JP2015186793A - particle manufacturing apparatus and particle manufacturing method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a particle manufacturing apparatus capable of manufacturing particles having a narrow particle size distribution while suppressing a temperature rise of discharge hole surfaces brought into contact with transportation air flows, and further to provide a particle manufacturing method.SOLUTION: A particle manufacturing apparatus comprises: air flow passage formation means; droplet formation means 11 having a plurality of discharge holes 19 on a flat surface, discharging resin composition liquid 14 containing resin and solvent into air flow passages through the plurality of discharge holes 19 and forming droplets 21; air flow supply means supplying transportation air flows 41 having a high temperature into the air flow passages such that the air flows 41 flow in a direction parallel with a surface direction of discharge hole surfaces; and particle collection means 70 collecting particles dried and solidified in the transportation air flows having the high temperature. The air flow supply means supplies first transportation air flows supplied such that the first transportation air flows flow while being brought into contact with the discharge hole surfaces and second transportation air flows being supplied such that the second transportation air flows flow at opposite sides to the discharge hole surfaces with the first transportation air flows interposed thereamong and having a higher temperature than that of the first transportation air flows into the air flow passages.

Description

  The present invention relates to a particle manufacturing apparatus such as a toner manufacturing apparatus including a droplet discharge device that discharges liquid from discharge holes into droplets, and a particle manufacturing method.

  As a method for producing toner for developing an electrostatic image used in image forming apparatuses such as copying machines, printers, facsimiles, and composite machines based on the electrophotographic recording method, a pulverization method has been mainly used. In recent years, a polymerization method is increasingly employed. The polymerization method is a method of forming toner particles in an aqueous medium, and is referred to as such because it involves a polymerization reaction of the toner raw material at the time of toner particle formation or in the process. Various polymerization methods have been put into practical use, and those utilizing suspension polymerization, emulsion aggregation, polymer suspension (polymer aggregation), ester elongation reaction, and the like are known. The toner manufactured by the polymerization method is called a polymerization toner or a chemical toner.

  The toner obtained by the polymerization method generally has the characteristics that it is easy to obtain a small particle size, the particle size distribution is narrow, and the shape is almost spherical compared to the toner obtained by the pulverization method. These characteristics bring about an effect that it is easy to obtain high image quality as an image formed by an electrophotographic method. However, it takes a long time for the polymerization process, and further, it is necessary to separate the solvent and toner particles after completion of solidification, and then repeat washing and drying, which requires a lot of time, a lot of water and a lot of energy. There is a problem.

  Also, a liquid (toner component liquid) in which the raw material components of the toner are dissolved or dispersed in an organic solvent is discharged into fine droplets using a sprayer (atomizer), etc., and dried to form a fine particle toner A toner production method called a jet granulation method is known (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.

  In the case of producing fine particles such as toner by the jet granulation method, fine particle-containing liquids such as toner component liquids (raw raw material components of fine particles are used as solvents from a plurality of discharge holes opened on the discharge hole surface of the droplet discharge device by the droplet forming means. The discharging operation for discharging the liquid droplets of the liquid dissolved or dispersed in the liquid crystal is continued. Particles are produced by solidifying the droplets discharged by the solidifying means.

  For example, in the particle manufacturing apparatuses of Patent Documents 5 and 6, vibration generating means for applying vibration to the liquid is provided in the liquid chamber, and the standing wave by liquid column resonance is applied to the liquid in the liquid chamber by applying vibration to the liquid in the liquid chamber. Form. Liquid is discharged from the discharge hole formed in the region where the antinode of the standing wave flows into the air flow path where the high-temperature carrier airflow flows, and the liquid droplets are dried and solidified in the carrier airflow. To do. Particles are produced by collecting the solidified particles by the collecting means.

  However, in the fine particle manufacturing apparatuses of Patent Documents 5 and 6, the discharge holes are exposed to a high-temperature carrier airflow. For this reason, there is a risk that the fine particle-containing liquid dries in the discharge holes and the discharge holes are clogged, resulting in a discharge failure, making it difficult to secure a target production amount. When the number of clogged discharge holes increases with time and the discharge amount of droplets decreases, the amount of latent heat of vaporization when particles are formed also decreases, and the decrease in the temperature of the conveying airflow decreases. Since the dried particles are transported along the transport airflow, the temperature of the particles is almost the same as the temperature of the transport airflow, and the temperature of the dried particles is higher than intended. As a result, the particles become soft, the particles adhere to each other, and there is a problem that particles having a narrow particle size distribution cannot be obtained.

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

  In order to achieve the above object, the invention of claim 1 includes 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 is discharged from the discharge holes into the air flow path. A droplet forming means for forming a droplet by discharging the liquid, a gas flow supplying means for supplying a 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 the high-temperature carrier In a particle production apparatus comprising a collection means for collecting particles dried and solidified in an air flow, the air flow supply means supplies a first conveying air flow to flow while in contact with the discharge hole surface; A second carrier airflow having a temperature higher than that of the first carrier airflow supplied so as to flow on the side opposite to the discharge hole surface across the first carrier airflow is supplied into the air flow path. is there.

  According to the present invention, it is possible to obtain a specific effect that particles having a narrow particle size distribution can be manufactured while suppressing an increase in the temperature of the discharge hole surface that the carrier airflow contacts.

It is the schematic diagram which expanded and showed a part of droplet formation means of the liquid column resonance type droplet discharge apparatus used by this embodiment. It is sectional drawing which showed typically a part of liquid column resonance droplet formation unit which is the droplet discharge device. 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 and pressure fluctuation | variation in case of N = 1,2,3. (A)-(e) is a schematic diagram explaining the state 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 of the state which the basic particle bound. It is the schematic which shows the mode of the coalesced particle. It is the schematic which shows the mode of the coalesced particle. FIG. 6 is a diagram illustrating a particle size distribution of toner collected when the adhesion between droplets occurs. FIG. 6 is a diagram illustrating a particle size distribution of toner collected when adhesion between droplets does not occur. It is a figure explaining the droplet formation phenomenon of a Rayleigh division type liquid column. It is the schematic diagram which expanded and showed a part of droplet discharge part of the Rayleigh division type droplet discharge device.

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

  The droplet discharge device of the present embodiment preferably has a narrow particle size distribution of discharged droplets, but there is no particular limitation and a known one can be used. As a droplet discharge device, there are 1 fluid nozzle, 2 fluid nozzle, membrane vibration type droplet discharge means, Rayleigh split type droplet discharge means, liquid vibration type droplet discharge means, liquid column resonance type droplet discharge Means etc. are mentioned. An example of the membrane vibration type droplet discharge means is disclosed in Japanese Patent Application Laid-Open No. 2008-292976. Further, as a Rayleigh splitting 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 ensure the productivity of the toner with a narrow droplet size distribution, vibration is imparted to the liquid in the liquid column resonance liquid chamber in which a plurality of ejection holes are formed to form a standing wave by liquid column resonance. To do. A liquid column resonance type liquid droplet ejection device that ejects liquid from the ejection holes formed in the region that becomes the antinode of the standing wave is suitable. In the present embodiment, an example in which toner is manufactured using a liquid column resonance type droplet discharge device will be described.

  The particle production apparatus of the present invention includes at least an air flow path forming unit, a droplet forming unit, an air flow supplying unit, and a collecting unit, and further includes other units as necessary. The particle production method of the present invention includes at least an air channel 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 preferably carried out by a particle production apparatus, the air channel forming step can be suitably carried out by an air channel forming unit, the droplet forming step can be suitably carried out by a droplet forming unit, and the air flow supplying step is The air flow supplying means can be preferably implemented, 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 particle production 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 removed in the carrier air stream. Collect the particles obtained by volatilization.

  When the discharged droplets are released into the carrier airflow, the droplet temperature once reaches the wet bulb temperature due to the relationship between the vapor pressure around the droplet and the temperature, but the amount of solvent in the droplet is small. As a result, the temperature of the droplet rises to the temperature of the carrier airflow. For this reason, the temperature of the particles obtained by drying the droplets is almost the same as the temperature of the airflow.

  When the solvent evaporates from the droplets in the transport airflow, the temperature of the transport airflow decreases because latent heat of vaporization is removed from the transport airflow. That is, it is necessary to set the temperature of the airflow in advance in anticipation of the temperature taken away by the latent heat of vaporization. When the discharge amount of the resin composition liquid varies, the amount of latent heat of vaporization when the particles are formed changes, so that the temperature of the conveying air flow varies depending on the discharge amount of the resin composition liquid. For this reason, when the discharge hole is clogged and the discharge amount of the resin composition liquid is reduced, the decrease in the temperature of the conveying airflow is reduced. And since the temperature of the particle | grains dried in the particle | grain formation process becomes substantially the same as the temperature of a conveyance airflow, if the discharge amount of a resin composition liquid reduces, the temperature of the dried particle | grain will become high.

  Then, when the dried particles are collected, the particles adhere to each other and particles having a narrow particle size distribution cannot be obtained. Some particles to be produced have a low softening temperature, but the tendency is remarkable for particles having a low softening temperature. For example, toner tends to be designed at a low softening temperature to reduce power consumption during operation of the electrophotographic system. When the particles are collected in a state where the temperature of the particles is higher than the softening temperature of the particles, the particles are solidified in a state where the particles adhere to each other, and even if particles having a particle size distribution close to monodispersion can be generated immediately before collection. In this case, the particle size distribution is greatly broadened in the collecting part. The cause of the deterioration of the particle size distribution is caused by the instability of the droplet forming means, and by improving this, not only the productivity is improved, but the particles are always in a stable dry state, The quality can be stabilized.

  Therefore, the present inventors have intensively studied. As a result, the particle manufacturing apparatus has a plurality of discharge holes on at least a plane, and discharges a resin composition liquid containing a resin and a solvent from the discharge holes to form liquid droplets, and an air flow 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 is suppressed, the clogging due to the drying of the nozzle is suppressed, the droplet discharge amount can be greatly improved, and the particle collection can be performed stably. It has been found that particles having a narrow particle size distribution can be produced over a long period of time by preventing coalescence.

  Any droplet forming means may be used as long as it has a plurality of discharge holes on a plane and discharges a resin composition liquid containing a resin and a solvent from the discharge holes to form droplets having a uniform particle diameter. There is no particular limitation, and it can be appropriately selected according to the purpose, and examples thereof include a membrane vibration type, a Rayleigh splitting type, a liquid vibration type, and a liquid column resonance type. Examples of the membrane vibration type include those described in JP-A-2008-292976. Examples of the Rayleigh split type include those described in Japanese Patent No. 4647506. Examples of the liquid vibration type include those described in JP2010-102195A. Among these, the droplet forming means is preferably a liquid column resonance type in that the particle size distribution of the droplets is narrow and the productivity of the particles can be secured.

  The droplet forming step is not particularly limited as long as it is a step for 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 is appropriately selected according to the purpose. However, it is preferably performed by a 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 the pressure standing It is means for discharging the resin composition liquid from at least one discharge hole disposed in the region where the wave is located to form droplets.

  The liquid column resonance type droplet forming means has a liquid column resonance liquid chamber having at least one ejection hole, and a vibration generating unit for applying vibration to the resin composition liquid in the liquid column resonance liquid chamber. By doing so, it is preferable that a plurality of nozzle holes be arranged on a plane. The vibration generating unit imparts 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 from the discharge hole formed in the antinode of 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 of the pressure wave of the liquid column resonance standing wave is large and the pressure fluctuation is large, and the pressure is large enough to discharge a droplet. This is a region having variation. There is no particular limitation on the region that becomes the antinode of such a pressure standing wave, and it can be appropriately selected according to the purpose. However, the position where the amplitude of the pressure standing wave becomes a maximum (as a velocity standing wave) ± 1/3 wavelength is preferable from the node) toward the minimum position, and ± 1/4 wavelength is more preferable. It is preferable that the discharge holes are formed in a region where the antistatic wave is antinode, because even if a plurality of discharge holes are opened, substantially uniform droplets can be formed from the respective discharge holes. .

  The liquid column resonance liquid chamber is a liquid chamber in which a pressure standing wave can be formed by the vibration applied by the vibration generating unit in accordance with the principle of the liquid column resonance phenomenon described later. Examples of the material for forming the liquid column resonance liquid chamber include metals, ceramics, plastics, and silicones. Among these, those that do not dissolve in the resin composition liquid and do not cause modification of the resin composition liquid are preferable.

FIG. 1 is an enlarged schematic view showing a part of droplet forming means of a liquid column resonance type droplet discharge apparatus used in the present embodiment.
As shown in FIG. 1, the droplet forming means 11 of this embodiment includes 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). Of these side wall portions, the liquid common supply passage 17 is communicated with through a communication passage 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 portion (the bottom wall portion on the lower side in FIG. 1) of the wall portions connecting the side wall portions at both ends in the longitudinal direction. A hole 19 is provided. The carrier airflow 41 is caused to flow in a direction parallel to the surface direction of the discharge hole surface. As a result, the droplet 21 ejected from the ejection hole 19 receives a transport airflow from a direction orthogonal to the ejection direction and is transported in an oblique direction. Thereby, the space | interval of the droplet 21 is expanded and coalescence of the droplet 21 is suppressed. In addition, vibration generating means 20 that generates high-frequency vibrations to form a liquid column resonance standing wave is provided on the side of the upper wall portion facing the discharge hole 19 in the liquid column resonance liquid chamber 18 via a vibration plate 22. Is provided. The vibration generating means 20 is connected to a high frequency power source (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 a liquid column resonance standing wave is generated by a mechanism described later as a droplet 21 from the discharge hole 19. To 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 can be appropriately selected according to the purpose. It is preferably determined based on the column resonance principle. Further, as shown in FIG. 2, the width W of the liquid column resonance liquid chamber 18 is not particularly limited and can be appropriately selected according to the purpose. However, so as not to give an extra frequency to the liquid column resonance. It is preferable that the length is less than one half of the length L of the liquid column resonance liquid chamber 18.

  There is no restriction | limiting in particular as the number of the liquid column resonance liquid chambers in a droplet formation means, According to the objective, it can select suitably. In order to drastically improve the productivity of droplets, it is preferable that a plurality of droplets are arranged with respect to one droplet forming unit. In terms of compatibility between operability and productivity, 100 to 2,000 are preferable. More preferably, 200 to 1,000 are more preferable, and 300 to 700 are particularly preferable.

  The discharge hole is not particularly limited and may be appropriately selected depending on the purpose. However, it is preferable that at least one discharge hole is disposed in at least one region of the antinode of the pressure standing wave. In addition, it is preferable that a plurality of liquid column resonance liquid chambers are disposed.

  There is no restriction | limiting in particular as the number of discharge holes, According to the objective, it can select suitably. When the droplet forming means is a liquid column resonance type, the number of ejection 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 ejection holes. 2 to 100 are preferable, 4 to 60 are more preferable, and 4 to 20 are particularly preferable. When the number of ejection holes formed in one liquid column resonance liquid chamber exceeds 100, the voltage applied to the vibration generating means is set high when droplets of a desired resin composition liquid are formed from the ejection holes. The necessity arises and the behavior of the vibration generating means may become unstable. On the other hand, in the case of 4 to 20, the pressure standing wave is stable and productivity is maintained. The productivity increases as the number of ejection holes increases, but if the number exceeds 20, the ejection holes become too dense and the discharged droplets coalesce into coarse particles, which may adversely affect 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 [micrometer]-40 [micrometer] are preferable, and 2 [micrometer]-15 [micrometer] are more preferable, 6 [μm] to 12 [μm] is particularly preferable. If the opening diameter is less than 1 [μm], the formed droplets are very small, and thus particles (for example, toner) may not be obtained. In addition, when the opening diameter exceeds 40 [μm], the diameter of the droplet of the resin composition liquid is large, and when this is dried and solidified to obtain a desired particle diameter of 3 [μm] to 6 [μm], an organic solvent Therefore, it is necessary to dilute the resin composition liquid (for example, toner composition liquid) into 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 become long. On the other hand, when the opening diameter is 6 [μm] to 12 [μm], when manufacturing a member in which the discharge holes are opened, it is possible to keep small variations in the diameters of the many discharge holes, and to collect the discharge holes densely. This is advantageous in that 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 where the liquid droplets are discharged. If it is a perfect circle, it means the diameter and is an ellipse, square, hexagon, or octagon. If it is a polygon or regular polygon such as, it means the average diameter.

There is no restriction | limiting in particular as cross-sectional shape of a discharge hole, According to the objective, it can select suitably.
3A to 3D show examples of the cross-sectional shape of the discharge holes. The discharge hole 19 shown in FIG. 3A has such a shape that the opening diameter becomes narrow while having a round shape from the liquid contact surface of the discharge hole 19 toward the discharge port. Therefore, when the thin film 42 in which the discharge hole of the liquid column resonance liquid chamber is formed vibrates, the pressure applied to the liquid in the vicinity of the outlet of the discharge hole 19 is maximized.
The discharge hole 19 shown in FIG. 3B has a taper shape having a taper angle A such that the opening diameter is narrowed at a certain angle from the liquid contact surface of the discharge hole 19 toward the discharge port. Here, the taper angle refers to a perpendicular (opening axis) to the opening surface of the discharge hole 19 (a surface perpendicular to the thickness direction of the formation surface of the discharge hole 19) and a cross section in the thickness direction of the formation surface of the discharge hole 19. The angle formed by the side surface of the cross-sectional shape of the discharge hole 19 in FIG. 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. The range of the taper angle A is 60 [°]. ~ 90 [°] is preferable. When the taper angle A is less than 60 [°], it is difficult for pressure to 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. In this case, it may be difficult to apply pressure to the outlet of the discharge hole 19. When the taper angle exceeds 90 [°], no pressure is applied to the outlet of the discharge hole 19 and the droplet discharge may become very unstable. FIG. 3D shows a shape combining FIG. 3A and FIG. In this way, the shape may be changed step by step.

  In addition, when a plurality of discharge holes are formed, there is no particular limitation on the pitch between the discharge holes (the shortest distance between the central portions of the adjacent discharge holes) in one of the regions that become the antinodes of the pressure standing wave. Can be appropriately selected according to the purpose. It is preferably 20 [μm] or more and not more than the length L of the liquid column resonance liquid chamber, more preferably 20 [μm] to 200 [μm], still more preferably 40 [μm] to 135 [μm], 40 [μm] to 80 [μm] is particularly preferable. If the pitch between the discharge holes is less than 20 [μm], there is a high probability that droplets discharged from adjacent discharge holes collide with each other to form large droplets, leading to deterioration in particle size distribution. 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. However, all of them are equally spaced to obtain particles having a uniform particle size. It is preferable at the point which can do.

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. Examples include a piezoelectric body and an ultrasonic vibration generator. There is no restriction | limiting in particular as a piezoelectric material, According to the objective, it can select suitably. For example, a piezoelectric material made of a material such as a piezoelectric ceramic such as lead zirconate titanate (PZT), a piezoelectric polymer such as polyvinylidene fluoride (PVDF), a single crystal such as quartz, LiNbO ₃ , LiTaO ₃ , or KNbO ₃ 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 by being laminated because the displacement is small. A form in which a piezoelectric body is bonded to an elastic plate is preferable. The elastic plate forms a part of the wall of the liquid column resonance liquid chamber so that the piezoelectric body does not come into contact with the liquid.

  The arrangement of the vibration generating means is not particularly limited and may be appropriately selected according to the purpose. However, the wall surface (longitudinal surface) of the liquid column resonance liquid chamber in which at least one discharge hole is formed is provided. It is preferable that it is formed in the wall which faces. Further, the vibration generating means is preferably bonded to an elastic plate, and the elastic plate preferably forms part of the wall of the liquid column resonance liquid chamber so that the vibration generating means does not come into contact with the liquid. . Furthermore, it is preferable that the vibration generating means is arranged so that it can be individually controlled for each liquid column resonance liquid chamber. In addition, it is preferable to arrange vibration generating means such as a block-shaped piezoelectric body via an elastic plate in accordance with the arrangement of the liquid column resonance liquid chambers, from the viewpoint that each liquid column resonance liquid chamber can be individually controlled.

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

Here, in the case where the liquid column resonance liquid chamber is a fixed end on both sides or equivalent to the fixed ends on both sides, the length between the reflection wall surfaces at both ends in the longitudinal direction of the liquid column resonance liquid chamber is expressed as The length L in the longitudinal direction of In this case, resonance is formed most efficiently when the length L matches an even multiple of one-fourth of the wavelength λ. That is, it is represented by the following formula (2).
L = (N / 4) λ (2)
However, N is an even number.
In addition, “when it is equivalent to the fixed ends on both sides” is a case where it can be considered that there is no pressure relief portion at a certain end. For example, when the height of the reflecting wall surface at one end is more than twice the height of the communication port for supplying the resin composition liquid, and the area of the reflecting wall surface at one end is the communication space for supplying the resin composition liquid. The case where it is 2 times or more of the area of the opening part of a mouth is pointed out. 1, the length from the end of the frame on the fixed end side of the liquid column resonance liquid chamber 18 to the end on the liquid common supply path 17 side corresponds to the length L in FIG. The height h1 (= about 80 [μm]) of the end of the frame on the liquid common 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 on both sides.

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

For the drive frequency f with the highest efficiency, the following formula (3) is derived from the above formula (1) and the above formula (2).
f = N × c / (4L) (3)
However, L represents the length of the liquid column resonance liquid chamber in the longitudinal direction, c represents the speed of sound waves 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 impart vibration of the frequency f at which the above formula (3) is established to the resin composition liquid. However, in actuality, the resin composition liquid has a viscosity that attenuates resonance, so that the vibration is not infinitely amplified, and has a Q value, as shown in equations (4) and (5) described later. In addition, resonance occurs at a frequency in the vicinity of the drive frequency f with the highest efficiency shown in the above equation (3).

  FIGS. 4A to 4D show the standing wave shape (resonance mode) of the velocity and pressure fluctuation when N = 1, 2, and 3. FIG. Although it is originally a sparse / dense wave (longitudinal wave), it is generally expressed as shown in FIGS. 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 one fixed end with N = 1, in the case of a speed standing wave, the amplitude of the speed standing wave is zero at the closed end and the amplitude is maximum at the open 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 resonates is λ, and the integer N is 1 to 5 (N = 4, 5 is not shown) Standing waves are generated most efficiently. In addition, since the standing wave pattern varies depending on the open / closed state of both ends, they are also shown. As will be described later, the condition of the end is determined by the state of the opening of the discharge hole and the opening of 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. Conversely, the closed end 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 reflection occurs. When ideally completely closed or open, a resonance standing wave having a form as shown in FIGS. 4A to 4D is generated by superposition of the waves. However, the standing wave pattern varies depending on the number of ejection holes and the opening position of the ejection holes, and a resonance frequency appears at a position shifted from the position obtained from the above equation (3). In that case, stable ejection 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 are completely equivalent to the fixed ends on both sides. When N = 2 resonance mode is used, the most efficient resonance frequency is derived from the above equation (3) as 324 [kHz]. In another example, 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 the same conditions as described above are used, and there are wall surfaces at both ends. When N = 4 resonance mode equivalent to the fixed ends on both sides is used, the most efficient resonance frequency is derived from the above equation (3) as 648 [kHz], and even in the liquid column resonance liquid chamber having the same configuration, Higher order resonances can be utilized.

  The liquid column resonance liquid chamber 18 in the droplet forming means 11 shown in FIG. 1 has an end that can be described as a soft wall acoustically due to 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 an open end may be used. The influence of the opening of the discharge hole here means that the acoustic impedance is reduced, and in particular, the compliance component is increased. Therefore, the configuration in which the wall surfaces are formed at both ends in the longitudinal direction of the liquid column resonance liquid chamber as shown in FIG. 4B is the resonance mode of the both-side fixed end and all the resonance modes of the one-side open end that the discharge hole side is regarded as an opening. Is a preferable configuration.

  In addition, the numerical aperture of the discharge holes, the opening arrangement position, and the cross-sectional shape of the discharge holes are factors that determine the drive frequency, and the drive frequency can be appropriately determined accordingly. For example, when the number of ejection holes is increased, the restriction at the tip of the liquid column resonance liquid chamber, which has been the fixed end, gradually loosens, a resonance standing wave that is almost close to the open end is generated, and the drive frequency increases. In addition, the opening position of the discharge hole that is closest to the liquid supply path is the starting point, and it becomes a loose constraint condition. 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 driving frequency. When a voltage is applied to the vibration generating unit at the drive frequency determined in this way, the vibration generating unit is deformed, and a resonant standing wave is generated most efficiently at the drive frequency. Further, the liquid column resonance standing wave is generated even at a frequency in the vicinity of the drive frequency at which the resonance standing wave is generated most efficiently. That is, the length between both ends in the longitudinal direction of the liquid column resonance liquid chamber was L, and the distance to the discharge hole closest to the end on the liquid supply side was Le. At this time, the vibration generating unit is vibrated using a drive waveform whose main component is a drive frequency f in a range determined by the following formula (4) and the following formula (5) using both the lengths of L and Le. It is possible to eject liquid droplets from the ejection holes by inducing liquid column resonance.

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

  A liquid column resonance pressure standing wave is formed in the liquid column resonance liquid chamber 18 of FIG. 1 using the principle of the liquid column resonance phenomenon described above, and the discharge holes 19 arranged in a part of the liquid column resonance liquid chamber 18. In this case, the droplets 21 are continuously discharged. Note that it is preferable to dispose the discharge hole 19 at a position where the pressure of the standing wave fluctuates the most, since the discharge efficiency is increased and the driving can be performed with a low voltage.

Next, the state of the liquid column resonance phenomenon occurring in the liquid column resonance liquid chamber in the droplet discharge head in the droplet forming means will be described with reference to FIGS. In FIGS. 5A to 5E, the solid lines drawn in the liquid column resonance liquid chamber indicate arbitrary measurement positions between the fixed end side in the liquid column resonance liquid chamber and the end portion on the liquid common supply path side. The velocity distribution in which the velocity is plotted is shown, the direction from the common liquid supply path to the liquid column resonance liquid chamber is “+”, and the opposite direction is “−”. In addition, the dotted line written in the liquid column resonance liquid chamber indicates a pressure distribution in which the pressure value at any measurement position between the fixed end side and the liquid common supply path side end in the liquid column resonance liquid chamber is plotted, The positive pressure is “+” and the negative pressure is “−” with respect to the atmospheric pressure. Moreover, if it is a positive pressure, a pressure will be applied to the downward direction in the figure, and if it is a negative pressure, a pressure will be applied to the upward direction in the figure.
Further, in FIGS. 5A to 5E, the liquid common supply path side is opened as described above, but the height of the opening through which the liquid common supply path 17 and the liquid column resonance liquid chamber 18 communicate (FIG. 1). The height (the height h1 shown in FIG. 1) of the frame serving as the fixed end is about twice or more than the height h2) shown in FIG. Therefore, the temporal change of the velocity distribution and the pressure distribution is shown under the approximate condition that the liquid column resonance liquid chamber 18 is substantially fixed on both sides.

  FIG. 5A shows a pressure waveform (pressure distribution) and a velocity waveform (velocity distribution) in the liquid column resonance liquid chamber 18 when droplets are discharged. FIG. 5B shows a state in which the meniscus pressure increases again after the liquid is drawn immediately after the droplet is discharged. As shown in FIGS. 5A and 5B, the pressure in the flow path in the liquid column resonance liquid chamber 18 provided with the discharge holes 19 is maximum. Thereafter, as shown in FIG. 5C, the positive pressure in the vicinity of the ejection hole 19 decreases, and the liquid droplet 21 is ejected in a negative pressure direction. And as shown in FIG.5 (d), the pressure of the discharge hole 19 vicinity becomes minimum. From this time, 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 becomes smaller and shifts to the positive pressure direction. At this time, the filling of the resin composition liquid 14 is completed. Then, as shown in FIG. 5A again, the positive pressure in the droplet discharge region of the liquid column resonance liquid chamber 18 becomes maximum, and the droplet 21 is discharged from the discharge hole 19. Thus, a standing wave due to liquid column resonance is generated in the liquid column resonance liquid chamber by high-frequency driving of the vibration generating unit. Further, since the discharge hole 19 is arranged in the droplet discharge region corresponding to the antinode of the standing wave due to the liquid column resonance at the position where the pressure fluctuates the most, the droplet 21 corresponds to the antinode period. The ink is continuously discharged from the discharge hole 19.

Next, the configuration of the particle manufacturing apparatus of the present embodiment will be described.
FIG. 6 is a schematic diagram illustrating the configuration of the particle manufacturing apparatus according to the present embodiment. As shown in FIG. 6, the droplets 21 ejected by the droplet forming unit 11 are supplied by the airflow supply unit 30 and are transported by a transported airflow whose temperature is adjusted. And it is conveyed by the particle formation means 60, and a droplet is dried and solidified, is conveyed to the particle collection means 70 as a collection means, and is collected as a solid particle. The droplets discharged from the droplet forming means 11 can be formed continuously. It is desirable that the airflow supply unit 30 supplies a transport airflow from a lateral direction to the air flow path with respect to the droplet discharge direction, and transports the droplets by the transport airflow. This is because the distance between the droplets can be efficiently separated. In the case of the same direction as the droplet discharge direction, the airflow stays in the vicinity of the discharge holes arranged on the plane, so that the droplets cannot be separated from each other, and the droplets easily come into contact with each other.

  As shown in FIG. 6, an example of a form of feeding the resin composition liquid 14 to the droplet forming unit 11 (droplet forming unit) will be described. In the particle manufacturing apparatus 1, the resin composition liquid 14 accommodated in the raw material container 13 is pumped by the liquid circulation pump 15 through the liquid supply pipe 16 and supplied to the droplet forming means 11. Further, 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 accommodated in the raw material container 13 shown in FIG. 6 flows into the liquid common supply path 17 through the liquid supply pipe 16 by the liquid circulation pump 15 for circulating the resin composition liquid 14. And supplied to the liquid column resonance liquid chamber 18. A pressure distribution is formed in the liquid column resonance liquid chamber 18 filled with the resin composition liquid 14 by the liquid column resonance standing wave generated by the vibration generating means 20. Then, the droplet 21 is ejected from the ejection hole 19 arranged in a region where the amplitude of the liquid column resonance standing wave is large and the pressure fluctuation is large and which is an antinode of the pressure standing wave.

  The liquid feeding pressure to the droplet forming means 11 and the pressure in the particle forming means 60 are managed by a liquid pressure gauge P1 and a pressure gauge P2 in the particle forming means 60. At this time, if the relationship of P1> P2, the resin composition liquid 14 may ooze out from the discharge hole, and if P1 <P2, gas may enter the droplet forming unit 11 and discharge may stop. Therefore, it is desirable that P1≈P2.

  The resin composition liquid 14 that has passed through the liquid common 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 is reduced. Then, a suction force due to the action of the liquid column resonance standing wave in the liquid column resonance liquid chamber 18 acts, 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. 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 liquid common 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.

  In addition, as shown in FIG. 1, the droplet 21 of the resin composition liquid 14 discharged from the droplet forming means 11 in the droplet forming step is transported in the airflow passage 12 by a transport airflow generating means (not shown). When the air flow 41 passes, it flows out to the particle forming means 60 side shown in FIG.

  As shown in FIG. 6, the droplet 21 formed by the droplet forming unit (droplet forming unit 11) falls in the chamber 61 of the particle forming unit 60. At that time, the droplet 21 falls on the airflow sent from the transport airflow inlet 64 at the top of the chamber 61 and is dried in the airflow until it reaches the transport airflow 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 droplet 21 discharged from the droplet forming means 11 in the right direction in FIG. 6 is conveyed by a conveying airflow 41 flowing from above in FIG. 6. When the ejected droplets come into contact with each other before drying, the droplets coalesce into one particle (hereinafter, this phenomenon may be referred to as “coalescence”). In order to obtain solidified particles having a uniform particle size distribution, it is necessary to maintain the distance between the ejected droplets. However, the ejected droplets have a constant initial velocity, but eventually become stalled due to air resistance. The jetted droplets catch up with the stalled particles and coalesce as a result. Since this phenomenon occurs constantly, the particle size distribution is greatly deteriorated when the particles are collected. In order to prevent coalescence, it is preferable to transport the liquid droplets while solidifying the liquid droplets while preventing the liquid droplets from decreasing in speed and preventing the liquid droplets from coming into contact with each other. Therefore, it is preferable in terms of manufacturing efficiency that the solidified particles are conveyed to the particle collecting means 70 by an air flow.

  As shown in FIG. 6, there is no particular limitation as long as it is a means that can adjust the temperature of the carrier airflow 41 supplied by the airflow supply means 30 and supply the carrier airflow 41 into the air flow path, and appropriately depending on the purpose. You can choose. The temperature adjustment step is not particularly limited as long as it is a step capable of adjusting the temperature of the transport airflow 41 in the droplet transport means, and can be appropriately selected according to the purpose, but the airflow supply means 30 is used. preferable. As the air flow supply means 30, although not shown in FIG. 6, the air flow adjustment means preferably has a control mechanism that measures the air flow temperature and stabilizes the air flow temperature. In this embodiment, although it has a some air flow supply means, it has a mechanism which can adjust temperature for every air flow supply means.

  As shown in FIG. 6, the particle forming means 60 is not particularly limited as long as it is a means for drying and solidifying the droplets 21 in an air current to form particles, and can 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 drying and solidifying the droplet 21 in an air stream to form particles, and can be appropriately selected according to the purpose. It is preferable to carry out.

  The method of drying and solidifying the droplet 21 in an air stream (hereinafter referred to simply as “air stream” to distinguish from the above-mentioned “conveying air stream”) is not particularly limited and may be appropriately selected depending on the purpose. After the droplet 21 is discharged out of the discharge hole by the droplet forming means 11, the droplet 21 is dried while being transported by an air stream, that is, the solvent in the droplet is being transported while the droplet 21 is being transported by the air stream. The method of volatilizing with is mentioned. There is no restriction | limiting in particular as a speed | rate of airflow, Although it can select suitably according to the objective, It is preferable that it is faster than the free fall speed | velocity | rate of the droplet and the particle | grains from which the droplet dried. There is no restriction | limiting in particular as atmosphere (temperature, vapor pressure, the kind of gas, etc.) of the gas used for an airflow, According to the objective, it can select suitably. Examples of the type of gas include air or incombustible gas such as nitrogen. These may be used individually by 1 type and may use 2 or more types together.

  It should be noted that the particles obtained by drying the droplets may not be completely dried as long as the solid state can be maintained. In order to increase the productivity, the particles can be collected in the minimum dry state that can be collected, and further dried in a state separated from the carrier airflow with a large amount of solvent vapor, thereby reducing the time for drying the particles.

  As shown in FIG. 6, the particle collecting means 70 as the collecting means is not particularly limited as long as it can separate and collect the air flow and the solidified particles, and a known one such as a cyclone or a bag filter may be used. it can. Further, both a cyclone and a bag filter may be used. In the present invention, since the solidified particles tend to soften, a cyclone is used in the front stage and a bag filter is used in the rear stage. Thereby, filter clogging when particles are softened by the bag filter can be easily suppressed, and passage of a very small amount of microscopic particles that cannot be collected by the cyclone can be reliably suppressed, and release to the atmosphere can be suppressed.

  After the solidified particles are collected, it is preferable that a secondary drying step described later is further performed.

  Examples of other means include secondary drying means. Examples of other processes include a secondary drying process.

  The secondary drying means is not particularly limited as long as it is means for further drying the particles formed in the particle forming step, and can be appropriately selected according to the purpose. For example, a fluid bed drying apparatus, a vacuum drying apparatus 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 is preferably performed by a secondary drying means. .

  If the particles are toner particles, the toner characteristics such as heat-resistant storage stability, fixability, and charging characteristics fluctuate over time if the solvent content contained (residual) in the particles formed in the particle formation process is large. In addition, the solvent volatilizes during fixing by heating. For this reason, possibility that it will have a bad influence on a user and peripheral devices increases. Therefore, it is preferable to reduce the solvent in the particles by the secondary drying step.

  When the particles to be produced are particles that do not contain a resin component, such as particles for secondary battery positive electrode materials, the resin is produced after the particles are prepared from the resin composition liquid (after the particle forming step) or during the particle forming step. A 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. The heating temperature in the heat treatment is not particularly limited as long as it is a temperature at which the resin component contained in the resin composition liquid can be thermally decomposed, and can be appropriately selected according to the purpose.

  If some of the discharge holes are clogged, for example, and non-discharge occurs over time, and the discharge amount of the resin composition liquid decreases, the amount of solvent that volatilizes in the particle forming means or the particle forming step decreases. When the solvent volatilizes, the latent heat of vaporization is removed from the airflow, so the temperature of the airflow at the transport airflow outlet 65 (see FIG. 6) is lower than the temperature of the transport airflow inlet 64 (see FIG. 6). When the amount of droplets to be dried decreases with time, the temperature of the airflow at the transport airflow outlet increases with time.

Therefore, the temperature of the air flow and the temperature of the particles in the particle forming means or the particle forming process when the discharge amount of the resin composition liquid was decreased were measured.
For example, consider the case where the following collection condition 1 is used.
Air flow rate at the carrier air flow inlet 64 (see FIG. 6): 60 [m ³ / hour]
Airflow gas type: Nitrogen gas Airflow temperature at the carrier airflow inlet: 95 [° C]
Solid content concentration of resin composition liquid: 10 [% by mass]
Solvent type of resin composition liquid: ethyl acetate (boiling point 77 [° C.])
Evaporation latent heat of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara et al., P. 569)
Average particle diameter of manufactured particles: 5.4 [μm]
Specific gravity of particles: 1.2 [g / cm ³ ]
Droplet forming means: liquid column resonance type (see FIGS. 1 and 2)
Number of ejection holes of the droplet forming unit: 10240 [pieces]
Frequency when discharging: 310 [kHz]
Distance from transport airflow inlet 64 to transport airflow outlet 65: 3000 [mm]
Assuming that 6 [% by mass] of the solvent was dried and the dried particles were obtained under the above conditions, the temperature of the airflow decreased due to the latent heat of evaporation of the solvent, and the airflow and particles in the transport airflow outlet 65 after 60 seconds from the start of discharge. The temperature became 31 [° C.].

  However, since the droplet forming unit 11 is exposed to a 95 [° C.] conveying airflow, the temperature gradually rises and the droplet discharge amount decreases. After 10 minutes, the droplet discharge amount was halved, and the temperature of the airflow at the transport airflow 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, and the temperature of the droplet forming means rises due to the heat from the carrier air stream.

  As described above, when the discharge amount of the resin composition liquid decreases with time, the temperature drop of the airflow decreases accordingly. Therefore, drying over time becomes unstable. In addition, as described above, the temperature of the solidified particles substantially coincides with the temperature of the airflow at the transport airflow outlet 65, and therefore, in the case of the collection condition 2, the solidified particles have a higher temperature than the collection condition 1. It solidifies in a state and reaches the particle collecting means 70 (see FIG. 6). The softening temperature of the solidified particles collected at the beginning of droplet discharge was about 37 [° C.]. Under the collection condition 1, since the temperature of the solidified particles collected in the initial stage is lower than the softening temperature, the particles remain in a hard state and can be collected by the collection means and the collection step. However, after about 10 minutes, the airflow temperature reaches 55 ° C., and the temperature of the solidified particles exceeds the softening temperature, so that the particles are collected in a softened state. Since the collected particles have a much higher probability of contact between the particles, the solidified basic particles (see FIG. 8) adhere to each other and a large amount of grape-like particles (see FIGS. 9 and 10) are generated. In addition, there is a problem that the particle size distribution deteriorates. Once in the form of grape-like particles, it is very difficult to solve. For reference, the particle size distribution when grape-like particles are included is shown in FIG. 11, and the particle size distribution when no grape-like particles are included is shown in FIG. Comparing the particle size distributions of FIGS. 11 and 12, it can be seen that the grape-like particles greatly deteriorate the particle size distribution.

  As shown in FIG. 6, in the particle manufacturing apparatus 1, the discharge holes of the droplet forming unit 11 are exposed to the transport airflow 41, and therefore have substantially the same temperature as the transport airflow 41. The carrier airflow 41 needs to have a high temperature for particle drying as described above. When the discharge hole of the droplet forming unit 11 is directly exposed to the transport air flow 41, the raw material liquid present in the discharge hole formed in a flat shape of the droplet forming unit 11 is dried and solidified to be blocked or a droplet is formed. The solvent in the raw material liquid inside the means 11 boils or the droplets 21 cannot be discharged. Therefore, by using the first airflow supply means 31, the second airflow supply means 32, and the airflow distribution means 35, the first transport airflow 41a flowing in the vicinity of the droplet forming means 11 and the amount of heat necessary for drying the droplets are obtained. The second conveying airflow 41b is divided. Thereby, it is possible to efficiently dry the droplet 21 and obtain fine particles while preventing the nozzle from being blocked. Therefore, in the present embodiment, the temperature of the first conveying airflow 41a flowing in the vicinity of the droplet forming means needs to be relatively low by a plurality of airflow supply means so as to prevent the discharge holes from drying. The boiling point is preferably equal to or lower than the boiling point of the raw material liquid, more preferably 20 [° C.] lower than the boiling point of the raw material liquid, and further preferably lower than 40 [° C.] of 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 dissolved matter may occur, and it is desirable to set the temperature of the first conveying airflow 41a as low as possible. The 1st air current supply means 31 and the 2nd air current supply means 32 are provided with a heater and a fan.

  The plurality of transport airflows 41 (first transport airflow 41a and second transport airflow 41b) are transported by the airflow distribution means 35, and the layer thickness (height of the transport airflow 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. Since the transport airflows at the plurality of temperatures (the first transport airflow 41a and the second transport airflow 41b) are eventually mixed, the airflow distribution unit 35 is able to create the transport airflow 41 of the droplet forming unit 11 within the droplet transporting unit as much as possible. 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 cannot be sufficiently obtained. If it is 10 [mm] or more, it is necessary to increase the temperature of the second transport airflow 41b very much, so that it is difficult to impart a sufficient amount of heat to the airflow to dry the droplets.

  Furthermore, in order to enhance the effect of the present embodiment, an airflow rectifying means 36 that forms a parallel flow and rectifies the transported airflow is provided immediately after the airflow distribution means 35. Thereby, the 1st conveyance airflow 41a and the 2nd conveyance airflow 41b of several temperature pass the droplet formation means 11 vicinity in the state which maintained the layer form, without mixing. For this reason, the temperature rise of the discharge hole surface formed in the droplet forming means 11 can be further reduced. The airflow rectifying means 36 may have a honeycomb shape, or may be a flat plate in which a plurality of flat plates are perpendicular to the direction of the airflow and parallel to the air flow path surface on which the droplet forming means 11 is disposed. The flat plate parallel to the air flow path surface on which the gas is disposed may be stacked in layers. A known means can be used as long as a rectifying effect is obtained, and a honeycomb shape is preferable. When the honeycomb shape is used, the type of plate constituting the honeycomb shape is preferably a metal and thin plate, but any material or shape may be used as long as it has an airflow rectifying effect. As the pore diameter of the honeycomb shape is finer, a rectifying effect can be expected, but if it is too fine, pressure loss increases and hinders the flow of airflow, so the pore diameter is preferably about 0.1 [mm] to 10 [mm], More preferably, it is 0.5 [mm] to 2 “mm”. In FIG. 6, although two air flow supply means are provided as airflows having a plurality of temperatures, two or three or more airflow supply means may be provided. As shown in FIG. 7, you may have two or more three air flow supply means. In this case, the temperature of the airflow may be increased stepwise as it moves away from the droplet shape 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 necessary. 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. In this case, the resin composition liquid 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 adjusting agent, a magnetic substance, and an additive. Hereinafter, the composition of a resin composition liquid (toner composition liquid) particularly suitable for toner production will be described in detail. However, the resin composition liquid in the present invention is not limited to the resin composition liquid for producing toner. Further, it may be a resin composition liquid for producing spacer particles for liquid crystal panels, a resin composition liquid for producing colored fine particles for electronic paper, or a resin composition liquid for producing a pharmaceutical drug carrier.

(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 disperse | distributing thru | or melt | dissolving in a solvent, for example, binder resin etc. are mentioned. As the binder resin, for example, a vinyl polymer comprising a styrene monomer, an acrylic monomer, a methacrylic monomer, etc., a copolymer comprising these monomers or two or more types, a polyester resin, Examples include polyol resins, phenol resins, silicone resins, polyurethane resins, polyamide resins, furan resins, epoxy resins, xylene resins, terpene resins, coumarone indene resins, polycarbonate resins, petroleum resins, and the like. These may be used individually by 1 type and may use 2 or more types together.

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

  Examples of the alcohol component include a divalent alcohol component, a trivalent or higher alcohol component, and the like. 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, Examples include 1,6-hexanediol, neopentyl glycol, 2-ethyl-1,3-hexanediol, hydrogenated bisphenol A, and diol obtained by polymerizing cyclic ethers 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, 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. Is mentioned.

Examples of the acid component include divalent carboxylic acids and trivalent or higher carboxylic acids. Examples of the divalent carboxylic acid include benzene dicarboxylic acid or its anhydride, alkyl dicarboxylic acid or its anhydride, unsaturated dibasic acid or its anhydride, and the like. Examples of benzenedicarboxylic acid include phthalic acid, isophthalic acid, terephthalic acid, and the like. Examples of the alkyldicarboxylic acid include succinic acid, adipic acid, sebacic acid, azelaic acid and the like. Examples of the unsaturated dibasic acid include maleic acid, citraconic acid, itaconic acid, alkenyl succinic acid, fumaric acid, mesaconic acid and the like.
Examples of the trivalent or higher carboxylic acid component 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-octanetetracarboxylic acid, empol trimer acid, anhydrides thereof, partial lower alkyl esters and the like.

  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 the addition amount of a small quantity of the range which does not prevent that resin melt | dissolves in a solvent.

  When the binder resin is a polyester resin, the molecular weight thereof is not particularly limited and can be appropriately selected according to the purpose. However, the molecular weight distribution by GPC (gel permeation chromatography) shows a molecular weight of 3,000 to 3,000. The presence of at least one peak in the region of 50,000 is preferable in terms of toner fixing properties and hot offset resistance. In addition, as a molecular weight of a tetrahydrofuran (THF) soluble component, a binder resin in which a component of 100,000 or less is 60 [%] to 100 “%” is preferable from the viewpoint of dischargeability, and a molecular weight of 5,000 to Binder resins having at least one peak in the 20,000 region are more preferred.

  When the binder resin is a polyester resin, the acid value is not particularly limited and can be appropriately selected depending on the purpose, but is preferably 0.1 [mgKOH / g] to 100 [mgKOH / g] 0.1 [mgKOH / g] to 70 [mgKOH / g] is more preferable, and 0.1 [mgKOH / g] to 50 [mgKOH / g] is particularly preferable. In the present invention, the acid value of the resin is measured according to 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, the solvent is a droplet forming unit or a droplet formed in the droplet forming step (from the discharge hole). Since the droplets discharged into the gas phase are dried by the particle forming means or the particle forming step, a solvent that can be easily dried is preferable. As such a solvent, a solvent having a boiling point of 100 [° C.] or less is preferable in terms of a high drying rate. Examples of the solvent having a boiling point of 100 [° C.] or lower include ethers, ketones, esters, aromatic hydrocarbons, alcohols and the like. Examples of ethers include tetrahydrofuran (THF). Examples of ketones include acetone, methyl ethyl ketone (MEK), and methyl isobutyl ketone. Examples of the esters include ethyl acetate and butyl acetate. Examples of aromatic hydrocarbons include toluene and xylene. Examples of alcohols include methanol, ethanol, butanol and the like. These may be used individually by 1 type and may use 2 or more types together. Among these, tetrahydrofuran (THF), acetone, methyl ethyl ketone (MEK), ethyl acetate, toluene, and xylene are preferable.

(Coloring agent)
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%] are preferable with respect to the toner obtained, 3 [mass%]-10 [mass%] is more preferable.

  The colorant can also be used as a master batch combined with a resin (master batch resin). In general, the master batch is obtained by dispersing the pigment in hardness in the master batch resin by applying high shear to the mixture of the pigment and the master batch resin. Therefore, the masterbatch need not be used as long as the pigment is sufficiently dispersed.

  There is no restriction | limiting in particular as resin for masterbatch, A conventionally well-known thing can be used. These may be used individually by 1 type, and 2 or more types may be mixed and used for them.

  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 dispersant may be used to increase the dispersibility of the pigment during the production of the masterbatch. The dispersant is preferably highly compatible with the binder resin from the viewpoint of pigment dispersibility, and conventionally known dispersants can be used. Specific examples of commercially available dispersants include, for example, trade names such as Ajisper PB821, Azisper PB822 (above, manufactured by Ajinomoto Fine Techno Co., Ltd.), Disperbyk-2001 (manufactured by Big Chemie Co., Ltd.), and EFKA (registered trademark) -4010. (Manufactured by EFKA).

  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. When the content 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, A wax is preferable. The wax is not particularly limited and can be appropriately selected depending on the purpose. For example, aliphatic hydrocarbon wax, oxide of aliphatic hydrocarbon wax or block copolymer thereof, plant wax, Examples include animal waxes, mineral waxes, and fatty acid esters. Moreover, what deoxidized one part or all part of fatty acid ester can also be used. Examples of the aliphatic hydrocarbon wax include low molecular weight polyethylene, low molecular weight polypropylene, polyolefin wax, microcrystalline wax, paraffin wax, and sazol wax. Examples of the oxide of the aliphatic hydrocarbon wax include polyethylene oxide wax. Examples of plant waxes include candelilla wax, carnauba wax, wood wax, jojoba wax, and the like. Examples of animal waxes include beeswax, lanolin, and whale wax. Examples of the mineral wax include ozokerite, ceresin, and petrolatum. As what has fatty acid ester as a main component, a montanic acid ester wax, caster wax, etc. are mentioned, for example.

  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 [degrees C] are preferable at the point which balances fixing property and hot offset resistance. 70 [° C.] to 120 [° C.] is more preferable. When the melting point is less than 70 [° C.], the blocking resistance may be lowered, and when it exceeds 140 [° C.], the hot offset resistance effect may be hardly exhibited. The peak top temperature of the endothermic peak of the release agent measured by DSC (differential scanning calorimetry) is defined as the melting point of the release agent.

  The DSC is preferably measured with a highly accurate internal heat input compensation type differential scanning calorimeter. As a measuring method, it carries out according to ASTM D3418-82. The DSC curve is measured when the temperature is raised at a temperature rate of 10 [° C./min] after raising and lowering the temperature once and taking a previous history.

  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 mass part-10 mass parts are more preferable.

(Additive)
There is no restriction | limiting in particular as an additive, According to the objective, it can select suitably. Resin composition liquid (toner composition liquid) includes, for example, protection of electrostatic latent image carrier and carrier, improvement of cleaning properties, adjustment of thermal characteristics, electrical characteristics, physical characteristics, resistance adjustment, softening point adjustment, and improvement of fixing rate For the purpose, various metal soaps, fluorine-based surfactants, dioctyl phthalate, conductivity-imparting agents, inorganic fine particles and the like can be added as necessary. The inorganic fine particles may be hydrophobized as necessary. Further, a small amount of an abrasive, an anti-caking agent, and white and black fine particles having a polarity opposite to that of the toner particles can be used as a developing improver which is one type of additive. These may be used individually by 1 type and may use 2 or more types together. Among these, inorganic fine particles are preferable.

  These additives may be those subjected to surface treatment with a surface treatment agent for the purpose of controlling the charge amount. When the surface treatment is performed on the additive, it is advantageous in that the hydrophobicity is increased and deterioration of the additive itself can be prevented even under high humidity. Examples of the surface treatment agent include a silane coupling agent, a silylating agent, a silane coupling agent having a functional group, an organic silicon compound, an organic titanate coupling agent, an aluminum coupling agent, a silicone varnish, a silicone oil, Examples thereof include modified silicone oil.

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

  The solid content 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. Less change in physical properties such as solution viscosity, liquid sound speed, and liquid surface tension is preferable because it is not necessary to change the discharge conditions greatly, and is preferably 30% by mass or less, more preferably 5% by mass to 20% by mass. % By mass] is more preferable. When the solid content concentration is less than 5 [mass%], drying energy and the like may increase in the particle forming step, and the efficiency in production may decrease. Since it is necessary to greatly change the conditions, stable and uniform droplet formation may not be possible.

  The particle production apparatus and the particle production method of the present invention include toner for electrophotography, spacer particles for liquid crystal panels, colored fine particles for electronic paper, particles for electrode materials for secondary batteries and fuel cells, pharmaceutical drug carriers, etc. It can be used for the production of various particles.

  Examples of the present invention will be described below, but the present invention is not limited to the following examples. “Part” represents “part by mass” unless otherwise specified. “%” Represents “% by mass” unless otherwise specified.

(Production example)
<Manufacture of resin composition liquid (toner composition liquid)>
(Preparation of colorant dispersion)
First, a carbon black dispersion 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 primary dispersion was performed using a mixer having stirring blades. As the pigment dispersant, Ajisper PB821 (manufactured by Ajinomoto Fine Techno Co., Ltd.) was used. The obtained primary dispersion is finely dispersed by a strong shearing force using a bead mill (LMZ type manufactured by Ashizawa Finetech Co., Ltd., zirconia bead diameter 0.3 [mm]), and aggregates of 5 [μm] or more are completely obtained. A secondary dispersion (colorant dispersion) was removed.

(Preparation of wax dispersion)
Next, a wax dispersion was prepared.
18 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 primary dispersion was heated to 80 [° C.] while stirring to dissolve the carnauba wax, and then the temperature of the liquid was lowered to room temperature to precipitate wax particles so that the maximum diameter was 3 [μm] or less. As the wax dispersant, a polyethylene wax grafted with a styrene-butyl acrylate copolymer was used. The obtained dispersion is further finely dispersed by a strong shearing force using a bead mill (LMZ type manufactured by Ashizawa Finetech Co., Ltd., zirconia bead diameter 0.3 [mm]) so that the maximum diameter is 1 [μm] or less. This was adjusted to obtain a wax dispersion.

(Dissolution, preparation of dispersion)
Next, a toner composition liquid having the following composition to which a resin as a binder resin, a colorant dispersion liquid, and a wax dispersion liquid 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 are used in 840 parts of ethyl acetate. The mixture was stirred for 10 minutes using a mixer having a stirring blade and dispersed uniformly. Pigments and wax particles did not aggregate due to shock due to solvent dilution.

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

  As shown in FIG. 5A, in the resonance mode in which the length L between both ends in the longitudinal direction of the liquid column resonance liquid chamber in the droplet forming means is 1.85 [mm], N = 2, The first to fourth discharge holes are arranged at the antinodes of the pressure standing wave in the resonance mode of N = 2. A function generator (WF1973, manufactured by NF Circuit Design Block Co., Ltd.) was used as a drive signal generation source (not shown) and connected to the vibration generating means 20 with 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 airflow: nitrogen gas Temperature of first carrier airflow 41a, air flow rate: 25 [° C.], 20 [m ³ / hr]
Temperature and air flow rate of the second carrier airflow 41b: 135 [° C.], 40 [m ³ / hr]
Height of air flow distribution means 35: 5 [mm] from the discharge hole surface of the droplet forming means
Solid content concentration of toner composition liquid: 10 [% by mass]
Solvent type of toner composition liquid: ethyl acetate latent heat of vaporization of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara et al., P. 569)
Average particle diameter of manufactured toner: 5.4 [μm]
Toner specific gravity: 1.2 [g / cm ³ ]
Droplet forming means: liquid column resonance type (see FIGS. 1 and 2)
Number of ejection holes of the droplet forming unit: 10,240 [pieces]
Frequency when discharging: 310 [kHz]
Distance from carrier airflow inlet 64 to carrier airflow outlet 65: 3,000 [mm]
The shape of the particle forming means 60 is a cyclone, 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], and the dust box shape is 80 [mmφ] × 110 [mm].
Under the above conditions, 6 [mass%] solvent was left and dried particles were obtained. The temperature of the airflow decreased due to the latent heat of evaporation of the solvent, and the temperature of the airflow at the transport airflow outlet 65 after 1 minute from the start of droplet discharge was 29 [° C.]. When the discharge was continued for 1 hour, the temperature of the airflow at the carrier airflow outlet 65 was 29 [° C.] and there was no fluctuation. The amount of collected particles at this point was 814 [g]. The collected toner was secondarily dried (40 [° C.], left to stand for 72 hours under ventilation) 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 particle image analyzer (manufactured by Sysmex Corporation, FPIA-3000) under the following measurement conditions. When this was repeated three times, the average of the volume average particle diameter (Dv) was 5.7 [μm], the average of the number average particle diameter (Dn) was 5.4 [μm], and the average of Dv / Dn was 1.05 and almost no nozzle blockage was observed. From the particle image, the ratio of the number of particles in which two or more particles were combined in a grape shape to the total measured particles was 0.8 [%].

A method for measuring the volume average particle diameter and the number average particle diameter of the toner using a flow particle image analyzer will be described below.
The measurement using the flow type particle image analyzer was performed 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, an equivalent circle diameter of 0.60 [μm] or more and less than 159.21 [μm]) in 10 ⁻³ [cm ³ ] water. 10 mL of 20 or less water was prepared. Thereto, a few drops of a nonionic surfactant (preferably, Contaminone N manufactured by Wako Pure Chemical Industries, Ltd.) is added, and further 5 [mg] of a measurement sample is added, and an ultrasonic disperser (manufactured by STM, UH-50) The dispersion treatment was performed for 1 minute under the conditions of 20 [kHz] and 50 [W / 10 cm ³ ]. Furthermore, a dispersion treatment is performed for a total of 5 minutes, and the particle concentration of the measurement sample is 4,000 [pieces / 10 ⁻³ cm ³ ] to 8,000 [pieces / 10 ⁻³ cm ³ ] (particles in the measurement circle equivalent diameter range). A sample dispersion was obtained. Using this, the particle size distribution of particles having an equivalent circle diameter of 0.60 [μm] or more and less than 159.21 [μm] was measured. The sample dispersion was passed through a flat and flat transparent flow cell (thickness: about 200 [μm]) flow path (spread along the flow direction). In order to form an optical path that passes through the thickness of the flow cell, a strobe and a CCD camera are mounted on the flow cell so as to be opposite to each other. While the sample dispersion was flowing, strobe light was irradiated at 1/30 second intervals to obtain an image of 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. In about 1 minute, the equivalent circle diameter of 1,200 or more particles can be measured, and the number based on the equivalent circle diameter distribution and the ratio (number%) of particles having a prescribed 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 production apparatus of the above embodiment (hereinafter, this example is referred to as “Example 2”) will be described.
In Example 2, fine particle production was performed under the following conditions using the particle production apparatus of FIG. 7 in which an airflow supply unit and an airflow distribution unit were added to FIG. 6 one by one.
Same as Example 1.
The collection conditions are as follows.
Gas type of airflow: Nitrogen gas Temperature of first transport airflow 41a, air flow rate: 25 [° C.], 15 [m ³ / hr]
Temperature and air flow rate of the second carrier airflow 41b: 85 [° C.], 30 [m ³ / hr]
Temperature and air flow rate of the third carrier air flow 41c: 40 [° C.], 15 [m ³ / hr]
Height of the first air flow distributing means 35a: 3.75 [mm] from the discharge hole surface of the droplet forming means
Height of second air flow distributing means 35b: 3.75 [mm] from the wall surface facing the discharge hole surface of the droplet forming means
Solid content concentration of toner composition liquid: 10 [% by mass]
Solvent type of toner composition liquid: ethyl acetate latent heat of vaporization of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara et al., P. 569)
Average particle diameter of manufactured toner: 5.4 [μm]
Toner specific gravity: 1.2 [g / cm ³ ]
Droplet forming means: liquid column resonance type (see FIGS. 1 and 2)
Number of ejection holes of the droplet forming unit: 10,240 [pieces]
Frequency when discharging: 310 [kHz]
Distance from carrier airflow inlet 64 to carrier airflow outlet 65: 3,000 [mm]

  The shape of the particle forming means 60 is a cyclone, 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], and the dust box shape is 80 [mmφ]. X110 [mm]. Under the above conditions, 6 [mass%] solvent was left and dried particles were obtained. The temperature of the airflow decreased due to the latent heat of evaporation of the solvent, and the temperature of the airflow at the transport airflow outlet 65 after 1 minute from the start of droplet discharge was 29 [° C.]. When the discharge was continued for 1 hour, the temperature of the airflow at the carrier airflow outlet 65 was 29 [° C.] and there was no fluctuation. At this time, the amount of collected particles was 860 [g], and almost no nozzle blockage was observed. The collected toner was secondarily dried (40 [° C.], left to stand for 72 hours under ventilation) to obtain toner particles of Example 2 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 combined in a grape shape to the total measured particles was 0.5 [%].

The inventors have conducted extensive research and found that the particle size distribution of the collected particles is greatly widened when the environmental temperature in which the particle production apparatus is installed fluctuates. The environmental temperature is relatively lowered, the temperature of the member forming the air flow path is lowered, and the temperature of the second conveying airflow 41b in FIG. 6 flowing while contacting the inner wall surface of the member becomes lower than the target. In the mixed transport airflow in which the first transport airflow 41a and the second transport airflow 41b shown in FIG. 6 are mixed, the liquid droplets discharged from the discharge holes are dried while being transported. For this reason, when the temperature of the second transport airflow 41b becomes lower than the target, the temperature of the mixed transport airflow decreases from the target. As a result, it is considered that the droplets were not sufficiently dried and the particles were not sufficiently solidified, and the particles adhered to each other during transportation to become coarse particles.
Conversely, the environmental temperature rises and the temperature of the second transport airflow 41b becomes higher than the target. If the temperature of the 2nd conveyance airflow 41b becomes higher than aim, the temperature of mixed conveyance airflow will also rise from aim. Since the dried particles are transported on the mixed transport airflow, the temperature of the particles becomes substantially the same as the temperature of the mixed transport airflow higher than the target and becomes higher than the target. As a result, the particles became soft, and it was considered that the particles adhered to each other during transportation and became coarse particles. As described above, when the environmental temperature varies, particles adhere to each other and particles having a narrow particle size distribution cannot be obtained.

Accordingly, as a result of intensive studies, the inventors have made a third flow as shown in FIG. 7 while contacting the inner wall surface of the member forming the air flow path in addition to the first transport air flow 41a and the second transport air flow 41b. The carrier airflow 41c is supplied to the air flow path. It has been found that by adjusting the temperature of the third carrier air flow 41c, particles having a narrow particle size distribution can be produced even when the environmental temperature varies. Specifically, a heater (non-heater) provided in the third airflow supply means 37 is set so that the mixed transport airflow obtained by mixing the first transport airflow 41a, the second transport airflow 41b, and the third transport airflow 41c becomes a target temperature. The temperature of the third conveying airflow 41c is adjusted by adjusting the output temperature of the illustration. By offsetting the fluctuation of the environmental temperature with the temperature adjustment, the mixed transport airflow can be maintained at the target temperature. Thereby, while being able to fully dry and solidify a droplet, the solidification state of particle | grains can be maintained. Therefore, even if environmental temperature fluctuates, it can control that particles adhere and can obtain particles which have a narrow particle size distribution stably.
If the diameter of the discharge hole is increased and the discharge hole is not clogged even if the toner composition liquid is dried at the discharge hole, the first transport air flow 41a is not flowed in FIG. 41b is supplied so as to flow while contacting the surface of the discharge hole. Supplying the third carrier airflow 41c whose temperature can be adjusted according to the fluctuation of the environmental temperature so as to flow in contact with the inner wall surface of the member that forms the air flow path opposite to the discharge hole surface across the second carrier airflow 41b You may make it the structure to carry out.

(Example 3)
Next, another example of the particle production apparatus of the above embodiment (hereinafter, this example is referred to as “Example 3”) will be described.
In Example 3, fine particles were produced 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 airflow distribution means and the first and second transport airflows.

The following collection conditions were used.
Gas type of airflow: Nitrogen gas Temperature of first carrier airflow 41a, air flow rate: 25 [° C.], 4 [m ³ / hr]
Temperature and air flow rate of the second carrier airflow 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 [% by mass]
Solvent type of toner composition liquid: ethyl acetate latent heat of vaporization of solvent: 368.6 [J / g]
(Reference: Solvent Handbook, Shozo Asahara et al., P. 569)
Average particle diameter of manufactured toner: 5.4 [μm]
Toner specific gravity: 1.2 [g / cm ³ ]
Droplet forming means: liquid column resonance type (see FIGS. 1 and 2)
Number of ejection holes of the droplet forming unit: 10,240 [pieces]
Frequency when discharging: 310 [kHz]
Distance from carrier airflow inlet 64 to carrier airflow outlet 65: 3,000 [mm]

  The shape of the particle collecting means is a cyclone, the inner diameter of the circular tube is 70 [mmφ], the restriction is 35 [mm], the height is 350 [mm], the outlet diameter is 30 [mmφ], and the dust box shape is 80 [mmφ]. X110 [mm]. Under the above conditions, 6 [mass%] solvent was left and dried particles were obtained. The temperature of the airflow decreased due to the latent heat of evaporation of the solvent, and the temperature of the airflow at the transport airflow outlet 65 after 1 minute from the start of droplet discharge was 29 [° C.]. When the discharge was continued for 1 hour, the temperature of the airflow at the carrier airflow outlet 65 was 32 [° C.], and a slight increase was confirmed. The amount of particles collected at this time was 770 [g], and it was confirmed that the nozzle was slightly blocked. The collected toner was secondarily dried (40 [° C.], left for 72 hours under ventilation) to obtain toner particles of Example 3 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 combined in a grape shape to the total measured particles was 1.5 [%].

Example 4
Next, another example of the particle production apparatus of the above embodiment (hereinafter, this example is referred to as “Example 4”) will be described.
In Example 4, fine particles were produced 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 airflow distribution means and the first and second transport airflows.

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

  The shape of the particle collecting means is a cyclone, the inner diameter of the circular tube is 70 [mmφ], the restriction is 35 [mm], the height is 350 [mm], the outlet diameter is 30 [mmφ], and the dust box shape is 80 [mmφ]. X110 [mm]. Under the above conditions, 6 [mass%] solvent was left and dried particles were obtained. The temperature of the airflow decreased due to the latent heat of evaporation of the solvent, and the temperature of the airflow at the transported airflow outlet 65 after one minute from the start of droplet discharge was 28 [° C.]. When the discharge was continued for 1 hour, the temperature of the airflow at the conveying airflow outlet 65 was 28 [° C.] and there was no fluctuation. At this time, the amount of collected particles was 860 [g], and no nozzle clogging was observed. The collected toner was secondarily dried (40 [° C.], left for 72 hours under ventilation) to obtain toner particles of Example 3 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 combined in a grape shape to the total measured particles was 0.5 [%].

  In the first to fourth embodiments, a liquid column resonance type liquid droplet ejection unit is used as the liquid droplet ejection apparatus, but other types of liquid droplet ejection units such as a membrane vibration type and a Rayleigh splitting type may be used. In Example 5 below, a Rayleigh split type droplet discharge means is used as the droplet discharge device.

(Example 5)
Next, another example of the particle production apparatus of the above embodiment (hereinafter, this example is referred to as “Example 5”) will be described. In Example 5, the particle production apparatus of FIG. 6 was used, and the above-mentioned Rayleigh splitting type droplet discharge means was used as the droplet formation means, and the particles were produced under the following conditions. The difference from the first embodiment is the difference between the droplet forming means and the second transport airflow.

Here, the phenomenon of liquid column droplet formation in the Rayleigh split type droplet discharge means will be described with reference to FIG.
As explained in Non-Patent Document 1, the uniform liquid droplet formation phenomenon of the liquid column, the wavelength condition λ at which the liquid column is most unstable is expressed by the following equation (6) using the liquid column diameter d (jet). expressed.
λ = 4.5d (jet) (6)
Here, the frequency f of the generated disturbance phenomenon can be expressed by the following equation (7), where v is the velocity of the liquid column.
f = v / λ (7)
Further, as described in Non-Patent Document 2, as a result of deriving the conditions for forming stable uniform particles experimentally, uniform particles can be stably formed under the condition of the following formula (8). There is.
3.5 <λ / d (jet) <7.0 (8)
Furthermore, as explained in Non-Patent Document 3, based on the energy conservation law, the minimum jet V (min) speed at which the liquid discharged from the discharge hole forms a liquid column is expressed by the following equation (9). It is expressed as follows.
v (min) = (8σ / ρd (jet)) (1/2) (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 (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. The phenomenon that the liquid column is formed into droplets by the above-described disturbance by attaching the vibrator to the liquid chamber and vibrating the vibrator at the frequency f has been established in various liquids.

  Since the liquid storage unit needs to be held at least in a state where the toner composition liquid is pressurized, the liquid storage unit is made of a member such as 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. Further, for example, as shown in FIG. 14 described later, a structure in which a plurality of discharge holes are formed in a plate material that is connected by a pipe for supplying a liquid to the liquid storage part and forms a part of the liquid storage part is desirable. In addition, vibration generating means for vibrating the entire liquid storage unit is in contact with the liquid storage unit. It is desirable that the vibration generating means is connected to the driving device by a conductive wire and the vibration state is controlled by the driving device.

The vibration generating means preferably excites the entire liquid storage part having the discharge holes. The vibration generating means is not particularly limited as long as reliable vibration can be given at a constant frequency, and can be appropriately selected and used. Examples thereof include a piezoelectric body and an ultrasonic vibration generating section. 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 thereof include a piezoelectric body formed of a material such as a single crystal such as 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 fixed frequency is not particularly limited and can be appropriately selected according to the purpose. However, 100 [kHz] to 500 [kHz] is preferable, from the viewpoint of generating fine droplets having a uniform particle diameter. 200 [kHz] to 400 [kHz] is more preferable.

  The vibration generating means is in contact with the liquid storage portion, and the plate member having the discharge holes is most preferably arranged in parallel from the viewpoint of uniformly applying vibration to the liquid column generated from the discharge holes. As long as droplet constriction 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 fine droplets having a very uniform particle diameter. Moreover, it is preferable to use what is shown in FIG. 3 for the opening cross-sectional shape of a discharge hole.

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

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

  Under the above conditions, 6.2 [mass%] solvent was left and dried particles were obtained. The temperature of the airflow decreased due to the latent heat of evaporation of the solvent, and the temperature of the airflow at the transport airflow outlet 65 after 31 minutes from the start of droplet discharge was 31 [° C.]. When the discharge was continued for 1 hour, the temperature of the airflow at the carrier airflow outlet 65 was 31 [° C.] and there was no fluctuation. The amount of particles collected at this time was 130 [g], and no nozzle clogging was observed. The collected toner was secondarily dried (40 [° C.], left to stand for 72 hours under ventilation) 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 combined in a grape shape to the total measured particles was 1.0 [%].

(Comparative Example 1)
Next, a comparative example (hereinafter referred to as “comparative example 1”) for the particle manufacturing apparatus of the above embodiment will be described.
In the comparative example 1, only the first airflow supply means 31 is used using the apparatus of FIG. 6, and the height of the airflow distribution means 35 is 15 [mm], that is, only the first conveying airflow 41a flows through 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 conveying air flow 41a were set to 82 [° C.] and 60 [m ³ / hr]. In addition, the total amount and airflow temperature of the 1st conveyance airflow 41a at this time are the same as what mixed the 1st conveyance airflow 41a and the 2nd conveyance airflow 42a in Example 1. FIG.

  Under the above conditions, 6 [mass%] solvent was left and dried particles were obtained. The temperature of the airflow decreased due to the latent heat of vaporization of the solvent, and the temperature of the airflow at the transported airflow outlet 65 after one minute from the start of droplet discharge became 29 [° C.]. After discharging for 1 hour, the temperature of the airflow at the carrier airflow outlet 65 increased to 48 [° C.]. At this time, the amount of collected particles was 407 [g], and about half of the nozzles were visually blocked. The obtained toner has an average volume average particle diameter (Dv) of 7.3 [μm], an average number average particle diameter (Dn) of 5.8 [μm], and an average of Dv / Dn is 1.25. Met. The toner was fixed to the cyclone in a semi-molten state. This is thought to be due to the drop in droplet ejection, which caused the temperature of the airflow to rise and the toner to stick more easily. Since the toners are easily fixed to each other, the ratio of the number of particles in which two or more particles are combined in a grape shape from the particle image to the total measured particles is 23.4 [%]. It was much worse than.

  From the above results, Examples 1 to 5 are more stable in droplet discharge than Comparative Example 1, there is no change in the temperature of the air flow, and the drying and collection of the droplets can be performed stably. It was confirmed that it was possible to produce particles having a narrow particle size distribution by preventing coalescence of the particles.

What has been described above is merely an example, and the present invention has a specific effect for each of the following modes.
(Aspect A)
A liquid droplet forming unit having a plurality of discharge holes 19 on a plane and forming a droplet 21 by discharging a resin composition liquid 14 containing a resin and a solvent from the discharge holes 19 into the air flow path. Means 11, air flow supply 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 collecting particles solidified by drying in the high-temperature carrier air flow In the particle manufacturing apparatus 1 including the particle collecting unit 70 that performs the flow, the air flow supply unit 30 sandwiches the first transport air flow 41a and the first transport air flow 41a supplied so as to flow while in contact with the discharge hole surface. A second carrier airflow 41b having a temperature higher than that of the first carrier airflow 41a 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 first transport air flow 41a having a temperature lower than the temperature of the second transport air flow 41b and not causing the clogging of the discharge holes 19 is brought into contact with the discharge hole surface. The resin composition liquid 14 is prevented from drying through the holes. Thereby, clogging of the discharge holes 19 can be suppressed and the number of clogged discharge holes 19 can be reduced. The temperature of the second transport airflow 41b is a temperature at which the droplets 21 can be sufficiently dried and solidified, but the second transport airflow 41b flows on the opposite side of the discharge hole surface across the first transport airflow 41a. Therefore, it does not touch the discharge hole surface. For this reason, the resin composition liquid 14 is not dried at the discharge holes, and the amount of latent heat of vaporization when the particles are formed can maintain the target value. The temperature of the carrier airflow becomes a target temperature, and the particles are solidified without adhering to each other, so that particles having a target particle diameter can be formed. As a result, it is possible to produce particles having a narrow particle size distribution while suppressing an increase in the temperature of the discharge hole surface that the carrier airflow contacts.

(Aspect B)
In (Aspect A), the air flow supply means 30 causes the third conveying air flow 41c flowing while contacting the inner wall surface of the member forming the air flow path on the side opposite to the discharge hole surface across the air flow path into the air flow path. The third carrier airflow 41c is supplied at a lower temperature than the second carrier airflow 41b.
According to this, as described in the above embodiment, for example, when the environmental temperature fluctuates, if the temperature of the third carrier airflow 41c is adjusted, the fluctuation of the environmental temperature can be offset by the temperature adjustment. For this reason, the mixed conveyance airflow which the several conveyance airflow of the 1st conveyance airflow 41a, the 2nd conveyance airflow 41b, and the 3rd conveyance airflow 41c mixed can be maintained at the target temperature. As a result, the droplets can be sufficiently dried and the particles can be prevented from adhering to each other. Thus, particles having a narrow particle size distribution can be produced.

(Aspect C)
In (Aspect A) or (Aspect B), the air flow rectifying means 36 or the like that arranges a plurality of transport airflows upstream of the discharge holes with respect to the flow direction of the high-temperature transport airflow 41 so that the airflows are parallel to the discharge hole surfaces. A rectifying means is provided. According to this, as described in the above embodiment, a plurality of transport airflows of the first transport airflow 41a, the second transport airflow 41b, and the third transport airflow 41c flow while maintaining parallel airflow to each other. Mixing of the carrier airflow can be suppressed. Thereby, the temperature of the 1st conveyance airflow 41a can be kept at the target temperature, the temperature rise of a discharge hole surface can be suppressed, and clogging of a discharge hole can be suppressed.

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

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

(Aspect F)
A liquid droplet forming unit having a plurality of discharge holes 19 on a plane and forming a droplet 21 by discharging a resin composition liquid 14 containing a resin and a solvent from the discharge holes 19 into the air flow path. Means 11, air flow supply 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 collecting particles solidified by drying in the high-temperature carrier air flow In the particle manufacturing apparatus 1 including the particle collecting means 70, the air flow supply means 30 flows while contacting the inner wall surface of the member that forms the air flow path on the side opposite to the discharge hole surface across the air flow path. The first transport airflow supplied to the air flow path and the second transport airflow higher in temperature than the first transport airflow supplied so as to flow on the opposite side of the inner wall surface across the first transport airflow are supplied into the air flow path.
According to this, as described in the above-described embodiment, when the environmental temperature changes, according to the change in the environmental temperature, the air flows in contact with the inner wall surface separately from the high-temperature second carrier airflow. If the temperature of the supplied first transport airflow is adjusted, the fluctuation of the environmental temperature can be offset by the temperature adjustment. Therefore, the mixed transport airflow in which the first transport airflow and the second transport airflow are mixed can be maintained at the target temperature. Thereby, a droplet can fully be dried, it can suppress that particles adhere, and the particle | grains which have a narrow particle size distribution can be manufactured.

(Aspect G)
In (Aspect A) to (Aspect F), the droplet formation means imparts vibration to the resin composition liquid in the liquid column resonance chamber in which a plurality of ejection holes are formed to form a pressure standing wave by liquid column resonance. Then, a resin composition liquid is discharged from a plurality of discharge holes formed in a region that becomes the antinode of the pressure standing wave to form droplets. According to this, as described in the above embodiment, the discharge efficiency is increased by arranging the discharge hole in the antinode region where the pressure of the pressure standing wave fluctuates the most, and the particles can be efficiently manufactured. it can. A plurality of droplets having substantially the same liquid amount are continuously ejected from the ejection holes in accordance with the antinode period of the pressure standing wave, whereby particles having a narrow particle size distribution can be produced.

(Aspect H)
In (Aspect A) to (Aspect F), the droplet forming means pressurizes the resin composition liquid in the liquid storage portion while applying vibration to the liquid storage portion having a plurality of ejection holes and vibration means by the vibration means, The resin composition liquid discharged from the plurality of discharge holes forms a droplet through a constricted state from the columnar shape. According to this, as described in the above embodiment, the number of droplets formed from the ejection holes can be made relatively large by vibrating the liquid storage portion at a high vibration frequency, and the ejection holes are not easily blocked. For this reason, droplets having a uniform droplet diameter can be obtained, and sufficient productivity can be obtained.

(Aspect I)
A plurality of discharge holes 19 are provided on the plane, and a resin composition liquid 14 containing a resin and a solvent is discharged from the discharge holes 19 into the air flow path to form droplets 21, which are parallel to the surface direction of the discharge hole surface. In a particle manufacturing method in which a high-temperature carrier air flow 41 is supplied into an air flow path so as to flow in a certain direction, dried and solidified in a high-temperature carrier air stream, particles are formed, and particles are collected. A first transport airflow 41a that is supplied so as to flow while contacting, and a second transport airflow 41b that is hotter than the first transport airflow 41a that is supplied so as to flow on the opposite side of the discharge hole surface across the first transport airflow 41a. Are supplied into the air flow path.
According to this, as described in the above embodiment, the first transport air flow 41a having a temperature lower than the temperature of the second transport air flow 41b and not causing the clogging of the discharge holes 19 is brought into contact with the discharge hole surface. The resin composition liquid 14 is prevented from drying through the holes. Thereby, clogging of the discharge holes 19 can be suppressed and the number of clogged discharge holes 19 can be reduced. The temperature of the second transport airflow 41b is a temperature at which the droplets 21 can be sufficiently dried and solidified, but the second transport airflow 41b flows on the opposite side of the discharge hole surface across the first transport airflow 41a. Therefore, it does not touch the discharge hole surface. For this reason, the resin composition liquid 14 does not dry at the discharge holes, and the amount of latent heat of vaporization when the particles are formed can maintain the target value. The temperature of the carrier airflow becomes a target temperature, and the particles are solidified without adhering to each other, so that particles having a target particle diameter can be formed. As a result, it is possible to produce particles having a narrow particle size distribution while suppressing an increase in the temperature of the discharge hole surface that the carrier airflow contacts.

(Aspect J)
A plurality of discharge holes 19 are provided on the plane, and a resin composition liquid 14 containing a resin and a solvent is discharged from the discharge holes 19 into the air flow path to form droplets 21, which are parallel to the surface direction of the discharge hole surface. In a particle manufacturing method in which a high-temperature transport air flow 41 is supplied into an air flow path so as to flow in any direction, dried and solidified in a high-temperature transport air flow, particles are formed, and particles are collected. The first conveying airflow that is supplied so as to flow while contacting the inner wall surface of the member that forms the air flow path on the side opposite to the discharge hole surface, and the opposite side to the inner wall surface across the first conveying airflow A second carrier airflow having a temperature higher than that of the first carrier airflow to be supplied is supplied into the air flow path.
According to this, as described in the above-described embodiment, when the environmental temperature changes, according to the change in the environmental temperature, the air flows in contact with the inner wall surface separately from the high-temperature second carrier airflow. If the temperature of the supplied first transport airflow is adjusted, the fluctuation of the environmental temperature can be offset by the temperature adjustment. Therefore, the mixed transport airflow in which the first transport airflow and the second transport airflow are mixed can be maintained at the target temperature. Thereby, a droplet can fully be dried, it can suppress that particles adhere, and the particle | grains which have a narrow particle size distribution can be manufactured.

DESCRIPTION OF SYMBOLS 1 Particle manufacturing apparatus 11 Droplet formation means 14 Resin composition liquid 17 Liquid common supply path 18 Liquid column resonance liquid chamber 19 Discharge hole 20 Vibration generating means 21 Droplet 22 Vibration plate 30 Airflow supply means 31 First airflow supply means 32 Second Air flow supply means 33 First air flow path 34 Second air flow path 35 Air flow distribution means 36 Air flow rectification means 37 Third air flow supply means 38 Third air flow path 41 Transport air flow 41a First transport air flow 41b Second transport air flow 41c Third transport air flow 60 Particle forming means 61 Chamber 64 Conveying airflow inlet 65 Conveying airflow outlet 70 Particle collecting means 71 Particle collecting section 72 Particle storing section 100 Droplet forming unit 101 Liquid storing section 102 Vibration generating means 103 Discharge hole 104 Piping

Japanese Patent No. 3786034 Japanese Patent No. 3786035 JP-A-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 (10)

An air flow path forming means, a liquid droplet forming means having a plurality of discharge holes on a plane, and discharging a resin composition liquid containing a resin and a solvent into the air flow path from the discharge holes; An air flow supplying means for supplying a high-temperature transport air flow into the air flow path so as to flow in a direction parallel to the surface direction of the hole surface, and a collecting means for collecting particles solidified by drying in the high-temperature transport air flow In a particle manufacturing apparatus comprising:
The air flow supply means supplies the first transport air flow supplied so as to flow while being in contact with the discharge hole surface, and the first transport air flow supplied so as to flow on the opposite side of the discharge hole surface across the first transport air flow. A particle manufacturing apparatus, characterized in that a second carrier airflow having a temperature higher than that of the carrier airflow is supplied into the air flow path. The particle production apparatus according to claim 1,
The air flow supply means supplies a third transport air flow that flows while contacting the inner wall surface of a member forming the air flow path on the opposite side of the discharge hole surface across the air flow path into the air flow path, 3. The particle manufacturing apparatus according to claim 1, wherein the third transport airflow is at a lower temperature than the second transport airflow. In the particle manufacturing apparatus according to claim 1 or 2,
2. A particle manufacturing apparatus, comprising: a rectifying unit that adjusts a plurality of conveying airflows upstream of the discharge holes with respect to a flow direction of the high-temperature conveying airflow so as to obtain an airflow parallel to the surface of the discharge holes. In the particle manufacturing apparatus according to any one of claims 1 to 3,
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 any one of claims 1 to 4,
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. An air flow path forming means, a liquid droplet forming means having a plurality of discharge holes on a plane, and discharging a resin composition liquid containing a resin and a solvent into the air flow path from the discharge holes; An air flow supplying means for supplying a high-temperature transport air flow into the air flow path so as to flow in a direction parallel to the surface direction of the hole surface, and a collecting means for collecting particles solidified by drying in the high-temperature transport air flow In a particle manufacturing apparatus comprising:
The air flow supply means includes a first transport air flow that is supplied so as to flow in contact with an inner wall surface of a member that forms the air flow path on the side opposite to the discharge hole surface across the air flow path, and the first transport. A particle manufacturing apparatus, characterized in that a 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 of the inner wall surface across an air stream is supplied into the air flow path. In the particle manufacturing apparatus according to any one of claims 1 to 6,
The droplet forming means applies vibration to the resin composition liquid in the liquid column resonance chamber in which a plurality of ejection holes are formed to form a pressure standing wave by liquid column resonance, A particle manufacturing apparatus, wherein the resin composition liquid is discharged from the plurality of discharge holes formed in a region to form droplets. In the particle manufacturing apparatus according to any one of claims 1 to 6,
The droplet forming means pressurizes 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 composition portion from the plurality of discharge holes. A particle production apparatus, wherein a resin composition liquid forms a droplet through a constricted state from a columnar shape. A plurality of discharge holes are formed on a plane, and a resin composition liquid containing a resin and a solvent is discharged from the discharge holes into the air flow path to form droplets, which flow in a direction parallel to the surface direction of the discharge hole surface. In the particle manufacturing method of supplying a high-temperature carrier airflow into the air flow path, drying and solidifying in the high-temperature carrier airflow, forming particles, and collecting the particles,
A first conveying airflow that is supplied to flow while in contact with the discharge hole surface, and a first conveying airflow that is hotter than the first conveying airflow that is supplied to flow on the opposite side of the discharge hole surface across the first conveying airflow. 2. A method for producing particles, comprising supplying a carrier airflow into the air flow path. A plurality of discharge holes are formed on a plane, and a resin composition liquid containing a resin and a solvent is discharged from the discharge holes into the air flow path to form droplets, which flow in a direction parallel to the surface direction of the discharge hole surface. In the particle manufacturing method of supplying a high-temperature carrier airflow into the air flow path, drying and solidifying in the high-temperature carrier airflow, forming particles, and collecting the particles,
A first conveying airflow that is supplied to be in contact with an inner wall surface of a member that forms the airflow path on the opposite side of the discharge hole surface across the air flow path; A method for producing particles, comprising: supplying a second carrier airflow having a temperature higher than that of the first carrier airflow supplied so as to flow on a side opposite to the wall surface into the air flow path.