 as the collecting means separates the air stream and the solidified particles, and there is no particular limitation as long as they can collect the particles. For example, known materials such as cyclones and bag filters may be used. it can. Also, both a cyclone and a bag filter may be used. In the present invention, since the solidified particles have the property of being easily softened, a cyclone is used at the front stage and a bag filter is used at the rear stage. As a result, filter clogging when particles are softened by the bag filter can be easily suppressed, and passage of an extremely small amount of ultrafine particles that can not be collected by the cyclone can be reliably suppressed, and emission to the atmosphere can be suppressed.

  After the solidified particles are collected, it is preferable to carry out a secondary drying step described later.

  As other means, secondary drying means etc. are mentioned, for example. As another process, a secondary drying process etc. are mentioned, for example.

  The secondary drying means is not particularly limited as long as it is a means for further drying the particles formed in the particle forming step, and can be appropriately selected according to the purpose. For example, a fluidized bed drying device, a vacuum drying device Etc. The secondary drying step is not particularly limited as long as it is a step of further drying the particles formed in the particle forming step, and can be appropriately selected according to the purpose, but it is preferable to carry out by the secondary drying means .

  When the particles are toner particles, when the content of the solvent contained (remained) in the particles formed in the particle forming step is large, the toner characteristics such as heat resistance storage stability, fixing property, charging characteristics, etc. fluctuate over time Not only that, the solvent evaporates at the time of fixing by heating. This increases the possibility of adversely affecting the user and peripheral devices. Therefore, it is preferable to reduce the solvent in the particles by the secondary drying step.

  In the case where the particles to be produced do not contain a resin component such as particles for secondary battery positive electrode materials, the resin is produced after producing the particles from the resin composition liquid (after the particle forming step) or in the particle forming step. Heat treatment is performed to thermally decompose the components. Thereby, the resin component can be thermally decomposed to obtain particles for a secondary battery positive electrode material. There is no restriction | limiting in particular as a heating temperature in heat processing, if it is the temperature which can thermally decompose the resin component contained in a resin composition liquid, According to the objective, it can select suitably.

  As some of the discharge holes become clogged and the discharge becomes discontinuous with time, and the discharge amount of the resin composition liquid decreases, the amount of solvent volatilized in the particle forming means or the particle forming step decreases. Since the latent heat of vaporization is deprived from the air flow when the solvent evaporates, the temperature of the air flow at the conveyance air flow outlet 65 (see FIG. 6) is lower than the temperature of the conveyance air flow inlet 64 (see FIG. 6). When the amount of droplets to be dried decreases with time, the temperature of the air flow at the transport air flow outlet increases with time.

Therefore, the temperature of the air stream and the temperature of the particles in the particle forming means or in the particle forming step were measured when the discharge amount of the resin composition liquid decreased.
For example, consider the case of the following collection condition 1.
Airflow volume of the carrier air flow inlet 64 (see FIG. 6): 60 [m ³ / hour]
Type of gas in air flow: Nitrogen gas Temperature of air flow in the carrier air flow inlet: 95 [° C]
Solid content concentration of resin composition liquid: 10 [mass%]
Solvent type of resin composition liquid: Ethyl acetate (boiling point 77 [° C])
Latent heat of evaporation of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara, et al., P. 569)
Average particle size of particles produced: 5.4 [μm]
Specific gravity of particle: 1.2 [g / cm ³ ]
Droplet forming means: liquid column resonance type (see FIGS. 1 and 2)
Number of discharge holes of droplet forming unit: 10240 [piece]
Frequency at discharge: 310 [kHz]
Distance from the carrier air flow inlet 64 to the carrier air flow outlet 65: 3000 [mm]
Under the above conditions, assuming that 6 [mass%] solvent is left to obtain dried particles, the temperature of the air flow is lowered by the latent heat of evaporation of the solvent, and the air flow and particles at the carrier air flow outlet 65 after 60 seconds from the discharge start Temperature became 31 [° C.].

  However, since the droplet forming means 11 is exposed to the carrier air flow of 95 ° C., the temperature gradually rises and the droplet discharge amount decreases. After 10 minutes, the droplet discharge amount was reduced by half, and the temperature of the air flow at the transfer air flow outlet 65 became 55 [° C.]. This is because the temperature of the carrier air flow greatly exceeds the boiling point of the solvent of the raw material liquid, the heat from the carrier air flow raises the temperature of the droplet forming means.

  As described above, when the discharge amount of the resin composition liquid decreases with time, the temperature decrease of the air flow decreases accordingly. Therefore, the drying over time becomes unstable. Further, as described above, since the temperature of the solidified particles substantially matches the temperature of the air flow of the carrier air flow outlet 65, in the case of the collection condition 2, the solidified particles have a temperature higher than the collection condition 1 It solidifies in the state and reaches the particle collection means 70 (see FIG. 6). The softening temperature of the solidified particles collected at the initial stage of droplet discharge was about 37 [° C.]. Under the collection condition 1, the temperature of the solidified particles collected in the initial stage is below the softening temperature, so the particles remain solid and can be collected by the collection means and the collection process. However, after about 10 minutes, the air stream temperature reaches 55 ° C., and the temperature of the solidified particles exceeds the softening temperature, so the particles are collected in a softened state. In the collected particles, the solidified basic particles (see FIG. 8) adhere to each other because the probability that the particles contact with each other is significantly increased, and a large amount of grape-like particles (see FIGS. 9 and 10) are generated. As a result, the particle size distribution is aggravated. Once it is vine-like, it is very difficult to solve. As a reference, the particle size distribution in the case of containing grape-like particles is shown in FIG. 11, and the particle size distribution in the case of not containing grape-like particles is shown in FIG. Comparing the particle size distributions of FIG. 11 and FIG. 12, it can be seen that the vine-like particles greatly deteriorate the particle size distribution.

  As shown in FIG. 6, in the particle manufacturing apparatus 1, since the discharge holes of the droplet forming means 11 are exposed to the carrier air flow 41, the temperature is almost the same as the carrier air flow 41. The carrier air stream 41 needs to be at a high temperature for particle drying as described above. When the discharge holes of the droplet forming means 11 are directly exposed to the carrier air flow 41, the raw material liquid present in the flatly formed discharge holes of the droplet forming means 11 is dried, solidified and clogged, or droplets are formed. The solvent in the raw material liquid inside the means 11 boils, and the droplet 21 can not be discharged. Therefore, by using the first air flow supply means 31, the second air flow supply means 32, and the air flow distribution means 35, the first carrier air flow 41a flowing around the droplet forming means 11 and the heat quantity necessary for drying the droplets are obtained. The second carrier air flow 41b is divided. Thereby, the droplets 21 can be efficiently dried to obtain fine particles while preventing nozzle clogging. Therefore, in the present embodiment, the temperature of the first carrier air stream 41a flowing in the vicinity of the droplet forming means by the plurality of air stream supplying means needs to be relatively low so as to prevent the drying of the discharge holes. The temperature is preferably not higher than the boiling point of the raw material liquid, more preferably 20 ° C. or more lower than the boiling point of the raw material liquid, and still more preferably 40 ° C. lower than the boiling point of the raw material liquid. However, depending on the raw material liquid, if the temperature is lowered too much, another problem such as precipitation of the melt may occur, and it is desirable to set the temperature of the first carrier air stream 41a as low as possible. The first air flow supply means 31 and the second air flow supply means 32 include a heater and a fan.

  The plurality of carrier air flows 41 (the first carrier air flow 41 a and the second carrier air flow 41 b) have a layer thickness (height) of the carrier air flow from the discharge hole surface of the droplet forming means 11 in which the discharge holes are formed. ) Can be adjusted. Thereby, the temperature rise of the discharge hole surface formed in the droplet forming means 11 can be reduced. In order to mix the transport air currents (the first transport air stream 41a and the second transport air stream 41b) at a plurality of temperatures in a short time, the air stream distribution means 35 is as possible of the transport air stream 41 of the droplet forming means 11 in the droplet transfer means. It is desirable to be located upstream. As for the layer thickness (height) of the conveyance airflow of the 1st conveyance airflow 41a, 0.5 [mm] or more and less than 10 [mm] are desirable. If it is less than 0.5 [mm], the effect of lowering the surface temperature of the discharge hole surface can not be obtained sufficiently. If it is 10 [mm] or more, it is necessary to extremely increase the temperature of the second carrier air flow 41b, so it becomes difficult to provide the air flow with a sufficient amount of heat to dry the droplets.

  Furthermore, in order to enhance the effect of the present embodiment, immediately after the air flow distribution means 35, an air flow straightening means 36 is provided which forms a parallel flow and rectifies the carrier air flow. As a result, the first transport air flow 41a and the second transport air flow 41b at a plurality of temperatures pass near the droplet forming means 11 in a layered state without mixing. Therefore, the temperature rise of the discharge hole surface formed in the droplet forming means 11 can be further reduced. The air flow straightening means 36 may have a honeycomb shape, or may be a flat plate parallel to the air flow path on which the droplet forming means 11 is disposed in a direction perpendicular to the direction of the air flow. The flat plate may be stacked in layers parallel to the air flow path on which the. A well-known means can be used if the rectification effect is obtained, and it is preferably in a honeycomb shape. In the case of using a honeycomb shape, the type of plate constituting the honeycomb shape is desirably a metal and thin plate, but any material or shape may be used as long as it has an airflow rectifying effect. The smaller the pore diameter of the honeycomb shape, the more the rectification effect can be expected, but if it is too small, the pressure loss increases and the flow of the air flow is hindered, so the pore diameter is preferably about 0.1 mm to 10 mm. More preferably, it is 0.5 [mm]-2 "mm". Although two airflow supply means are provided as airflows of a plurality of temperatures in FIG. 6, two or three or more airflow supply means may be provided. As shown in FIG. 7, two or more air flow supply means may be provided. In this case, the temperature of the air stream may be raised stepwise as it goes away from the droplet forming means.

Raw material liquid
(Resin composition liquid)
The resin composition liquid contains at least a resin and a solvent, and further contains other components as required. Examples of the resin composition liquid include a resin composition liquid in which at least a resin is dissolved or dispersed in a solvent. The particle production apparatus and the particle production method of the present invention can also be suitably used as a toner production apparatus and a toner production method. The resin composition liquid in this case is a toner composition liquid. When the resin composition liquid is a toner composition liquid, examples of other components in the toner composition liquid include a colorant, a release agent, a charge control agent, a magnetic material, an additive, and the like. Hereinafter, the composition of the resin composition liquid (toner composition liquid) particularly suitable for toner production will be described in detail, but the resin composition liquid in the present invention is not limited to the resin composition liquid for producing toner. It may be a resin composition liquid for producing spacer particles of a liquid crystal panel, a resin composition liquid for producing colored fine particles for electronic paper, or a resin composition liquid for producing a drug carrier of a medicine.

(resin)
There is no restriction | limiting in particular as resin, Although it can select suitably according to the objective, It is preferable that it is what is disperse | distributed thru | or melt | dissolved in a solvent, For example, binder resin etc. are mentioned. As the binder resin, for example, a vinyl polymer comprising a styrene-based monomer, an acrylic monomer, a methacrylic monomer, etc., a copolymer of these monomers or two or more kinds, a polyester resin, Polyol resin, phenol resin, silicone resin, polyurethane resin, polyamide resin, furan resin, epoxy resin, xylene resin, terpene resin, coumarone indene resin, polycarbonate resin, petroleum resin and the like. These may be used alone or in combination of two or more.

  As a monomer which comprises polyester resin, an alcohol component, an acid component, etc. are mentioned, for example.

  Examples of the alcohol component include dihydric alcohol components and trivalent or higher alcohol components. Examples of the divalent alcohol component include ethylene glycol, propylene glycol, 1,3-butanediol, 1,4-butanediol, 2,3-butanediol, diethylene glycol, triethylene glycol, 1,5-pentanediol, 1,6-hexanediol, neopentyl glycol, 2-ethyl-1,3-hexanediol, hydrogenated bisphenol A, diol obtained by polymerizing cyclic ether such as ethylene oxide and propylene oxide to bisphenol A . Examples of the trivalent or higher alcohol component include sorbitol, 1,2,3,6-hexanetetrol, 1,4-sorbitan, pentaerythritol, dipentaerythritol, tripentaerythritol, and 1,2,4-butane Triol, 1,2,5-pentatriol, glycerol, 2-methylpropanetriol, 2-methyl-1,2,4-butanetriol, trimethylolethane, trimethylolpropane, 1,3,5-trihydroxybenzene etc. Can be mentioned.

Examples of the acid component include divalent carboxylic acids and trivalent or higher carboxylic acids. Examples of the divalent carboxylic acid include benzenedicarboxylic acid or its anhydride, alkyldicarboxylic acid or its anhydride, unsaturated dibasic acid or its anhydride, and the like. Examples of benzenedicarboxylic acid include phthalic acid, isophthalic acid and terephthalic acid. Examples of the alkyl dicarboxylic acid include succinic acid, adipic acid, sebacic acid, azelaic acid and the like. Examples of unsaturated dibasic acids include maleic acid, citraconic acid, itaconic acid, alkenylsuccinic acid, fumaric acid, mesaconic acid and the like.
Examples of trivalent or higher carboxylic acid components include trimellitic acid, pyromellitic acid, 1,2,4-benzenetricarboxylic acid, 1,2,5-benzenetricarboxylic acid, 2,5,7-naphthalenetricarboxylic acid, 1,2,4-naphthalenetricarboxylic acid, 1,2,4-butanetricarboxylic acid, 1,2,5-hexanetricarboxylic acid, 1,3-dicarboxy-2-methyl-2-methylenecarboxypropane, tetra (methylene) Carboxy) methane, 1,2,7,8-octane tetracarboxylic acid, empol trimer acid, their anhydrides, partial lower alkyl esters, etc. may be mentioned.

  In order to crosslink the polyester resin, it is preferable to use a trivalent or higher alcohol or a trivalent or higher carboxylic acid in combination. In that case, it is necessary to make it a small addition amount of the range which does not prevent resin dissolving in a solvent.

  When the binder resin is a polyester resin, the molecular weight thereof is not particularly limited and may be appropriately selected depending on the purpose. However, the molecular weight distribution by GPC (gel permeation chromatography analysis) has a molecular weight of 3,000 to The presence of at least one peak in the area of 50,000 is preferable in terms of toner fixability and hot offset resistance. In addition, as the molecular weight of the tetrahydrofuran (THF) soluble component, a binder resin having a component of 100,000 or less at 60% to 100% is preferable from the viewpoint of dischargeability, and a molecular weight of 5,000 to More preferred is a binder resin having at least one peak in the 20,000 region.

  When the binder resin is a polyester resin, the acid value thereof is not particularly limited and may be appropriately selected depending on the purpose, but preferably 0.1 [mg KOH / g] to 100 [mg KOH / g], 0.1 [mg KOH / g] to 70 [mg KOH / g] is more preferable, and 0.1 [mg KOH / g] to 50 [mg KOH / g] is particularly preferable. In the present invention, the acid value of the resin is measured in accordance with JIS K-0070.

(solvent)
The solvent is not particularly limited as long as it can dissolve and disperse the resin, and can be appropriately selected according to the purpose. However, droplets formed in the droplet forming means or the droplet forming step (from the discharge holes) It is preferable to use a solvent which can be easily dried, since the droplets (liquid droplets) discharged into the gas phase are dried in the particle forming means or in the particle forming step. As such a solvent, one having a boiling point of 100 [° C.] or less is preferable in that the drying speed is fast. As a solvent whose boiling point is 100 [° C.] or less, for example, ethers, ketones, esters, aromatic hydrocarbons, alcohols and the like can be mentioned. Examples of the ethers include tetrahydrofuran (THF) and the like. As ketones, acetone, methyl ethyl ketone (MEK), methyl isobutyl ketone etc. are mentioned, for example. As esters, for example, ethyl acetate, butyl acetate and the like can be mentioned. Examples of aromatic hydrocarbons include toluene, xylene and the like. Examples of alcohols include methanol, ethanol, butanol and the like. These may be used alone or in combination of two or more. Among these, tetrahydrofuran (THF), acetone, methyl ethyl ketone (MEK), ethyl acetate, toluene and xylene are preferable.

(Colorant)
There is no restriction | limiting in particular as a coloring agent, A conventionally well-known pigment, dye, etc. can be used. There is no restriction | limiting in particular as content of the coloring agent in a resin composition liquid, Although it can select suitably according to the objective, 1 [mass%]-15 [mass%] is preferable with respect to the toner obtained. 3 [mass%]-10 [mass%] are more preferable.

  The coloring agent can also be used as a master batch complexed with a resin (resin for master batch). A masterbatch is generally one in which the pigment is dispersed in hardness in the masterbatch resin by subjecting the mixture of the pigment and the masterbatch resin to high shear. Therefore, if sufficient dispersion of the pigment is obtained, the masterbatch may not be used.

  The resin for master batch is not particularly limited, and conventionally known resins can be used. These may be used singly or in combination of two or more.

  As a usage-amount of a masterbatch, 0.1 mass part-20 mass parts are preferable with respect to 100 mass parts of binder resin.

  A dispersing agent may be used to enhance the dispersibility of the pigment during masterbatch production. The dispersant is preferably highly compatible with the binder resin in terms of pigment dispersibility, and conventionally known ones can be used. Specific examples of commercially available dispersants include, under the trade names, Addisper PB 821, Addisper PB 822 (all manufactured by Ajinomoto Fine Techno Co., Ltd.), Disperbyk-2001 (manufactured by Bick Chemie Co., Ltd.), EFKA (registered trademark)-4010 (Manufactured by EFKA) and the like.

  There is no restriction | limiting in particular as content of a dispersing agent, Although it can select suitably according to the objective, 0.1 [mass%]-10 [mass%] are preferable with respect to a coloring agent. When the content is less than 0.1% by mass, the pigment dispersibility may be insufficient, and when it exceeds 10% by mass, the chargeability under high humidity may be reduced. .

(Release agent)
There is no restriction | limiting in particular as a mold release agent, Although it can select suitably according to the objective, Wax is preferable. The wax is not particularly limited and may be appropriately selected according to the purpose. Examples thereof include aliphatic hydrocarbon waxes, oxides of aliphatic hydrocarbon waxes, and block copolymers thereof, vegetable waxes, Examples include animal waxes, mineral waxes, and fatty acid esters as main components. Further, it is also possible to use one obtained by deoxidizing a part or all of the fatty acid ester. Examples of aliphatic hydrocarbon waxes include low molecular weight polyethylene, low molecular weight polypropylene, polyolefin wax, microcrystalline wax, paraffin wax, and sasol wax. Examples of the oxide of aliphatic hydrocarbon wax include oxidized polyethylene wax and the like. Examples of plant waxes include candelilla wax, carnauba wax, wax wax, jojoba wax and the like. Examples of animal waxes include, for example, beeswax, lanolin, spermaceti and the like. As mineral-based wax, for example, ozokerite, ceresin, petrolatum and the like can be mentioned. Examples of the fatty acid ester as a main component include montanic acid ester wax and castor wax.

  There is no restriction | limiting in particular as melting | fusing point of a mold release agent, Although it can select suitably according to the objective, 70 [degreeC]-140 [degreeC] is preferred at the point which balances fixability and hot offset resistance. And 70 [° C.] to 120 [° C.] are more preferable. If the melting point is less than 70 ° C., the blocking resistance may be lowered, and if it exceeds 140 ° C., it may be difficult to exhibit the hot offset resistance effect. In addition, let the temperature of the peak top of the maximum peak of the endothermic peak of the mold release agent measured by DSC (differential scanning calorimetry) be the melting point of the mold release agent.

  The DSC is preferably measured by a high-precision, internally-heated, input-compensated, differential scanning calorimeter. As a measuring method, it carries out according to ASTM D3418-82. The DSC curve uses one that is measured when the temperature is raised at a temperature rate of 10 [° C./min] after the temperature rise and fall once to obtain a history before heat treatment.

  There is no restriction | limiting in particular as content of the mold release agent in a resin composition liquid, Although it can select suitably according to the objective, 0.2 mass part-20 mass parts are with respect to 100 mass parts of binder resin. Preferably, 0.5 parts by mass to 10 parts by mass is more preferable.

(Additive)
There is no restriction | limiting in particular as an additive, According to the objective, it can select suitably. For resin composition liquid (toner composition liquid), for example, protection of electrostatic latent image carrier and carrier, improvement of cleanability, adjustment of thermal characteristics, electrical characteristics, physical characteristics, resistance adjustment, softening point adjustment, fixing rate improvement Additives such as various metal soaps, fluorosurfactants, dioctyl phthalate, conductivity imparting agents, inorganic fine particles and the like can be added as necessary for the purpose. The inorganic fine particles may be made hydrophobic if necessary. In addition, a small amount of an abrasive, an anti-caking agent, and further, white particles and black particles of reverse polarity to toner particles can be used as a developability improver which is one of the additives. These may be used alone or in combination of two or more. Among these, inorganic fine particles are preferable.

  These additives may be subjected to surface treatment with a surface treatment agent for the purpose of charge amount control and the like. The surface treatment of the additive is advantageous in that the hydrophobicity can be increased and deterioration of the additive itself can be prevented even under high humidity. As a surface treatment agent, for example, a silane coupling agent, a silylating agent, a silane coupling agent having a functional group, an organosilicon compound, an organic titanate coupling agent, an aluminum coupling agent, a silicone varnish, a silicone oil, A modified silicone oil etc. are mentioned.

There is no restriction | limiting in particular as a primary particle diameter of an additive, Although it can select suitably according to the objective, 5 [nm]-2 [micrometers] are preferable, and 5 [nm]-500 [nm] are more preferable preferable. Moreover, there is no restriction | limiting in particular as a specific surface area by the BET method of an additive, Although it can select suitably according to the objective, 20 [m < ² > / g]-500 [m < ² > / g] is preferable. There is no restriction | limiting in particular as content of an additive, Although it can select suitably according to the objective, When particle | grains are used as a toner, 0.01 [mass%]-5 [mass] is said with respect to this toner. %] Is preferable and 0.01 [mass%]-2.0 [mass%] are more preferable.

  The solid concentration in the resin composition liquid is not particularly limited as long as droplets can be formed, and can be appropriately selected according to the purpose. It is preferable that the change in physical properties such as solution viscosity, sound velocity of liquid, surface tension of liquid, etc. is small because the discharge conditions do not need to be largely changed, and 30 mass% or less is more preferable, 5 mass% to 20 % By mass is more preferable. If the solid content concentration is less than 5 [mass%], drying energy etc. may increase in the particle forming step, and the efficiency in production may decrease, and if it exceeds 20 [mass%], discharge Since it is necessary to change the conditions largely, stable and uniform droplet formation may not be possible.

  The particle production apparatus and particle production method of the present invention are, for example, toners for electrophotography, spacer particles for liquid crystal panels, colored particles for electronic paper, particles for electrode materials of secondary batteries and fuel cells, drug carriers for medicines, etc. It can be used to produce various particles.

  EXAMPLES Hereinafter, examples of the present invention will be described, but the present invention is not limited to the following examples. The term "parts" refers to "parts by mass" unless otherwise specified. "%" Represents "% by mass" unless otherwise specified.

(Production example)
<Production of Resin Composition Liquid (Toner Composition Liquid)>
(Preparation of Colorant Dispersion)
First, a dispersion of carbon black as a colorant was prepared.
17 parts of carbon black (Rega L400, manufactured by Cabot) and 3 parts of a pigment dispersant were added to 80 parts of ethyl acetate, and were primarily dispersed using a mixer having a stirring blade. As the pigment dispersant, Agisper PB 821 (manufactured by Ajinomoto Fine Techno Co., Ltd.) was used. The obtained primary dispersion is finely dispersed by a strong shear force using a bead mill (LMZ type manufactured by Ashizawa Finetech, zirconia bead diameter 0.3 [mm]), and aggregates of 5 [μm] or more are completely eliminated. The secondary dispersion (colorant dispersion) was obtained.

(Preparation of wax dispersion)
Next, a wax dispersion was prepared.
Eighteen parts of carnauba wax (manufactured by Toa Kasei Co., Ltd .: WA-03) and 2 parts of a wax dispersant were added to 80 parts by mass of ethyl acetate, and primary dispersion was performed using a mixer having stirring blades. The temperature of the primary dispersion was raised to 80 ° C. while stirring to dissolve carnauba wax, and then the temperature of the solution was lowered to room temperature to precipitate wax particles so that the maximum diameter was 3 μm or less. As the wax dispersant, polyethylene wax on which a styrene-butyl acrylate copolymer was grafted was used. The obtained dispersion is further finely dispersed by a strong shear force using a bead mill (LMZ type manufactured by Ashizawa Finetech, zirconia bead diameter 0.3 [mm]) so that the maximum diameter is 1 μm or less Adjusted to obtain a wax dispersion.

(Dissolution, preparation of dispersion)
Next, a toner composition liquid comprising the following composition to which a resin as a binder resin, a colorant dispersion and a wax dispersion were added was prepared.
100 parts of a polyester resin as a binder resin (glass transition temperature = 60.5 [° C.], weight average molecular weight Mw = 35,000), 30 parts of a colorant dispersion, and 30 parts of a wax dispersion, 840 parts of ethyl acetate The mixture was stirred for 10 minutes using a mixer having a stirring blade and uniformly dispersed. Shock due to solvent dilution did not cause aggregation of pigment or wax particles.

Example 1
Next, an example of the particle manufacturing apparatus of the above embodiment (hereinafter, this example will be referred to as “example 1”) will be described.
In Example 1, a particle production apparatus shown in FIG. 6 was used. The details of the device are as follows.
The particle forming means 60 shown in FIG. 6 has a cylindrical shape with an inner diameter of 400 mm and a height of 3,000 mm, which is vertically fixed and has a chamber 61 in which the upper end and the lower end are narrowed. Have. The transport air flow introduction port 64 has a surface of droplet formation means of 80 mm and is formed in a rectangular cross section with a height of 15 mm. The inner diameter of the carrier air flow outlet 65 is 80 [mmφ]. The droplet forming means 11 is disposed at a position of 30 [mm] above the upper end in the chamber 61. In the conveyance air flow 41, nitrogen gas is used, and the air flow velocity is 10.0 [m / s], and the air flow temperature is 75 [° C.] (conditions at the conveyance air flow outlet 65).

  As shown in FIG. 5A, the resonance mode in which the length L between the longitudinal ends of the liquid column resonance liquid chamber in the droplet forming means is 1.85 mm and N = 2, The 1st to 4th discharge holes were used at the position of the antinode of the pressure standing wave of the resonance mode of N = 2. As a drive signal generation source (not shown), a function generator (WF 1973, manufactured by NF Circuit Design Block Co., Ltd.) was used, and it was connected to the vibration generation means 20 by a lead wire coated with polyethylene. The driving frequency at this time is 310 [kHz] in accordance with the liquid resonance frequency. The number of discharge holes of the droplet forming unit was 10,240 [pieces], and the opening diameter was 10 [μm].

The following collection conditions were used.
Gas type of air flow: Nitrogen gas Temperature of the first carrier air flow 41a, air flow rate: 25 [° C.], 20 [m ³ / hr]
Temperature and flow rate of the second carrier air flow 41b: 135 [° C.], 40 [m ³ / hr]
The height of the air flow distribution means 35: 5 [mm] from the discharge hole surface of the droplet formation means
Solid content concentration of toner composition liquid: 10 [mass%]
Solvent type of toner composition liquid: Ethyl acetate Latent heat of evaporation of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara, et al., P. 569)
Average particle diameter of manufactured toner: 5.4 [μm]
Specific gravity of toner: 1.2 [g / cm ³ ]
Droplet forming means: liquid column resonance type (see FIGS. 1 and 2)
Number of discharge holes of droplet forming unit: 10, 240 [pieces]
Frequency at discharge: 310 [kHz]
Distance from the carrier air flow inlet 64 to the carrier air flow outlet 65: 3,000 [mm]
The shape of the particle forming means 60 is a cyclone, and the inner diameter of the circular tube is 70 [mmφ], the aperture is 35 [mm], the height is 350 [mm], the outlet diameter is 30 [mmφ], the dust box shape 80 [mmφ] × It was set to 110 [mm].
Under the above conditions, dried particles were obtained leaving a solvent of 6% by mass. The temperature of the air flow was lowered due to the latent heat of evaporation of the solvent, and the temperature of the air flow at the carrier air flow outlet 65 one minute after the start of droplet discharge was 29 [° C.]. When the discharge was continued for one hour, the temperature of the air flow at the carrier air flow outlet 65 did not change at 29 [° C.]. The amount of collected particles at this point was 814 [g]. The collected toner was secondarily dried (40 ° C., left for 72 hours under air flow) to obtain toner particles of Example 1 from which the solvent was completely removed.

  The particle size distribution of the toner was measured with a flow type particle image analyzer (FPIA-3000, manufactured by Sysmex Corporation) under the measurement conditions shown below. Repeating this three times, the average of the volume average particle diameter (Dv) is 5.7 [μm], the average of the number average particle diameter (Dn) is 5.4 [μm], and the average of Dv / Dn is It was 1.05 and blockage of the nozzle was almost not observed. From the particle image, the ratio of the number of particles in which two or more particles are bound in a grape-like shape to the total measured particles was 0.8 [%].

The method of measuring the volume average particle diameter and number average particle diameter of toner using a flow particle image analyzer will be described below.
The measurement by a flow type particle image analyzer was measured using FPIA-3000 manufactured by Sysmex Corporation. In the measurement, fine dust is removed through a filter, and as a result, the number of particles in a measurement range (for example, circle equivalent diameter 0.60 [μm or more and less than 159.21 [μm]) in 10 ^-3 [cm ³ ] water. 10 mL or less of water were prepared. A few drops of a nonionic surfactant (preferably, Wako Pure Chemical Industries, Continon N) are added thereto, and 5 mg of the sample to be measured is further added thereto, and an ultrasonic disperser (UH-50, manufactured by STM) is added. The dispersion treatment was performed for 1 minute under the conditions of 20 [kHz] and 50 [W / 10 cm ³ ]. Furthermore, the dispersion treatment is carried out for a total of 5 minutes, and the particle concentration of the measurement sample is 4,000 [particles / 10 ⁻³ cm ³ ] to 8,000 [particles / 10 ⁻³ cm ³ ] (particles of measurement circle equivalent diameter range Sample dispersion was obtained. Using it, the particle size distribution of particles having a circle equivalent diameter of 0.60 [μm] or more and less than 159.21 [μm] was measured. The sample dispersion was passed through a flat, flat, transparent flow cell (having a thickness of about 200 μm) (which spreads along the flow direction). A strobe and a CCD camera are mounted on opposite sides of the flow cell to form an optical path that crosses and passes through the thickness of the flow cell. While the sample dispersion was flowing, strobe light was emitted at 1/30 second intervals to obtain an image of the particles flowing through the flow cell. As a result, each particle was photographed as a two-dimensional image having a certain range parallel to the flow cell. From the area of the two-dimensional image of each particle, the diameter of a circle having the same area was calculated as the equivalent circle diameter. The equivalent circle diameter of 1,200 or more particles can be measured in about one minute, and the number based on the equivalent circle diameter distribution and the percentage (number of particles) of particles having the defined equivalent circle diameter can be measured. The results (frequency% and cumulative%) can be obtained by dividing the range of 0.06 μm to 400 μm into 226 channels (divided into 30 channels for one octave).

(Example 2)
Next, another example of the particle manufacturing apparatus of the above embodiment (hereinafter, this example will be referred to as “example 2”) will be described.
In Example 2, fine particle production was carried out under the following conditions using the particle production apparatus of FIG. 7 to which one airflow supply means and one airflow distribution means were added with respect to FIG.
It is the same as Example 1.
The collection conditions are as follows.
Gas type of air stream: Nitrogen gas Temperature of the first carrier air stream 41a, air flow rate: 25 [° C], 15 [m ³ / hr]
Temperature and flow rate of the second carrier air stream 41b: 85 [° C.], 30 [m ³ / hr]
Temperature and flow rate of the third carrier air stream 41c: 40 [° C.], 15 [m ³ / hr]
The height of the first air flow distribution means 35a: 3.75 [mm] from the discharge hole surface of the droplet formation means
The height of the second air flow distribution means 35b: 3.75 [mm] from the wall surface facing the discharge hole surface of the droplet formation means
Solid content concentration of toner composition liquid: 10 [mass%]
Solvent type of toner composition liquid: Ethyl acetate Latent heat of evaporation of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara, et al., P. 569)
Average particle diameter of manufactured toner: 5.4 [μm]
Specific gravity of toner: 1.2 [g / cm ³ ]
Droplet forming means: liquid column resonance type (see FIGS. 1 and 2)
Number of discharge holes of droplet forming unit: 10, 240 [pieces]
Frequency at discharge: 310 [kHz]
Distance from the carrier air flow inlet 64 to the carrier air flow outlet 65: 3,000 [mm]

  The shape of the particle forming means 60 is a cyclone, and the inner diameter of the circular tube is 70 mm mm, the aperture is 35 mm, the height 350 mm, the outlet diameter is 30 mm diameter, and the dust box shape 80 mm diameter. × 110 [mm]. Under the above conditions, dried particles were obtained leaving a solvent of 6% by mass. The temperature of the air flow was lowered due to the latent heat of evaporation of the solvent, and the temperature of the air flow at the carrier air flow outlet 65 one minute after the start of droplet discharge was 29 [° C.]. When the discharge was continued for one hour, the temperature of the air flow at the carrier air flow outlet 65 did not change at 29 [° C.]. The amount of collected particles at this point was 860 [g], and blockage of the nozzle was hardly observed. The collected toner was secondarily dried (40 ° C., left for 72 hours under air flow) to obtain toner particles of Example 2 from which the solvent was completely removed. According to the particle image, the ratio of the number of particles in which two or more particles bound in a vine state to the total measured particles was 0.5 [%].

The inventors conducted earnest studies and found that when the environmental temperature at which the particle manufacturing apparatus is installed fluctuates, the particle size distribution of the collected particles is significantly broadened. The environmental temperature is relatively lowered, the temperature of the member forming the air flow passage is lowered, and the temperature of the second carrier air stream 41b of FIG. 6 flowing while contacting the inner wall surface of the member becomes lower than the target. The droplets discharged from the discharge holes are dried while being transported in the mixed transport air flow in which the first transport air flow 41a and the second transport air flow 41b shown in FIG. 6 are mixed. Therefore, when the temperature of the second carrier air stream 41b becomes lower than the target, the temperature of the mixed carrier air stream lowers than the target. As a result, it is considered that the drying of the droplets is insufficient and the particles are not sufficiently solidified, and the particles adhere to each other during transportation to become coarse particles.
Conversely, the environmental temperature rises, and the temperature of the second carrier air flow 41b becomes higher than the target. When the temperature of the second carrier air stream 41b becomes higher than the target, the temperature of the mixed carrier air stream also rises above the target. Since the dried particles are conveyed along the mixed conveying air stream, the temperature of the particles becomes substantially the same as the temperature of the mixed conveying air stream higher than the target, and becomes higher than the target. As a result, the particles become soft, and it is considered that the particles adhere to each other during transportation to become coarse particles. As described above, when the environmental temperature fluctuates, particles adhere to each other, and particles having a narrow particle size distribution can not be obtained.

Then, as a result of the inventors' earnestly examining, as shown in FIG. 7, in addition to the 1st conveyance air stream 41a and the 2nd conveyance air stream 41b, it flows, contacting with the inner wall surface of the member which forms an air channel. The carrier air flow 41 c is supplied to the air flow path. It has been found that by adjusting the temperature of the third carrier air stream 41c, particles having a narrow particle size distribution can be produced even when the environmental temperature fluctuates. Specifically, the heater provided in the third air flow supplying means 37 (in order to achieve the target temperature, the mixed conveyance air flow obtained by mixing the first conveyance air flow 41a, the second conveyance air flow 41b, and the third conveyance air flow 41c) The temperature of the third carrier air stream 41c is adjusted by adjusting the output temperature of FIG. By offsetting the fluctuation of the environmental temperature by the temperature adjustment, the mixed carrier air flow can be maintained at the target temperature. Thereby, the droplets can be sufficiently dried and solidified, and the solidified state of the particles can be maintained. Therefore, even if the environmental temperature fluctuates, adhesion of particles can be suppressed, and particles having a narrow particle size distribution can be stably obtained.
If the diameter of the discharge hole is increased and clogging of the discharge hole is eliminated even if the toner composition liquid is dried in the discharge hole, the first transfer air stream 41a does not flow in FIG. 41b is supplied to flow while contacting the discharge hole surface. The third carrier air stream 41c whose temperature can be adjusted according to the fluctuation of the environmental temperature is supplied so as to flow in contact with the inner wall surface of the member forming the air channel opposite to the discharge hole surface across the second carrier air stream 41b. It may be configured to

(Example 3)
Next, still another example of the particle manufacturing apparatus according to the above embodiment (hereinafter, this example will be referred to as “example 3”) will be described.
In Example 3, fine particle production was carried out using the apparatus shown in FIG. 6 under the following conditions. The difference from the first embodiment is the difference between the height of the air flow distribution means and the first transport air flow and the second transport air flow.

The following collection conditions were used.
Gas type of air stream: Nitrogen gas Temperature of the first carrier air stream 41 a, air flow rate: 25 [° C.], 4 [m ³ / hr]
Temperature and flow rate of the second carrier air flow 41b: 95 [° C.], 56 [m ³ / hr]
Height of air flow distribution means 35: 1 [mm] from the discharge hole surface of the droplet formation means
Solid content concentration of toner composition liquid: 10 [mass%]
Solvent type of toner composition liquid: Ethyl acetate Latent heat of evaporation of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara, et al., P. 569)
Average particle diameter of manufactured toner: 5.4 [μm]
Specific gravity of toner: 1.2 [g / cm ³ ]
Droplet forming means: liquid column resonance type (see FIGS. 1 and 2)
Number of discharge holes of droplet forming unit: 10, 240 [pieces]
Frequency at discharge: 310 [kHz]
Distance from the carrier air flow inlet 64 to the carrier air flow outlet 65: 3,000 [mm]

  The shape of the particle collection means is a cyclone, and the inner diameter of the circular tube is 70 mm mm, the aperture is 35 mm, the height is 350 mm, the outlet diameter is 30 mm diameter, and the dust box shape 80 mm diameter. × 110 [mm]. Under the above conditions, dried particles were obtained leaving a solvent of 6% by mass. The temperature of the air flow was lowered due to the latent heat of evaporation of the solvent, and the temperature of the air flow at the carrier air flow outlet 65 one minute after the start of droplet discharge was 29 [° C.]. When the discharge was continued for one hour, the temperature of the air flow at the transfer air flow outlet 65 was slightly increased at 32 ° C. The amount of collected particles at this point was 770 [g], and it was confirmed that the nozzle was slightly clogged. The collected toner was secondarily dried (40 ° C., left for 72 hours under air flow) to obtain toner particles of Example 3 from which the solvent was completely removed. According to the particle image, the ratio of the number of particles in which two or more particles bound in a vine state to the total measured particles was 1.5 [%].

(Example 4)
Next, still another example of the particle manufacturing apparatus according to the above embodiment (hereinafter, this example will be referred to as “example 4”) will be described.
In Example 4, fine particle production was carried out using the apparatus shown in FIG. 6 under the following conditions. The difference from the first embodiment is the difference between the height of the air flow distribution means and the first transport air flow and the second transport air flow.

The following collection conditions were used.
Gas type of air stream: Nitrogen gas Temperature of the first carrier air stream 41 a, air flow rate: 25 [° C.], 40 [m ³ / hr]
Temperature and flow rate of the second carrier air flow 41 b: 360 [° C.], 20 [m ³ / hr]
Height of air flow distribution means 35: 10 [mm] from the discharge hole surface of the droplet formation means
Solid content concentration of toner composition liquid: 10 [mass%]
Solvent type of toner composition liquid: Ethyl acetate Latent heat of evaporation of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara, et al., P. 569)
Average particle diameter of manufactured toner: 5.4 [μm]
Specific gravity of toner: 1.2 [g / cm ³ ]
Droplet forming means: liquid column resonance type (see FIGS. 1 and 2)
Number of discharge holes of droplet forming unit: 10, 240 [pieces]
Frequency at discharge: 310 [kHz]
Distance from the carrier air flow inlet 64 to the carrier air flow outlet 65: 3,000 [mm]

  The shape of the particle collection means is a cyclone, and the inner diameter of the circular tube is 70 mm mm, the aperture is 35 mm, the height is 350 mm, the outlet diameter is 30 mm diameter, and the dust box shape 80 mm diameter. × 110 [mm]. Under the above conditions, dried particles were obtained leaving a solvent of 6% by mass. The temperature of the air flow was lowered due to the latent heat of evaporation of the solvent, and the temperature of the air flow at the carrier air flow outlet 65 one minute after the start of droplet discharge was 28 [° C.]. When the discharge was continued for one hour, the temperature of the air flow at the transfer air flow outlet 65 did not change at 28 [° C.]. The amount of collected particles at this point was 860 [g], and no blockage of the nozzle was observed. The collected toner was secondarily dried (40 ° C., left for 72 hours under air flow) to obtain toner particles of Example 3 from which the solvent was completely removed. According to the particle image, the ratio of the number of particles in which two or more particles bound in a vine state to the total measured particles was 0.5 [%].

  Although liquid droplet discharge means of liquid column resonance type is mentioned as a droplet discharge device in the above-mentioned Examples 1-4, droplet discharge means of film vibration type, Rayleigh division type, etc. are mentioned as others. In the fifth embodiment described below, Rayleigh split type droplet discharge means is used as the droplet discharge device.

(Example 5)
Next, still another example of the particle manufacturing apparatus according to the above-described embodiment (hereinafter, this example will be referred to as “example 5”) will be described. In Example 5, particle production was carried out under the following conditions using the particle production apparatus of FIG. 6 and the above-mentioned Rayleigh split type droplet discharge means as the droplet formation means. The difference from the first embodiment is the difference between the droplet forming means and the second carrier air flow.

Here, the droplet formation phenomenon of the liquid column in the droplet discharge means of the Rayleigh split type will be described with reference to FIG.
As described in Non-Patent Document 1, the uniform droplet formation phenomenon of the liquid column is the wavelength condition λ at which the liquid column becomes most unstable by using the liquid column diameter d (jet) by the following equation (6) expressed.
λ = 4.5 d (jet) formula (6)
Here, the frequency f of the generated disturbance phenomenon can be expressed by the following equation (7) when the velocity of the liquid column is v.
f = v / λ (7)
Further, as described in Non-Patent Document 2, as a result of experimentally deriving conditions for stably forming uniform particles, it is possible to stably form uniform particles under the condition of the following formula (8) It is supposed to be.
3.5 <λ / d (jet) <7.0 ··· Formula (8)
Furthermore, as described in Non-Patent Document 3, the minimum jet V (min) velocity at which the liquid discharged from the discharge hole forms a liquid column based on the energy conservation law is expressed by the following equation (9) It is expressed as
v (min) = (8σ / d d (jet)) (1/2) formula (9)
In equation (9), σ represents the surface tension of the liquid, ρ represents the liquid density, and d (jet) represents the diameter of the liquid column. The conditional expressions of Equations (6) to (9) are useful for estimating the conditions for reproducing such a phenomenon. It has been confirmed that these relational expressions can vary depending on the type of liquid substance, mixture, dispersion and the like. By attaching a vibrator to the liquid chamber and vibrating it at the frequency f, the phenomenon that the liquid column is formed into droplets by the disturbance as described above is established in various liquids.

  The liquid storage portion must be at least held in a pressurized state of the toner composition liquid, and thus is made of a member such as a metal such as SUS or aluminum, and has a pressure resistance of at least about 1 [Mpa]. Although desirable, it is not limited to this. For example, as shown in FIG. 14 described later, it is desirable to have a structure in which a plate material is connected by a pipe for supplying the liquid to the liquid storage portion and which constitutes a part of the liquid storage portion. Further, vibration generating means for vibrating the entire liquid storage portion is in contact with the liquid storage portion. It is desirable that the vibration generating means be connected to the drive device by a conductive wire, and the vibration state be controlled by the drive device.

The vibration generating means preferably excites the entire liquid reservoir having the discharge hole. The vibration generating means is not particularly limited as long as it can give reliable vibration at a constant frequency, and can be appropriately selected and used, and examples include a piezoelectric body, an ultrasonic vibration generating portion, and the like. There is no restriction | limiting in particular as a piezoelectric material, According to the objective, it can select suitably, for example, piezoelectric ceramics, such as lead zirconate titanate (PZT), piezoelectric polymers, such as polyvinylidene fluoride (PVDF), quartz, Examples include piezoelectrics formed of materials such as single crystals of LiNbO ₃ , LiTaO ₃ , KNbO _{3 and the} like. There is no restriction | limiting in particular as an ultrasonic vibration generation part, According to the objective, it can select suitably, For example, a magnetostriction element etc. are mentioned. The constant frequency is not particularly limited and may be appropriately selected according to the purpose. However, 100 [kHz] to 500 [kHz] is preferable, and from the viewpoint of generating microdroplets having a uniform particle diameter, 200 [kHz]-400 [kHz] are more preferred.

  The vibration generating means is in contact with the liquid storage portion, and it is most preferable that the plate members having the discharge holes are arranged in parallel from the viewpoint of uniformly giving vibration to the liquid column generated from the discharge holes. Any form may be used as long as the liquid droplet narrowing as shown in FIG. Although it is possible to produce particles even if only one discharge hole is provided, it is preferable to provide a plurality of discharge holes from the viewpoint of efficiently generating microdroplets having a very uniform particle diameter. Further, it is preferable to use one as shown in FIG. 3 as the opening cross-sectional shape of the discharge hole.

  As shown in FIG. 14, the droplet forming unit 100 as the droplet forming unit includes at least a liquid storage portion 101 for storing a toner composition liquid, a vibration generating unit 102, and a toner composition discharged from a plurality of discharge holes 103. In order to supply the liquid quantitatively to the liquid storage portion 101, the liquid storage portion 101 is provided with a pipe 104 connected in communication with the liquid storage portion 101. The liquid chamber size of the liquid storage unit 101 is 60 mm in width, 5 mm in depth, and 5 mm in height, and the liquid storage unit 101 has a columnar shape (disk shape of 15 mmφ × 3 mm). ), And PZT (Fuji Ceramics Co., Ltd.) provided with electrodes on a circular plane with silver paste was fixed with an adhesive. As a drive signal generation source (not shown), a function generator (WF1973, manufactured by NF Circuit Design Block Co., Ltd.) was used, and it was connected to the electrodes of the vibration generation means 102 by a lead wire coated with polyethylene. The driving frequency at this time was 300 [kHz]. The number of the discharge holes 103 of the droplet forming unit 100 is 1000 and the discharge hole diameter is 8.0 μm. The solution was pressurized to be maintained at 400 [kPa] using a syringe pump.

The following collection conditions were used.
Gas type of air flow: Nitrogen gas Temperature of the first carrier air flow 41a, air flow rate: 25 [° C.], 20 [m ³ / hr]
Temperature and flow rate of the second carrier air stream 41b: 60 [° C.], 40 [m ³ / hr]
The height of the air flow distribution means 35: 5 [mm] from the discharge hole surface of the droplet formation means
Solid content concentration of toner composition liquid: 5 [mass%]
Solvent type of toner composition liquid: Ethyl acetate Latent heat of evaporation of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara, et al., P. 569)
Average particle size of manufactured toner: 6.3 [μm]
Specific gravity of toner: 1.2 [g / cm ³ ]
Droplet forming means: Rayleigh split type (see FIGS. 13 and 14)
Number of discharge holes 103 of the droplet forming unit 100: 1,000 [pieces]
Frequency at dispensing: 300 [kHz]

  Under the above conditions, dried particles were obtained leaving a solvent of 6.2% by mass. The temperature of the air flow decreased due to the latent heat of evaporation of the solvent, and the temperature of the air flow at the carrier air flow outlet 65 one minute after the start of droplet discharge was 31 [° C.]. When the discharge was continued for one hour, the temperature of the air flow at the transfer air flow outlet 65 did not change at 31 [° C.]. The amount of collected particles at this point was 130 [g], and no blockage of the nozzle was observed. The collected toner was secondarily dried (40 ° C., left for 72 hours under air flow) to obtain toner particles of Example 5 from which the solvent was completely removed. From the particle image, the ratio of the number of particles in which two or more particles were bound in a vine like to the total measured particles was 1.0 [%].

(Comparative example 1)
Next, a comparative example (hereinafter, this comparative example is referred to as “comparative example 1”) with respect to the particle manufacturing apparatus of the above embodiment will be described.
In Comparative Example 1, using the apparatus shown in FIG. 6, only the first air flow supply means 31 is used, and the height of the air flow distribution means 35 is 15 mm, that is, only the first transport air flow 41a flows in the entire height. did. The experiment was performed in the same manner as in Example 1 except that the temperature and the air volume of the first carrier air stream 41a were set to 82 [° C.] and 60 [m ³ / hr]. The total amount of the first carrier air flow 41a and the air flow temperature at this time are the same as those of the first carrier air flow 41a and the second carrier air flow 42a in the first embodiment.

  Under the above conditions, dried particles were obtained leaving a solvent of 6% by mass. The temperature of the air flow was lowered due to the latent heat of evaporation of the solvent, and the temperature of the air flow at the carrier air flow outlet 65 one minute after the start of droplet discharge became 29 [° C.]. After discharging for 1 hour, the temperature of the air flow at the transport air flow outlet 65 had increased to 48 [° C.]. The collected amount of particles at this point was 407 [g], and about half of the nozzles were visually blocked. The average volume average particle diameter (Dv) of the obtained toner is 7.3 [μm], the average number average particle diameter (Dn) is 5.8 [μm], and the average Dv / Dn is 1.25 Met. The toner was fixed in a semi-molten state to the cyclone. It is considered that this is because the temperature of the air flow is increased and the toner is easily fixed because the droplet discharge is lowered. The ratio of the number of particles in which two or more particles are bound like a grape to the total measured particles is 23.4 [%] because toners are easily fixed to each other, and Example 1 and Example 2 It was significantly worse than.

  From the above results, in Examples 1 to 5, the droplet discharge is more stable, the temperature of the carrier air flow is not changed, and the droplets can be dried and collected more stably than in Comparative Example 1. It has been confirmed that it is possible to prevent cohesion between particles and to produce particles having a narrow particle size distribution.

What has been described above is an example, and the present invention has unique effects in each of the following modes.
(Aspect A)
Droplet formation which forms a droplet 21 by discharging a resin composition liquid 14 containing a resin and a solvent from the discharge hole 19 into the air flow passage. Means 11, an air flow supplying means for supplying a high temperature carrier air flow 41 into the air flow path so as to flow in a direction parallel to the surface direction of the discharge hole surface, and particles which are dried and solidified in the high temperature carrier air flow In the particle manufacturing apparatus 1 including the particle collection means 70, the air flow supply means 30 sandwiches the first carrier air flow 41a supplied so as to flow while contacting the discharge hole surface, and the first carrier air flow 41a. The second carrier air flow 41 b having a temperature higher than that of the first carrier air flow 41 a supplied so as to flow on the side opposite to the discharge hole surface is supplied into the air flow path.
According to this, as described in the above embodiment, the discharge is performed by bringing the first transfer air flow 41 a at a temperature lower than the temperature of the second transfer air flow 41 b and at which clogging of the discharge hole 19 does not occur. The drying of the resin composition liquid 14 is suppressed at the holes. As a result, clogging of the discharge holes 19 can be suppressed, and the number of the discharged discharge holes 19 can be reduced. Further, the temperature of the second carrier air flow 41b is a temperature at which the droplets 21 can be sufficiently dried and solidified, but the second carrier air flow 41b flows on the opposite side to the ejection hole surface across the first carrier air flow 41a. Because it does not contact the discharge hole surface. For this reason, the resin composition liquid 14 is not dried in the discharge holes, and the amount of latent heat of vaporization when particles are formed can maintain the target value. The temperature of the carrier air flow becomes the target temperature, and the particles can be solidified without being attached to one another to form particles of the target particle diameter. As a result, it is possible to produce particles having a narrow particle size distribution while suppressing the temperature rise of the discharge hole surface in contact with the carrier air flow.

(Aspect B)
In (Aspect A), the air flow supply means 30 inserts the third carrier air flow 41c flowing in contact with the inner wall surface of the member forming the air flow path on the opposite side to the discharge hole surface across the air flow path. The third carrier air flow 41c is supplied at a lower temperature than the second carrier air flow 41b.
According to this, as described in the above embodiment, for example, when the environmental temperature fluctuates, if the temperature of the third carrier air stream 41c is adjusted, the fluctuation of the environmental temperature can be offset by the temperature adjustment. For this reason, it is possible to maintain a mixed transport airflow in which the plurality of transport airflows of the first transport airflow 41a, the second transport airflow 41b, and the third transport airflow 41c are mixed at a target temperature. As a result, the droplets can be sufficiently dried, and adhesion of particles can be suppressed. Thus, particles having a narrow particle size distribution can be produced.

(Aspect C)
In (Aspect A) or (Aspect B), the air flow straightening means 36 or the like which arranges a plurality of conveyance air currents on the upstream side of the discharge hole with respect to the flow direction of the high temperature carrier air flow 41 Providing rectifying means. According to this, as described in the above embodiment, the plurality of transport airflows of the first transport airflow 41a, the second transport airflow 41b, and the third transport airflow 41c flow while maintaining the airflow parallel to each other. It can suppress that conveyance air flow mixes. As a result, the temperature of the first carrier air stream 41a can be maintained at the target temperature, the temperature rise on the discharge hole surface can be suppressed, and the clogging of the discharge holes can be suppressed.

(Aspect D)
In (Aspect A) to (Aspect C), the temperature of the first carrier air stream 41a is equal to or less than the boiling point of the solvent. According to this, as described in the above embodiment, the clogging of the discharge hole due to the boiling of the solvent can be suppressed.

(Aspect E)
In (Aspects A) to (Aspect D), the temperature of the first carrier air stream 41a is lower than the boiling point of the solvent by 20 [° C.] or more. According to this, as described in the above embodiment, the clogging of the discharge hole due to the boiling of the solvent can be suppressed.

(Aspect F)
Droplet formation which forms a droplet 21 by discharging a resin composition liquid 14 containing a resin and a solvent from the discharge hole 19 into the air flow passage. Means 11, an air flow supplying means for supplying a high temperature carrier air flow 41 into the air flow path so as to flow in a direction parallel to the surface direction of the discharge hole surface, and particles which are dried and solidified in the high temperature carrier air flow In the particle manufacturing apparatus 1 including the particle collection means 70, the air flow supply means 30 flows while being in contact with the inner wall surface of the member forming the air flow path on the opposite side to the discharge hole surface across the air flow path. And a second transport air stream having a temperature higher than that of the first transport air stream supplied so as to flow on the opposite side to the inner wall surface sandwiching the first transport air stream into the air flow path.
According to this, as described in the above embodiment, when the environmental temperature fluctuates, it flows while contacting the inner wall surface separately from the high temperature second carrier air flow according to the fluctuation of the environmental temperature. By adjusting the temperature of the supplied first carrier air stream, it is possible to offset the fluctuation of the environmental temperature by the temperature adjustment. Therefore, the mixed conveyance airflow which the 1st conveyance airflow and the 2nd conveyance airflow mixed can be maintained at the target temperature. Thereby, the droplets can be sufficiently dried, adhesion of particles can be suppressed, and particles having a narrow particle size distribution can be produced.

(Aspect G)
In (Aspect A) to (Aspect F), the droplet forming means applies vibration to the resin composition liquid in the liquid column resonance chamber in which a plurality of discharge holes are formed to form a pressure standing wave by liquid column resonance. The resin composition liquid is discharged from a plurality of discharge holes formed in the region which becomes the antinode of the pressure standing wave to form a droplet. According to this, as described in the above embodiment, by disposing the discharge holes in the area of the antinode where the pressure of the pressure standing wave fluctuates most, the discharge efficiency becomes high, and the particles can be efficiently manufactured. it can. A particle having a narrow particle size distribution can be manufactured by continuously discharging a plurality of droplets having substantially the same liquid amount from the discharge hole in accordance with the cycle of the pressure standing wave.

(Aspect H)
In (Aspects A) to (Aspect F), the droplet formation means pressurizes the resin composition liquid in the liquid reservoir while applying vibration to the liquid reservoir having the plurality of discharge holes and the vibration means by the vibrator. The resin composition liquid discharged from the plurality of discharge holes forms a droplet from a columnar through a narrowing state. According to this, as described in the above embodiment, by vibrating the liquid storage portion at a high vibration frequency, the number of droplets formed from the discharge holes can be relatively increased, and the discharge holes are unlikely to be blocked. Therefore, droplets of uniform droplet diameter can be obtained, and sufficient productivity can be obtained.

(Aspect I)
A resin composition liquid 14 having a plurality of discharge holes 19 on a flat surface and containing a resin and a solvent is discharged from the discharge holes 19 into the air flow path to form droplets 21 and is parallel to the surface direction of the discharge hole surface. In the particle manufacturing method, the high temperature carrier air flow 41 is supplied into the air flow path so as to flow in any direction, dried and solidified in the high temperature carrier air flow, to form particles and collect the particles. The first carrier air flow 41a supplied so as to flow while contacting, and the second carrier air flow 41b having a temperature higher than that of the first carrier air flow 41a supplied so as to flow on the opposite side to the discharge hole surface across the first carrier air flow 41a. And into the air flow path.
According to this, as described in the above embodiment, the discharge is performed by bringing the first transfer air flow 41 a at a temperature lower than the temperature of the second transfer air flow 41 b and at which clogging of the discharge hole 19 does not occur. The drying of the resin composition liquid 14 is suppressed at the holes. As a result, clogging of the discharge holes 19 can be suppressed, and the number of the discharged discharge holes 19 can be reduced. Further, the temperature of the second carrier air flow 41b is a temperature at which the droplets 21 can be sufficiently dried and solidified, but the second carrier air flow 41b flows on the opposite side to the ejection hole surface across the first carrier air flow 41a. Because it does not contact the discharge hole surface. For this reason, the resin composition liquid 14 is not dried in the discharge holes, and the amount of latent heat of vaporization when particles are formed can maintain the target value. The temperature of the carrier air flow becomes the target temperature, and the particles can be solidified without being attached to one another to form particles of the target particle diameter. As a result, it is possible to produce particles having a narrow particle size distribution while suppressing the temperature rise of the discharge hole surface in contact with the carrier air flow.

(Aspect J)
A resin composition liquid 14 having a plurality of discharge holes 19 on a flat surface and containing a resin and a solvent is discharged from the discharge holes 19 into the air flow path to form droplets 21 and is parallel to the surface direction of the discharge hole surface. In the particle manufacturing method, the high temperature carrier air flow 41 is supplied into the air flow channel so as to flow in any direction, and dried and solidified in the high temperature carrier air flow to form particles and collect the particles. The first carrier air stream supplied so as to flow while contacting the inner wall surface of the member forming the air flow path on the opposite side of the discharge hole surface and the inner wall surface opposite to the inner wall surface sandwiching the first carrier air stream A second carrier air stream having a temperature higher than the supplied first carrier air stream is supplied into the air flow path.
According to this, as described in the above embodiment, when the environmental temperature fluctuates, it flows while contacting the inner wall surface separately from the high temperature second carrier air flow according to the fluctuation of the environmental temperature. By adjusting the temperature of the supplied first carrier air stream, it is possible to offset the fluctuation of the environmental temperature by the temperature adjustment. Therefore, the mixed conveyance airflow which the 1st conveyance airflow and the 2nd conveyance airflow mixed can be maintained at the target temperature. Thereby, the droplets can be sufficiently dried, adhesion of particles can be suppressed, and particles having a narrow particle size distribution can be produced.

DESCRIPTION OF SYMBOLS 1 particle manufacturing apparatus 11 droplet forming means 14 resin composition liquid 17 common solution supply channel 18 liquid column resonance liquid chamber 19 discharge hole 20 vibration generating means 21 droplet 22 diaphragm 30 air flow supplying means 31 first air flow supplying means 32 second The air flow supply means 33 The first air flow path 34 The second air flow path 35 The air flow distribution means 36 The air flow rectification means 37 The third air flow supply means 38 The third air flow path 41 The transport air stream 41a The first transport air stream 41b The second transport air stream 41c The third transport air stream DESCRIPTION OF SYMBOLS 60 particle formation means 61 chamber 64 conveyance air flow inlet 65 conveyance air flow outlet 70 particle collection means 71 particle collection part 72 particle storage part 100 droplet formation unit 101 liquid storage part 102 vibration generation means 103 discharge hole 104 piping

Patent No. 3786034 gazette Patent No. 3786035 gazette Japanese Patent Application Laid-Open No. 57-201248 JP, 2006-293320, A JP, 2013-047767, A JP, 2013-063406, A

Rayleigh, Lord "On the Instability of Jets" Proc. London Math. Soc. 110: 4 [1878] Schneider J. M., C. D. Hendricks, Rev. Instrum. 35 (10), 1349-50 [1964] Lindblad N. R. and J. M. Schneider, J. Sci. Instrum. 42, 635 [1965]

Claims (6)

Droplet forming means having a gas flow path forming means, a plurality of discharge holes on a flat surface, and discharging a resin composition liquid containing a resin and a solvent from the discharge holes into the gas flow path to form droplets; Air flow supply means for supplying a high temperature carrier air flow into the air flow passage so as to flow in a direction parallel to the surface direction of the hole surface, and collection means for collecting particles solidified by drying in the high temperature carrier air flow In a particle manufacturing apparatus comprising
The air flow supply means supplies a first carrier air flow supplied to flow while contacting the discharge hole surface, and a first supply air supplied so as to flow on the opposite side to the discharge hole surface across the first carrier air flow. It contacts the inner wall surface of the member forming the air flow path on the opposite side of the discharge hole surface, sandwiching both the second transfer air flow having a temperature higher than the transfer air flow, the first transfer air flow and the second transfer air flow. Supplying a third carrier air stream having a temperature lower than that of the second carrier air stream so as to flow while flowing into the air channel;
Temperature of the third conveying airflow Ri adjustable der in accordance with variations in ambient temperature,
Honeycomb having a hole diameter of 0.1 [mm] to 10 [mm] for arranging a plurality of carrier air flows on the upstream side of the discharge hole with respect to the flow direction of the high temperature carrier air flow so as to be a gas flow parallel to the discharge hole surface. particle production apparatus according to claim Rukoto provided rectifying means in the form. In the apparatus for producing particles according to 請 Motomeko 1,
The temperature of the said 1st conveyance airflow is below the boiling point of the said solvent, The particle manufacturing apparatus characterized by the above-mentioned. In the particle manufacturing apparatus according to claim 1 or 2 ,
The temperature of the said 1st conveyance airflow is 20 [degreeC] or more lower than the boiling point of the said solvent, The particle manufacturing apparatus characterized by the above-mentioned. In the particle manufacturing apparatus according to any one of claims 1 to 3 ,
The droplet forming means applies vibration to the resin composition liquid in the liquid column resonance chamber in which a plurality of discharge holes are formed to form a pressure standing wave by liquid column resonance, and the antinode of the pressure standing wave A particle manufacturing apparatus characterized in that the resin composition liquid is discharged from the plurality of discharge holes formed in the region to form droplets. In the particle manufacturing apparatus according to any one of claims 1 to 4 ,
The droplet formation means applies pressure to the resin composition liquid in the liquid storage portion while applying vibration to the liquid storage portion having a plurality of discharge holes and vibration means by the vibration means, and discharges the liquid from the plurality of discharge holes. What is claimed is: 1. A particle manufacturing apparatus characterized in that a resin composition liquid forms droplets from a columnar through a constricted state. A resin composition liquid containing a resin and a solvent is discharged into the air flow path from a plurality of discharge holes on a flat surface, and the discharge holes form droplets, which flow in a direction parallel to the surface direction of the discharge hole surface. In the particle manufacturing method, a high temperature carrier air flow is supplied into the air flow path, dried and solidified in the high temperature carrier air flow, to form particles, and collecting the particles,
A first carrier air flow supplied so as to flow while contacting the discharge hole surface, and a temperature higher than the first carrier air flow supplied so as to flow on the opposite side to the discharge hole surface across the first carrier air flow 2) Supply so as to flow while contacting with the inner wall surface of the member forming the air flow path on the opposite side of the discharge hole surface sandwiching both the transfer air flow, the first transfer air flow and the second transfer air flow Supplying a third carrier air stream having a temperature lower than that of the second carrier air stream into the air channel;
Temperature of the third conveying airflow Ri adjustable der in accordance with variations in ambient temperature,
It becomes an air flow parallel to the discharge hole surface by the honeycomb-shaped flow straightening means having a hole diameter of 0.1 [mm] to 10 [mm] provided on the upstream side of the discharge hole with respect to the flow direction of the high temperature carrier flow. A method of producing particles, comprising preparing a plurality of transport air flows .