JP2006000796A - Resin particulate manufacturing apparatus, particulate manufacturing method and particulate - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a particulate having a uniform shape and a small particle distribution range by a method gentle for an environment and a particulate manufacturing apparatus. <P>SOLUTION: The particulate manufacturing apparatus is a manufacturing apparatus for manufacturing the particulate using a dispersion liquid in which a dispersoid containing a raw material for manufacturing the particulate is finely dispersed in a dispersion medium, and has a head part provided with a jetting part for jetting the dispersion liquid and a conveying part for conveying the dispersion liquid jetted from the head part and it has a wetting means for wetting the jetting part side of the head part. The wetting means for spraying a liquid mainly constituted of a constitution material of the dispersion medium and containing no dispersion to an area near the delivery part is provided. The liquid is sprayed in a direction perpendicular to the jetting direction of the dispersion liquid jetted from the head part. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a fine particle production apparatus, a fine particle production method, and a fine particle.

A number of methods are known as electrophotographic methods. In general, a process (exposure process) of forming an electrical latent image on a photoconductor by various means using a photoconductive substance, A developing step of developing the latent image using toner (fine particles), a transferring step of transferring the toner image onto a transfer material such as paper, and a step of fixing the toner image by heating, pressing, etc. using a fixing roller. And have.
As a method for producing a toner used in such an electrophotographic method, a pulverization method, a polymerization method, and a spray drying method are used.

  In the pulverization method, a raw material containing a resin as a main component (hereinafter also simply referred to as “resin”) and a colorant is kneaded at a temperature equal to or higher than the softening point of the resin to obtain a kneaded product, and then the kneading. This is a method of cooling and crushing an object. Such a pulverization method is excellent in that the range of selection of raw materials is wide and toner can be produced relatively easily. However, the toner obtained by the pulverization method has the disadvantages that the variation in shape among the particles is large and the particle size distribution tends to be wide. As a result, variations in charging characteristics, fixing characteristics, and the like among the toner particles increase, and the reliability of the entire toner decreases.

  In the polymerization method, toner particles are produced by performing a polymerization reaction in a liquid phase or the like using a monomer that is a constituent component of a resin to produce a target resin. Such a polymerization method is excellent in that the shape of the obtained toner particles can be made to have a relatively high sphericity (geometrically close to a perfect sphere). However, in the polymerization method, there may be a case where the particle size variation cannot be sufficiently reduced between the particles. Further, in the polymerization method, the selection range of the resin material is narrow, and it may be difficult to obtain a toner having the desired characteristics.

  The spray drying method is a method of obtaining a fine powder as a toner by spraying a raw material for toner production dissolved in a solvent using a high-pressure gas. The spray drying method has an advantage that the pulverization step as described above is unnecessary. However, in such a spray drying method, since the raw material is sprayed using a high-pressure gas, it is difficult to accurately control the raw material spraying conditions. For this reason, for example, it is difficult to efficiently produce toner particles having a desired shape and size. Further, in the spray drying method, since the variation in the size of the particles formed by spraying is large, the variation in the moving speed of each particle is also large. For this reason, before the sprayed raw material solidifies, the sprayed particles collide and agglomerate to form an irregularly shaped powder, and the resulting variation in the shape and size of the toner particles is even greater. Sometimes. As described above, since the toner obtained by the spray drying method has a large variation in shape and size among the particles, the variation in charging characteristics and fixing characteristics among the toner particles is large, and the toner as a whole is large. Reliability decreases.

By the way, as a manufacturing apparatus (manufacturing method) for manufacturing a toner having a small variation in shape and size between the particles as described above, a so-called ink jet method is used to disperse a dispersion liquid containing a raw material for toner manufacturing. An apparatus (method) for producing toner particles by discharging from a section has been proposed (see, for example, Patent Document 1).
However, the apparatus described in Patent Document 1 has a problem that when the production of toner is stopped, the dispersion medium or the like in the dispersion liquid is removed in the vicinity of the discharge unit, and the discharge unit is gradually blocked. It was. As a result, toner particles having a uniform shape and size may not be sufficiently obtained. Further, when the removal of the dispersion medium further progresses, clogging or the like may occur and ejection may become impossible. Even when the dispersion liquid is discharged continuously for a long time, the dispersion medium in the dispersion liquid is removed in the vicinity of the discharge section of the head section, and the concentration of the discharged dispersion liquid changes. Occurs, and the discharge portion is gradually blocked, resulting in a change in the discharge amount.

JP 2004-70303 A

  An object of the present invention is to provide fine particles having a uniform shape and a narrow particle size distribution, and a fine particle production method and fine particle production apparatus capable of efficiently producing such fine particles. There is.

Such an object is achieved by the present invention described below.
The fine particle production apparatus of the present invention is a production apparatus for producing fine particles using a dispersion liquid in which a dispersoid containing a raw material for fine particle production is finely dispersed in a dispersion medium,
A head unit including a discharge unit that discharges the dispersion liquid, and a transport unit that transports the dispersion liquid discharged from the head unit,
Wetting means for wetting the ejection part side of the head part is provided.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion can be effectively suppressed, and various problems such as clogging can be prevented. As a result, it is possible to efficiently obtain fine particles with a uniform shape and a small particle size distribution width even when the toner is continuously produced for a long time or when the production is temporarily stopped. Can do.

In the fine particle manufacturing apparatus of the present invention, the wetting means for spraying a liquid that is mainly composed of the constituent material of the dispersion medium and does not contain the dispersoid is provided in the region near the discharge unit. It is preferable.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion can be more effectively suppressed, and various problems such as clogging can be prevented more reliably.

In the fine particle manufacturing apparatus according to the aspect of the invention, it is preferable that the liquid is sprayed in a direction perpendicular to a discharge direction of the dispersion liquid discharged from the head unit.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion can be more effectively suppressed, and various problems such as clogging can be prevented more reliably.
In the fine particle manufacturing apparatus of the present invention, the head unit includes a plurality of the ejection units,
It is preferable that the wetting unit that discharges a liquid that is mainly composed of the constituent material of the dispersion medium and does not contain the dispersoid is provided between at least the plurality of discharge units.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion can be more effectively suppressed, and various problems such as clogging can be prevented more reliably.

In the fine particle manufacturing apparatus of the present invention, it is preferable that the dispersion liquid discharged from the head portion is configured to be discharged into a gas flow flowing substantially in one direction.
Thereby, the granular dispersion liquid (fine particle) in a conveyance part can be conveyed more efficiently.
In the fine particle production apparatus of the present invention, the humidity of the gas is preferably 60% RH or more.
Thereby, it can suppress more effectively that a dispersion medium evaporates from a dispersion liquid in the vicinity of a head part.

In the fine particle production apparatus of the present invention, as the wetting means, a liquid which wipes the surface of the head portion on the discharge portion side, which is mainly composed of the constituent material of the dispersion medium and does not contain the dispersoid. It is preferable that a wiping member impregnated with is provided.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion can be more effectively suppressed, and various problems such as clogging can be prevented more reliably.

In the fine particle manufacturing apparatus of the present invention, it is preferable that the head portion discharges the dispersion liquid vertically upward.
As a result, the concentration of the dispersion medium in the vicinity of the head portion can be made high, and as a result, clogging and the like can be prevented more reliably.

In the fine particle manufacturing apparatus of the present invention, it is preferable that a cooled cooling region is provided in the vicinity of the head portion.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion can be more effectively suppressed, and various problems such as clogging can be prevented more reliably.
In the fine particle manufacturing apparatus of the present invention, it is preferable that a heated heating region is provided downstream of the cooling region in the transport direction of the discharged dispersion liquid.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion is more effectively suppressed, and various problems such as clogging are surely prevented, and the dispersion medium is removed from the dispersion liquid. It can be effectively removed.

In the fine particle manufacturing apparatus of the present invention, it is preferable that the temperature of the heating region is 30 to 150 ° C.
This makes it possible to more efficiently remove the dispersion medium in the dispersion and further improve the productivity of the fine particles.
The fine particle production apparatus of the present invention is preferably configured to introduce a dry gas into the heating region.
This makes it possible to more efficiently remove the dispersion medium in the dispersion and further improve the productivity of the fine particles.

In the fine particle production apparatus of the present invention, the humidity of the dry gas is preferably 50% RH or less.
This makes it possible to more efficiently remove the dispersion medium in the dispersion and further improve the productivity of the fine particles.
In the fine particle production apparatus of the present invention, the fine particles are preferably resin fine particles.
Thereby, resin fine particles having a uniform shape and a small width of the particle size distribution can be provided.

In the fine particle production apparatus of the present invention, the fine particles are preferably toner.
Thereby, a toner having a uniform shape and a small width of the particle size distribution can be provided.
The fine particle production apparatus of the present invention is preferably configured to intermittently discharge the dispersion liquid by piezoelectric pulses.
As a result, the dispersion liquid sprayed (discharged) after being atomized can be discharged intermittently drop by drop, and the stability of the shape of the discharged dispersion liquid is improved. As a result, fine particles with small variations in shape and size between particles can be obtained, and the produced fine particles have a high sphericity (geometrically close to a spherical shape). Is relatively easy.

In the fine particle manufacturing apparatus of the present invention, the head unit includes a dispersion liquid storage unit that stores the dispersion liquid, a piezoelectric body that applies a piezoelectric pulse to the dispersion liquid stored in the dispersion liquid storage unit, and the piezoelectric pulse. It is preferable to have the discharge section that discharges the dispersion liquid.
As a result, the dispersion liquid sprayed (discharged) after being atomized can be discharged intermittently drop by drop, and the stability of the shape of the discharged dispersion liquid is improved. As a result, fine particles with small variations in shape and size between particles can be obtained, and the produced fine particles have a high sphericity (geometrically close to a spherical shape). Is relatively easy.

In the fine particle manufacturing apparatus of the present invention, the frequency of the piezoelectric pulse is preferably 1 kHz to 500 MHz.
Thereby, it is possible to improve the productivity of the fine particles while sufficiently reducing the variation in the shape and size of the discharged liquid dispersion.
The method for producing fine particles of the present invention is characterized by using the fine particle production apparatus of the present invention.
Thereby, it is possible to provide fine particles having a uniform shape and a small width of the particle size distribution.

The method for producing fine particles of the present invention is a method for producing fine particles using a dispersion in which a dispersoid containing a raw material for producing fine particles is finely dispersed in a dispersion medium,
A step of making the dispersion into fine particles and discharging it from a head unit having a discharge unit, solidifying while transporting the inside of the transport unit,
In a state where the discharge unit side of the head unit is wetted, the dispersion liquid is discharged from the head unit to obtain fine particles.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion can be effectively suppressed, and various problems such as clogging can be prevented. As a result, fine particles having a uniform shape and a narrow particle size distribution can be provided.

In the method for producing fine particles of the present invention, the head unit has a plurality of the ejection units,
It is preferable that the liquid is made wet by discharging a liquid that is mainly composed of the constituent material of the dispersion medium and does not contain the dispersoid from between at least the plurality of discharge portions.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion can be more effectively suppressed, and various problems such as clogging can be prevented more reliably.

In the method for producing fine particles of the present invention, it is preferable that the dispersion medium in the dispersion liquid is removed after the dispersion liquid is cooled in a region near the head portion.
Thereby, the evaporation (volatilization) of the unintentional dispersion medium from the dispersion liquid in the vicinity of the head portion is more effectively suppressed, and various problems such as clogging are surely prevented, and the dispersion medium is removed from the dispersion liquid. It can be effectively removed.

In the method for producing fine particles of the present invention, the dispersion medium is preferably removed mainly by heating.
This makes it possible to more efficiently remove the dispersion medium in the dispersion and further improve the productivity of the fine particles.
In the method for producing fine particles of the present invention, it is preferable that the dispersion medium is mainly composed of water and / or a liquid having excellent compatibility with water.
Thereby, for example, the dispersibility of the dispersoid in the dispersion medium can be enhanced, and the dispersoid in the dispersion can have a relatively small particle size and a particularly small variation in size. . As a result, it is possible to obtain fine particles having a particularly small variation in size and shape between particles and a high degree of circularity.

In the method for producing fine particles of the present invention, the dispersion is preferably a suspension.
Thereby, it can prevent more effectively that unnecessary components, such as a solvent, remain in the fine particles finally obtained. As a result, the reliability of the fine particles is particularly excellent.
In the method for producing fine particles of the present invention, the fine particles are preferably resin fine particles.
Thereby, resin fine particles having a uniform shape and a small width of the particle size distribution can be provided.

In the method for producing fine particles of the present invention, the fine particles are preferably toner.
Thereby, a toner having a uniform shape and a small width of the particle size distribution can be provided.
The fine particles of the present invention are produced using the fine particle production apparatus of the present invention.
Thereby, it is possible to provide fine particles having a uniform shape and a small width of the particle size distribution.

The fine particles of the present invention are produced by the method of the present invention.
Thereby, it is possible to provide fine particles having a uniform shape and a small width of the particle size distribution.
In the fine particles of the present invention, the average particle size is preferably 2 to 20 μm.
As a result, for example, when fine particles are applied to the toner, the variation in characteristics such as charging characteristics and fixing characteristics among the toner particles is particularly small, and the reliability of the toner as a whole is particularly high. The resolution of the formed image can be made sufficiently high.

In the fine particles of the present invention, the standard deviation of the particle size between the particles is preferably 1.3 μm or less.
Thereby, for example, when fine particles are applied to the toner, variations in characteristics such as charging characteristics and fixing characteristics among the toner particles are particularly reduced, and the reliability of the toner as a whole is further improved.

In the fine particles of the present invention, the average circularity R represented by the following formula (I) is preferably 0.96 or more.
R = L ₀ / L ₁ (I)
(Wherein, L ₁ [μm] is the peripheral length of the projected image of the fine particle to be measured, and L ₀ [μm] is the peripheral length of a perfect circle having an area equal to the area of the projected image of the fine particle to be measured. To express.)
Thereby, for example, when fine particles are applied to the toner, the transfer efficiency and mechanical strength of the toner particles can be made particularly excellent while the particle diameter of the toner particles is sufficiently small. Also, the fluidity of the toner is improved.
In the fine particles of the present invention, the standard deviation of the average circularity between the particles is preferably 0.015 or less.
As a result, for example, when fine particles are applied to the toner, variations such as charging characteristics and fixing characteristics are particularly reduced, and the reliability of the toner as a whole is further improved.

DESCRIPTION OF EXEMPLARY EMBODIMENTS Preferred embodiments of the fine particle production apparatus, fine particle production method, and fine particles of the present invention will be described below in detail with reference to the accompanying drawings.
The fine particles obtained by the fine particle production apparatus of the present invention may be any particle, but are preferably resin fine particles mainly composed of a resin material, and are used for producing toner particles or toner particles (for example, And toner base particles). Among various fine particles, the toner is required to have a more uniform size and shape uniformity among the particles, and the effect of applying the present invention is particularly remarkable. Therefore, in the following description, toner particles will be representatively described as an example of fine particles.
FIG. 1 is a longitudinal sectional view schematically showing a first embodiment of the toner manufacturing apparatus of the present invention, and FIG. 2 is an enlarged sectional view of the vicinity of the head portion of the toner manufacturing apparatus shown in FIG. In the following description, the upper side in FIG. 1 is referred to as “upper” or “upper”, and the lower side is referred to as “lower” or “lower”.

[Dispersion]
First, the dispersion 6 used in the present invention will be described.
Examples of the dispersion include suspensions (suspensions) and emulsions (emulsions, emulsions, and emulsions). In this specification, “suspension” refers to a dispersion (including a suspended colloid) in which a solid (solid) dispersoid (suspended particle) is dispersed in a liquid dispersion medium. The term “emulsified liquid (emulsion, emulsion, milky liquid)” refers to a dispersion in which a liquid dispersoid (dispersed particles) is dispersed in a liquid dispersion medium. In the dispersion liquid, a solid dispersoid and a liquid dispersoid may coexist. In such a case, among the dispersoids in the dispersion, those in which the proportion of the solid dispersoid is larger than the proportion of the liquid dispersoid is called a suspension, and the proportion of the liquid dispersoid is solid. What is larger than the proportion of the dispersoid in the form of a powder is called an emulsion. In particular, it is preferable that the dispersion used in the present invention has been deaerated. The deaeration process will be described in detail later.
The dispersion 6 has a configuration in which a dispersoid (dispersed phase) 61 is finely dispersed in a dispersion medium 62.

<Dispersion medium>
The dispersion medium 62 may be any material as long as the dispersoid 61 described below can be dispersed, but is mainly a material generally used as a solvent (hereinafter also referred to as “solvent material”). It is preferred that it is constructed.
Examples of such materials include inorganic solvents such as water, carbon disulfide, and carbon tetrachloride, methyl ethyl ketone (MEK), acetone, diethyl ketone, methyl isobutyl ketone (MIBK), methyl isopropyl ketone (MIPK), cyclohexanone, Ketone solvents such as 3-heptanone and 4-heptanone, methanol, ethanol, n-propanol, isopropanol, n-butanol, i-butanol, t-butanol, 3-methyl-1-butanol, 1-pentanol, 2- Alcohol solvents such as pentanol, n-hexanol, cyclohexanol, 1-heptanol, 1-octanol, 2-octanol, 2-methoxyethanol, allyl alcohol, furfuryl alcohol, phenol, diethyl ether, dipropyl ether Ether solvents such as diisopropyl ether, dibutyl ether, 1,2-dimethoxyethane (DME), 1,4-dioxane, tetrahydrofuran (THF), tetrahydropyran (THP), anisole, diethylene glycol dimethyl ether (diglyme), 2-methoxyethanol Cellosolve solvents such as methyl cellosolve, ethyl cellosolve, phenyl cellosolve, aliphatic hydrocarbon solvents such as hexane, pentane, heptane, cyclohexane, methylcyclohexane, octane, didecane, methylcyclohexene, isoprene, toluene, xylene, benzene, ethylbenzene , Aromatic hydrocarbon solvents such as naphthalene, pyridine, pyrazine, furan, pyrrole, thiophene, 2-methylpyridine, 3-methylpyridine, 4-methyl Aromatic heterocyclic compound solvents such as pyridine and furfuryl alcohol, amide solvents such as N, N-dimethylformamide (DMF) and N, N-dimethylacetamide (DMA), dichloromethane, chloroform, 1,2-dichloroethane, Halogenated solvents such as trichloroethylene and chlorobenzene, acetylacetone, ethyl acetate, methyl acetate, isopropyl acetate, isobutyl acetate, isopentyl acetate, ethyl chloroacetate, butyl chloroacetate, isobutyl chloroacetate, ethyl formate, isobutyl formate, ethyl acrylate, methacrylic acid Ester solvents such as methyl acid, ethyl benzoate, amine solvents such as trimethylamine, hexylamine, triethylamine, aniline, nitrile solvents such as acrylonitrile, acetonitrile, nitromethane, Examples include nitro solvents such as nitroethane, organic solvents such as aldehyde solvents such as acetaldehyde, propionaldehyde, butyraldehyde, pentanal, and acrylic aldehyde. A mixture of one or more selected from these is used. be able to.

  Among the above materials, the dispersion medium 62 is mainly composed of water and / or a liquid having excellent compatibility with water (for example, a liquid having a solubility in 100 g of water at 25 ° C. of 30 g or more). preferable. Thereby, for example, the dispersibility of the dispersoid 61 in the dispersion medium 62 can be enhanced, and the dispersoid 61 in the dispersion liquid 6 has a relatively small particle diameter and small variation in size. be able to. As a result, the finally obtained toner particles 9 are small in size and shape variation between the particles, and have high circularity. In particular, when the dispersion medium 62 is composed of water, for example, in the toner manufacturing process, the organic solvent can be substantially prevented from volatilizing. As a result, the toner can be produced by a method that hardly causes adverse effects on the environment, that is, an environmentally friendly method.

  When a mixture of a plurality of components is used as the constituent material of the dispersion medium 62, the constituent material of the dispersion medium is an azeotrope (lowest boiling point azeotrope) between at least two components constituting the mixture. It is preferable to use one that can form As a result, the dispersion medium 62 can be efficiently removed in the conveyance unit of the toner manufacturing apparatus described later. In addition, it becomes possible to remove the dispersion medium 62 at a relatively low temperature in a conveyance unit of a toner manufacturing apparatus, which will be described later, and it is possible to more effectively prevent deterioration of characteristics of the obtained toner particles 9. For example, liquids that can form an azeotrope with water include carbon disulfide, carbon tetrachloride, methyl ethyl ketone (MEK), acetone, cyclohexanone, 3-heptanone, 4-heptanone, ethanol, n-propanol, Isopropanol, n-butanol, i-butanol, t-butanol, 3-methyl-1-butanol, 1-pentanol, 2-pentanol, n-hexanol, cyclohexanol, 1-heptanol, 1-octanol, 2-octanol 2-methoxyethanol, allyl alcohol, furfuryl alcohol, phenol, dipropyl ether, dibutyl ether, 1,4-dioxane, anisole, 2-methoxyethanol, hexane, heptane, cyclohexane, methylcyclohexane, octane, dideca , Methylcyclohexene, isoprene, toluene, benzene, ethylbenzene, naphthalene, pyridine, 2-methylpyridine, 3-methylpyridine, 4-methylpyridine, furfuryl alcohol, chloroform, 1,2-dichloroethane, trichloroethylene, chlorobenzene, acetylacetone, acetic acid Ethyl acetate, methyl acetate, isopropyl acetate, isobutyl acetate, isopentyl acetate, ethyl chloroacetate, butyl chloroacetate, isobutyl chloroacetate, ethyl formate, isobutyl formate, ethyl acrylate, methyl methacrylate, ethyl benzoate, trimethylamine, hexylamine, triethylamine Aniline, acrylonitrile, acetonitrile, nitromethane, nitroethane, acrylic aldehyde and the like.

Further, the boiling point of the dispersion medium 62 is not particularly limited, but is preferably 180 ° C. or lower, more preferably 150 ° C. or lower, and further preferably 35 to 130 ° C. As described above, when the boiling point of the dispersion medium 62 is relatively low, the dispersion medium 62 can be removed relatively easily in the conveyance unit of the toner manufacturing apparatus described later. Further, by using such a material as the dispersion medium 62, the residual amount of the dispersion medium 62 in the finally obtained toner particles 9 can be made particularly small. As a result, the reliability as a toner is further increased.
The dispersion medium 62 may contain components other than the materials described above. For example, in the dispersion medium 62, various materials such as materials exemplified later as constituents of the dispersoid 61, inorganic fine powders such as silica, titanium oxide, and iron oxide, organic fine powders such as fatty acids and fatty acid metal salts, etc. Additives and the like may be included.

<Dispersed quality>
The dispersoid 61 is usually made of a material containing at least a resin as a main component or a precursor thereof (hereinafter collectively referred to as “resin material”). Examples of the resin precursor include a monomer, a dimer, and an oligomer of the resin.

Hereinafter, the constituent material of the dispersoid 61 will be described.
1. Resin (binder resin)
Examples of the resin (binder resin) include polystyrene, poly-α-methylstyrene, chloropolystyrene, styrene-chlorostyrene copolymer, styrene-propylene copolymer, styrene-butadiene copolymer, and styrene-vinyl chloride copolymer. Polymer, styrene-vinyl acetate copolymer, styrene-maleic acid copolymer, styrene-acrylic acid ester copolymer, styrene-methacrylic acid ester copolymer, styrene-acrylic acid ester-methacrylic acid ester copolymer, styrene -Monopolymer or copolymer containing styrene or styrene-substituted styrene resin such as methyl α-chloroacrylate copolymer, styrene-acrylonitrile-acrylic acid ester copolymer, styrene-vinyl methyl ether copolymer , Polyester resin, epoxy tree Fat, urethane-modified epoxy resin, silicone-modified epoxy resin, vinyl chloride resin, rosin-modified maleic acid resin, phenyl resin, polyethylene, polypropylene, ionomer resin, polyurethane resin, silicone resin, ketone resin, ethylene-ethyl acrylate copolymer, xylene Examples thereof include resins, polyvinyl butyral resins, terpene resins, phenol resins, aliphatic or alicyclic hydrocarbon resins, and one or more of these can be used in combination. In addition, when a toner is manufactured by polymerizing a raw material in the dispersoid 61 in a transport unit of a toner manufacturing apparatus to be described later, the above resin material monomers, dimers, oligomers and the like are usually used.
The content of the resin in the dispersoid 61 is not particularly limited, but is preferably 2 to 98 wt%, more preferably 5 to 95 wt%.

2. Solvent The dispersoid 61 may contain a solvent that dissolves at least a part of its components. Thereby, for example, the fluidity of the dispersoid 61 in the dispersion liquid 6 can be improved, and the dispersoid 61 in the dispersion liquid 6 has a relatively small particle size and small variation in size. be able to. As a result, the finally obtained toner particles 9 are small in size and shape variation between the particles, and have high circularity.

Any solvent can be used as long as it dissolves at least a part of the components constituting the dispersoid 61. However, the solvent can be easily removed by a transport unit of a toner manufacturing apparatus as described below. Preferably there is.
The solvent is preferably a solvent having low compatibility with the dispersion medium 62 described above (for example, a solvent having a solubility in 100 g of the dispersion medium at 25 ° C. of 30 g or less). Thereby, the dispersoid 61 can be finely dispersed in the dispersion 6 in a stable state.
Moreover, the composition of the solvent can be appropriately selected according to, for example, the composition of the resin and the colorant described above, the composition of the dispersion medium, and the like.

  Examples of the solvent include inorganic solvents such as water, carbon disulfide, and carbon tetrachloride, methyl ethyl ketone (MEK), acetone, diethyl ketone, methyl isobutyl ketone (MIBK), methyl isopropyl ketone (MIPK), cyclohexanone, and 3-heptanone. , Ketone solvents such as 4-heptanone, methanol, ethanol, n-propanol, isopropanol, n-butanol, i-butanol, t-butanol, 3-methyl-1-butanol, 1-pentanol, 2-pentanol, Alcohol solvents such as n-hexanol, cyclohexanol, 1-heptanol, 1-octanol, 2-octanol, 2-methoxyethanol, allyl alcohol, furfuryl alcohol, phenol, diethyl ether, dipropyl ether, diisopropyl Ether solvents such as pyr ether, dibutyl ether, 1,2-dimethoxyethane (DME), 1,4-dioxane, tetrahydrofuran (THF), tetrahydropyran (THP), anisole, diethylene glycol dimethyl ether (diglyme), 2-methoxyethanol Cellosolve solvents such as methyl cellosolve, ethyl cellosolve, phenyl cellosolve, aliphatic hydrocarbon solvents such as hexane, pentane, heptane, cyclohexane, methylcyclohexane, octane, didecane, methylcyclohexene, isoprene, toluene, xylene, benzene, ethylbenzene , Aromatic hydrocarbon solvents such as naphthalene, pyridine, pyrazine, furan, pyrrole, thiophene, 2-methylpyridine, 3-methylpyridine, 4-methylpyridine Aromatic heterocyclic compound solvents such as furfuryl alcohol, amide solvents such as N, N-dimethylformamide (DMF), N, N-dimethylacetamide (DMA), dichloromethane, chloroform, 1,2-dichloroethane, trichlorethylene, Halogenated solvents such as chlorobenzene, acetylacetone, ethyl acetate, methyl acetate, isopropyl acetate, isobutyl acetate, isopentyl acetate, ethyl chloroacetate, butyl chloroacetate, isobutyl chloroacetate, ethyl formate, isobutyl formate, ethyl acrylate, methyl methacrylate Ester solvents such as ethyl benzoate, amine solvents such as trimethylamine, hexylamine, triethylamine and aniline, nitrile solvents such as acrylonitrile and acetonitrile, nitromethane, nitroethane Organic solvents such as nitro solvents such as aldehyde, aldehyde solvents such as acetaldehyde, propionaldehyde, butyraldehyde, pentanal, acrylic aldehyde, etc. are used, and one or a mixture of two or more selected from these is used. be able to. Among these, those containing an organic solvent are preferred, and ether solvents, cellosolve solvents, aliphatic hydrocarbon solvents, aromatic hydrocarbon solvents, aromatic heterocyclic compounds solvents, amide solvents, halogen compound solvents. More preferably, the solvent contains one or more selected from a solvent, an ester solvent, a nitrile solvent, a nitro solvent, and an aldehyde solvent. By using such a solvent, the above-described components can be dispersed sufficiently uniformly in the dispersoid 61 relatively easily.

  In addition, the dispersoid 61 usually contains a colorant. Examples of the colorant that can be used include pigments and dyes. Examples of such pigments and dyes include carbon black, spirit black, lamp black (CI No. 77266), magnetite, titanium black, chrome lead, cadmium yellow, mineral fast yellow, navel yellow, and naphthol yellow S. , Hansa Yellow G, Permanent Yellow NCG, Chrome Yellow, Benzidine Yellow, Quinoline Yellow, Tartrazine Lake, Red Mouth Lead, Molybdenum Orange, Permanent Orange GTR, Pyrazolone Orange, Benzidine Orange G, Cadmium Red, Permanent Red 4R, Watching Red Calcium salt, eosin lake, brilliant carmine 3B, manganese purple, fast violet B, methyl violet lake, bitumen, cobalt blue, al Reblue Lake, Victoria Blue Lake, First Sky Blue, Indanthrene Blue BC, Ultramarine, Aniline Blue, Phthalocyanine Blue, Calco Oil Blue, Chrome Green, Chrome Oxide, Pigment Green B, Malachite Green Lake, Phthalocyanine Green, Final Yellow Green G, Rhodamine 6G, quinacridone, rose bengal (C.I. No. 45432), C.I. I. Direct Red 1, C.I. I. Direct Red 4, C.I. I. Acid Red 1, C.I. I. Basic Red 1, C.I. I. Modern Tread 30, C.I. I. Pigment red 48: 1, C.I. I. Pigment red 57: 1, C.I. I. Pigment red 122, C.I. I. Pigment red 184, C.I. I. Direct Blue 1, C.I. I. Direct Blue 2, C.I. I. Acid Blue 9, C.I. I. Acid Blue 15, C.I. I. Basic Blue 3, C.I. I. Basic Blue 5, C.I. I. Modern Blue 7, C.I. I. Pigment blue 15: 1, C.I. I. Pigment blue 15: 3, C.I. I. Pigment blue 5: 1, C.I. I. Direct Green 6, C.I. I. Basic Green 4, C.I. I. Basic Green 6, C.I. I. Pigment yellow 17, C.I. I. Pigment yellow 93, C.I. I. Pigment yellow 97, C.I. I. Pigment yellow 12, C.I. I. Pigment yellow 180, C.I. I. Pigment Yellow 162, nigrosine dye (CI No. 50415B), metal complex dye, silica, aluminum oxide, magnetite, maghemite, various ferrites, cupric oxide, nickel oxide, zinc oxide, zirconium oxide, titanium oxide, Examples thereof include metal oxides such as magnesium oxide, and magnetic materials containing magnetic metals such as Fe, Co, and Ni, and one or more of these can be used in combination. Such a colorant is usually contained in the dispersoid 61 in the dispersion liquid 6.

  The content of the colorant in the dispersoid 61 is not particularly limited, but is preferably 0.1 to 10 wt%, and more preferably 0.3 to 3.0 wt%. If the content of the colorant is less than the lower limit, it may be difficult to form a visible image having a sufficient density depending on the type of the colorant. On the other hand, when the content of the colorant exceeds the upper limit, the fixing characteristics and charging characteristics of the finally obtained toner may be deteriorated.

  Further, the dispersoid 61 may contain a wax. The wax is usually used for the purpose of improving releasability. Examples of such wax include plant waxes such as candelilla wax, carnauba wax, rice wax, cotton wax, and wood wax, animal waxes such as beeswax and lanolin, montan wax, ozokerite, and ceresin. Mineral waxes such as mineral waxes, paraffin waxes, microwaxes, microcrystalline waxes, petroleum waxes such as petrolatum waxes, Fischer-Tropsch waxes, polyethylene waxes (polyethylene resins), polypropylene waxes (polypropylene resins) ), Synthetic hydrocarbon waxes such as oxidized polyethylene wax, oxidized polypropylene wax, 12-hydroxystearic acid amide, stearic acid amide, phthalic anhydride imide, chlorinated hydrocarbons Fatty acid amides, esters, ketones, synthetic wax wax such as ether and the like, can be used singly or in combination of two or more of them. Further, as the wax, a crystalline polymer resin having a lower molecular weight may be used. For example, a homopolymer or copolymer of polyacrylate such as poly n-stearyl methacrylate and poly n-lauryl methacrylate (for example, It is also possible to use a crystalline polymer having a long alkyl group in the side chain, such as a copolymer of n-stearyl acrylate-ethyl methacrylate).

The content of the wax in the dispersoid 61 is not particularly limited, but is preferably 0.1 to 10 wt%, and more preferably 0.1 to 5 wt%. If the content of the wax is too large, the wax is liberated and coarsened in the finally obtained toner particles, and the toner seeps into the toner particle surface and the transfer efficiency of the toner tends to decrease. Indicates.
The softening point of the wax is not particularly limited, but is preferably 50 to 180 ° C, and more preferably 60 to 160 ° C.

  Further, the dispersion 6 and / or the dispersoid 61 may contain the above components. Examples of such components include emulsifying dispersants, charge control agents, magnetic powders, and the like. Among these, when the emulsifying dispersant is used, for example, the dispersibility of the dispersoid 61 in the dispersion 6 can be improved. Here, examples of the emulsifying dispersant include emulsifiers, dispersants, and dispersion aids.

Examples of the dispersant include inorganic dispersants such as tricalcium phosphate, nonionic organic dispersants such as polyvinyl alcohol, carboxymethyl cellulose, and polyethylene glycol, metal tristearate (for example, aluminum salt), and metal distearate. Salt (eg, aluminum salt, barium salt, etc.), stearic acid metal salt (eg, calcium salt, lead salt, zinc salt, etc.), linolenic acid metal salt (eg, cobalt salt, manganese salt, lead salt, zinc salt, etc.) , Octanoic acid metal salts (eg, aluminum salts, calcium salts, cobalt salts, etc.), oleic acid metal salts (eg, calcium salts, cobalt salts, etc.), palmitic acid metal salts (eg, zinc salts, etc.), naphthenic acid metal salts (For example, calcium salt, cobalt salt, manganese salt, lead salt, zinc salt, etc.), Resin metal salt (example For example, calcium salt, cobalt salt, manganese lead salt, zinc salt, etc.), polyacrylic acid metal salt (for example, sodium salt), polymethacrylic acid metal salt (for example, sodium salt), polymaleic acid metal salt (for example, Sodium salts, etc.), anionic organic dispersants such as acrylic acid-maleic acid copolymer metal salts (eg, sodium salts), polystyrenesulfonic acid metal salts (eg, sodium salts), etc., cations such as quaternary ammonium salts Organic dispersants and the like. Among these, nonionic organic dispersants or anionic organic dispersants are particularly preferable.
The content of the dispersant in the dispersion 6 is not particularly limited, but is preferably 3.0 wt% or less, and more preferably 0.01 to 1.0 wt%.

Examples of the dispersion aid include anions, cations, and nonionic surfactants.
The dispersing aid is preferably used in combination with a dispersing agent. When the dispersion 6 contains a dispersant, the content of the dispersion aid in the dispersion 6 is not particularly limited, but is preferably 2.0 wt% or less, and is 0.005 to 0.5 wt%. Is more preferable.
Examples of the charge control agent include a metal salt of benzoic acid, a metal salt of salicylic acid, a metal salt of alkyl salicylic acid, a metal salt of catechol, a metal-containing bisazo dye, a nigrosine dye, a tetraphenylborate derivative, a quaternary ammonium salt, Examples thereof include alkyl pyridinium salts, chlorinated polyesters, and nitrohumic acid.

Examples of the magnetic powder include magnetite, maghemite, various ferrites, cupric oxide, nickel oxide, zinc oxide, zirconium oxide, titanium oxide, magnesium oxide, and other metal oxides such as Fe, Co, and Ni. The thing comprised with the magnetic material containing a magnetic metal etc. are mentioned.
In addition to the above materials, for example, zinc stearate, zinc oxide, cerium oxide or the like may be added to the dispersion liquid 6.
In addition, components other than the dispersoid 61 may be dispersed in the dispersion 6 as insoluble matters. For example, in the dispersion 6, inorganic fine powders such as silica, titanium oxide, and iron oxide, organic fine powders such as fatty acids and fatty acid metal salts, and the like may be dispersed.

  When the resin fine particles of the present invention are applied to the toner, the content of the constituent component (solid component) of the toner in the dispersion 6 is determined by the size (opening area) of the ejection portion 23 of the head portion 2 described later. Although it is not specifically limited, Usually, it is preferable that it is 1-99 vol%, and it is more preferable that it is 2-20 vol%. When the content of the constituent components of the toner is a value within the above range, a toner having an appropriate size and a particularly small variation in size and shape between particles is manufactured relatively easily. Can do. Further, the circularity of the obtained toner particles 9 can be easily made relatively large. On the other hand, when the toner component content is less than the lower limit value, in order to obtain toner particles 9 having a desired size, in the toner manufacturing apparatus 1 as will be described later, relatively large droplets are formed. The dispersion 6 must be discharged. As a result, depending on the viscosity of the dispersion 6 and the like, the stability of the shape of the droplet-like dispersion 6 is lowered, and the toner particles 9 finally obtained have a large variation in shape and the degree of circularity also tends to be lowered. There is. Moreover, the energy required for solidification of the discharged dispersion liquid 6 also increases. Further, when the content of the constituent components of the toner exceeds the upper limit, depending on the constituent material of the dispersion 6, the viscosity of the dispersion 6 may become too large. As a result, it may be difficult to discharge the liquid dispersion 6 in the toner manufacturing apparatus 1 as described later. In addition, when the content ratio of the constituent components of the toner is particularly high, the droplet-like dispersion liquid 6 to be discharged must be made small, and the above-described tendency becomes particularly remarkable. Here, the “toner component” includes not only the final toner component itself but also a precursor of the component (eg, monomer, dimer, oligomer, etc. of the final toner component). It refers to the component that contributes to the final toner.

In the dispersion 6, the dispersoid 61 is finely dispersed in the dispersion medium 62.
Although the average particle diameter of the dispersoid 61 in the dispersion liquid 6 is not specifically limited, It is preferable that it is 0.05-1.0 micrometer, and it is more preferable that it is 0.1-0.8 micrometer. When the average particle size of the dispersoid 61 is in such a range, the finally obtained toner particles 9 have a sufficiently high circularity and excellent properties and shape uniformity among the particles. It becomes.

  The content of the dispersoid 61 in the dispersion liquid 6 is not particularly limited, but is preferably 1 to 99 wt%, and more preferably 2 to 20 wt%. When the content of the dispersoid 61 is less than the lower limit, the circularity of the finally obtained toner particles 9 tends to decrease. On the other hand, when the content of the dispersoid 61 exceeds the upper limit, depending on the composition of the dispersion medium 62 and the like, the viscosity of the dispersion 6 is increased, and the shape and size of the finally obtained toner particles 9 vary. It shows a tendency to increase.

In the dispersion 6, the dispersoid 61 may be in a solid form, in a liquid form, or may coexist. That is, the dispersion 6 may be a suspension or an emulsion.
When the dispersoid 61 is liquid (for example, in a solution state or a molten state), the average particle diameter of the dispersoid 61 finely dispersed in the dispersion medium 62 is relatively easily set to a value in the above range. can do. In addition, when the dispersoid 61 is in a liquid form, variation in shape and size between the dispersoids 61 can be made particularly small. The variation in shape and size is particularly small.

  Further, when the dispersoid 61 is solid, unnecessary components such as a solvent can be effectively prevented from remaining in the finally obtained toner. As a result, the reliability of the toner is particularly excellent. When the dispersoid 61 is solid, that is, when the dispersion 6 is a suspension, for example, the suspension as the dispersion 6 is prepared via an emulsion. There may be. Thereby, the advantage in the case where the dispersoid 61 is in a liquid state is also effectively exhibited while sufficiently exhibiting the advantage in the case where the dispersoid 61 is in a solid state as described above.

Further, the dispersoid 61 dispersed in the dispersion medium 62 may have, for example, substantially the same composition among the particles or may have different compositions. For example, the dispersion 6 may include, as the dispersoid 61, one mainly composed of a resin material and one mainly composed of wax.
Further, when the dispersion 6 is an emulsion (emulsion), the dispersion 6 is an O / W emulsion, that is, a liquid having a low solubility in water in the aqueous dispersion medium 62. The dispersoid 61 is preferably dispersed. As a result, a toner having a small variation in shape and size between the particles can be stably produced. In addition, by using an aqueous liquid for the dispersion medium 62, the volatilization amount of the organic solvent in the conveying unit of the toner manufacturing apparatus as described later can be reduced, or the organic solvent can be substantially not volatilized. As a result, the toner can be manufactured by a method that hardly causes adverse effects on the environment.

  Further, when the average particle size of the dispersoid 61 in the dispersion 6 is Dm [μm] and the average particle size of the toner particles 9 is Dt [μm], the relationship of 0.005 ≦ Dm / Dt ≦ 0.5 is established. It is preferable to satisfy, and it is more preferable to satisfy the relationship of 0.01 ≦ Dm / Dt ≦ 0.2. By satisfying such a relationship, a toner having a particularly small variation in shape and size among the particles can be obtained.

The dispersion 6 as described above can be prepared using, for example, the following method (first method).
First, an aqueous solution in which a dispersant and / or a dispersion medium is added to water or a liquid excellent in compatibility with water (water-soluble liquid) as necessary is prepared.

  On the other hand, a resin liquid containing a resin as a main component of the toner or a precursor thereof (hereinafter collectively referred to as “resin material”) is prepared. For the preparation of the resin liquid, for example, the above-described solvent may be used in addition to the resin material. The resin liquid may be a molten liquid obtained by heating a resin material.

  Next, the dispersion liquid 6 in which the dispersoid 61 containing the resin material is dispersed in the aqueous dispersion medium 62 is obtained by adding the resin liquid while gradually dropping into the stirred aqueous solution. can get. By preparing the dispersion 6 by such a method, the circularity of the dispersoid 61 in the dispersion 6 can be further increased. As a result, the toner particles 9 have a particularly high degree of circularity and a particularly small variation in shape between the particles. In addition, when dripping a resin liquid, you may heat an aqueous solution and / or a resin liquid. In addition, when a solvent is used for the preparation of the resin liquid, for example, after the dropwise addition as described above, the obtained dispersion liquid 6 is heated or placed in a reduced-pressure atmosphere or the like in the dispersoid 61. You may remove at least one part of the solvent contained. For example, the dispersion 6 can be obtained as a suspension by removing most of the solvent contained in the dispersoid 61.

As mentioned above, although the example of the preparation method of the dispersion liquid 6 was demonstrated, the dispersion liquid is not limited to what was prepared by such a method. For example, the dispersion liquid 6 can also be prepared by the following method (second method).
First, an aqueous solution is prepared by adding a dispersant and / or a dispersion medium as necessary to water or a liquid having excellent compatibility with water.

On the other hand, a powdery or granular material containing a resin material is prepared.
Next, a dispersion liquid in which the dispersoid 61 containing the resin material is dispersed in the aqueous dispersion medium 62 by gradually adding the powdery or granular material into the stirred aqueous solution. 6 is obtained. When the dispersion liquid 6 is prepared by such a method, the organic solvent can be substantially prevented from volatilizing in the transport section of the toner manufacturing apparatus as described later. As a result, the toner can be manufactured by a method that hardly causes adverse effects on the environment. In addition, when adding the said material, you may heat an aqueous solution, for example.

The dispersion 6 can also be prepared by the following method (third method).
First, a resin dispersion in which at least a resin material is dispersed and a colorant dispersion in which at least a colorant is dispersed are prepared.
Next, the resin dispersion and the colorant dispersion are mixed and stirred. At this time, if necessary, an aggregating agent such as an inorganic metal salt may be added while stirring.
By stirring for a predetermined time, an aggregate in which the resin material, the colorant and the like are aggregated is formed. As a result, a dispersion 6 in which the aggregate is dispersed as the dispersoid 61 is obtained.

  In the method for preparing a dispersion as described above, a kneaded material containing a resin material (binder resin) may be used. That is, as the “resin material” in the first method and the third method described above, a kneaded material containing a resin material may be used, or as the “powdered or granular material” in the second method, A kneaded material containing a resin material may be used. Thereby, for example, the toner particles 9 can be obtained as a mixture of the constituent components more uniformly. In particular, even when the toner includes two or more components having poor dispersibility and compatibility, the above-described effects can be obtained. In addition, as a kneaded material, what contains components (for example, components, such as a coloring agent, a wax, a charge control agent) other than a resin component, for example can be used. Thereby, the above effects become more remarkable.

  Further, for example, the method described in Japanese Patent Application No. 2003-113428 may be applied to the preparation of the dispersion liquid 6. That is, a liquid containing a powdered or granular resin material (kneaded material) is ejected from a plurality of nozzles, the liquids ejected from the nozzles collide with each other, and the resin material (kneaded material) is atomized to form fine particles. A method of obtaining the dispersion 6 containing the dispersed dispersoid 61 may be applied. Thereby, the size of the dispersoid 61 contained in the dispersion liquid 6 can be easily made relatively small (the size in the above-described range), and the dispersion of the sizes of the dispersoids 61 can be easily achieved. Can be reduced.

  Further, it is preferable that the dispersion 6 obtained by the above method is subjected to a degassing treatment (subjected to a degassing step) before being used for discharge in a toner manufacturing apparatus described later. Thereby, the dissolved amount of the gas in the dispersion liquid 6 can be reduced, and when the dispersion medium 62 is removed from the dispersion liquid 6 ejected in the form of droplets in the transport unit of the toner manufacturing apparatus described later, It is possible to effectively prevent bubbles and the like from being generated in the dispersion liquid 6. As a result, it is possible to effectively prevent toner particles having irregular shapes (hollow particles, missing particles, etc.) from being mixed into the finally obtained toner. Therefore, it is possible to easily and reliably obtain a toner in which each toner particle has a uniform shape and a narrow particle size distribution. Thereby, the finally obtained toner can be made particularly excellent in properties such as transferability, fluidity, and cleaning properties. Further, by subjecting the dispersion liquid 6 to deaeration treatment, the ratio of pores (voids) in the finally obtained toner particles can be reduced. As a result, the reliability of the toner is further improved.

The method of deaeration treatment is not particularly limited, and for example, a method of applying ultrasonic vibration to the dispersion (ultrasonic vibration method), a method of placing the dispersion in a reduced-pressure atmosphere (decompression method), or the like can be used. .
When the decompression method is used as the degassing method, the pressure of the atmosphere in which the dispersion is placed is preferably 80 kPa or less, more preferably 0.1 to 40 kPa, and further preferably 1 to 27 kPa. preferable. When the atmospheric pressure during the degassing treatment is a value within such a range, the dissolved gas can be efficiently removed while maintaining the shape of the dispersoid 61 in the dispersion 6 sufficiently.

[Particle production equipment]
Next, the fine particle production apparatus of the present invention will be described with reference to the accompanying drawings.
In the following description, a case where the fine particle manufacturing apparatus of the present invention is applied to a toner manufacturing apparatus will be described.
The toner manufacturing apparatus 1 includes a head unit 2 that discharges the dispersion liquid 6 (particularly, the dispersion liquid 6 that has been degassed), and a dispersion liquid supply unit 4 that supplies the dispersion liquid 6 to the head unit 2. The transport unit 3 transports the dispersion 6 discharged from the head unit 2 and the recovery unit 5 that recovers the manufactured toner particles (fine particles) 9.

A dispersion liquid 6 to be described later is stored in the dispersion liquid supply unit 4, and the dispersion liquid 6 is sent to the head unit 2.
The dispersion liquid supply unit 4 may have any function as long as it has a function of supplying the dispersion liquid 6 to the head unit 2. Alternatively, the dispersion liquid supply unit 4 may have stirring means 41 for stirring the dispersion liquid 6 as illustrated. Thereby, for example, even if the dispersoid 61 is difficult to disperse in the dispersion medium, the dispersion 6 in which the dispersoid 61 is sufficiently uniformly dispersed can be supplied into the head portion 2.

The head unit 2 includes a plurality of liquid droplet ejection heads 27 including a dispersion liquid storage unit 21, piezoelectric elements 22, and ejection units 23.
The dispersion liquid storage section 21 stores the dispersion liquid 6 as described above.
The dispersion liquid 6 stored in the dispersion liquid storage unit 21 is discharged from the discharge unit 23 to the transport unit 3 by the pressure pulse of the piezoelectric element 22.

  By the way, in the conventional toner manufacturing apparatus, when the production of the toner is stopped, there is a problem that the dispersion medium in the dispersion liquid is removed in the vicinity of the discharge unit, and the discharge unit is gradually closed. As a result, toner particles having a uniform shape and size may not be sufficiently obtained. Further, when the removal of the dispersion medium further progresses, clogging or the like may occur and ejection may become impossible. Even when the dispersion liquid is discharged continuously for a long time, the dispersion medium in the dispersion liquid is removed in the vicinity of the discharge section of the head section, and the concentration of the discharged dispersion liquid changes. Occurs, and the discharge portion is gradually blocked, resulting in a change in the discharge amount.

  Therefore, as a result of intensive studies to solve the above problems, the present inventor has provided a wetting means for moistening the discharge part side of the head part, so that the unintentional dispersion medium from the dispersion liquid in the vicinity of the head part can be provided. It has been found that evaporation (volatilization) can be effectively suppressed and problems such as clogging can be prevented. As a result, even if the toner is produced continuously for a long time, or even when the production is temporarily stopped (when the discharge of the dispersion liquid is stopped), the particle size distribution is uniform. It has been found that fine particles (toner) having a small width can be efficiently obtained, and the present invention has been completed.

In the toner manufacturing apparatus 1 of the present embodiment, as shown in FIG. 2, the head unit 2 is mainly composed of the constituent material of the dispersion medium 62 in addition to the droplet discharge head 27 that discharges the dispersion liquid 6, and It has a droplet discharge head 27 ′ that discharges a liquid (wetting liquid) 62 ′ that does not contain the dispersoid. This droplet discharge head 27 'has a function as a wetting means.
The droplet discharge head 27 ′ has the same configuration as the droplet discharge head 27. That is, the droplet discharge head 27 ′ includes the wetting liquid storage unit 21 ′, the piezoelectric element 22 ′, and the discharge unit 23 ′.

The droplet discharge heads 27 ′ are randomly arranged among the plurality of droplet discharge heads 27.
By setting it as such a structure, the discharge part 23 side of the head part 2 can be moistened. As a result, involuntary evaporation (volatilization) of the dispersion medium from the dispersion liquid in the vicinity of the head portion can be more effectively suppressed, and problems such as clogging can be prevented more reliably.

  The ratio of the discharge unit 23 ′ that discharges the wetting liquid 62 ′ among the plurality of discharge units (discharge unit 23 and discharge unit 23 ′) is not particularly limited, but is preferably 1 to 10%, More preferably, it is 5%. Thereby, the evaporation (volatilization) of the unintentional dispersion medium 62 from the dispersion liquid 6 in the vicinity of the ejection unit 23 side of the head unit 2 (hereinafter also simply referred to as the vicinity of the head unit 2) is more effectively suppressed. Thus, various problems such as clogging can be prevented more reliably.

The transport unit 3 is configured by a cylindrical housing 31.
As shown in FIG. 1, the transport unit 3 is provided with a cooling region 321 near (directly below) the head unit 2. As shown in the figure, the cooling region 321 is formed by cooling the region immediately below (in the vicinity of) the head unit 2 by the cooling means 32 provided in the housing 31.
Further, as shown in FIG. 1, the transport unit 3 is provided with a heating region 331 on the downstream side in the transport direction of the discharged dispersion 6 (hereinafter also simply referred to as the downstream side) from the cooling region 321. ing. The heating region 331 is formed by heating means 33 provided in the housing 31 as shown in the figure.

  In this way, by providing the cooling region 321 in the vicinity of the head unit 2 and providing the heating region 331 in the downstream side of the cooling region 321, the involuntary dispersion medium 62 evaporates from the dispersion liquid 6 in the vicinity of the head unit 2. It is possible to efficiently remove the dispersion medium 62 from the dispersion 6 while effectively suppressing (volatilization) and more effectively preventing clogging of the discharge unit 23 and the like. As a result, a toner having a uniform shape and a small width of the particle size distribution can be obtained efficiently.

Although the temperature of the cooling region 321 varies depending on the composition of the dispersion medium 62 and the like, it is preferably 10 to 35 ° C., particularly 20 to 25 ° C. when the dispersion medium 62 includes water. Is more preferable. If the temperature of the cooling region 321 is less than the lower limit, depending on the composition of the dispersion 6 and the like, the viscosity of the dispersion 6 may become too high and it may be difficult to discharge from the head unit 2. On the other hand, when the temperature of the cooling region 321 exceeds the upper limit, depending on the composition of the dispersion 6 and the like, the evaporation (volatilization) of the unintentional dispersion medium 62 from the dispersion 6 may not be sufficiently suppressed. .
In the configuration shown in the figure, the cooling region 321 is shorter than the straight traveling region 36, but is not limited to this. For example, the cooling region 321 and the straight traveling region 36 are configured to be substantially the same region. Alternatively, the cooling region 321 may be configured to be longer than the rectilinear region 36.

The heating region (high temperature region) 331 is a region having a higher temperature than the cooling region (low temperature region) 321.
The temperature of the heating region 331 only needs to be higher than the temperature of the cooling region 321. Specifically, the temperature varies depending on the composition of the dispersion medium 62, but particularly when the dispersion medium 62 includes water. Is preferably 30 to 150 ° C., more preferably 50 to 80 ° C. If the temperature of the heating region 331 is less than the lower limit, it may be difficult to sufficiently remove the dispersion medium 62 from the dispersion 6 depending on the composition of the dispersion 6 and the like. On the other hand, when the temperature of the heating region 331 exceeds the upper limit value, depending on the composition of the dispersion 6 and the like, the dispersion medium 62 is abruptly removed, and as a result, voids are generated inside the obtained toner particles. there is a possibility.

  Further, at least a part of the inner wall surface of the housing 31 is subjected to a liquid repellent treatment so as to have liquid repellency with respect to the dispersion liquid 6. Thereby, the dispersion liquid 6 (toner particles 9) can be effectively prevented from adhering to the inner wall surface of the housing 31. As a result, the collection efficiency of the toner particles 9 is also improved. Further, variations in the shape, size, etc. of the toner particles 9 obtained can be made small.

Such a liquid repellent treatment can be performed by applying a liquid repellent material such as a fluororesin such as polytetrafluoroethylene (PTFE) or a silicone resin.
Further, it is preferable that at least a part of the inner wall surface of the housing 31 is subjected to a hydrophobic treatment. Thereby, for example, when the dispersion medium 62 of the dispersion 6 is mainly composed of water, the above-described liquid repellency can be more suitably exhibited, and the above effects are more remarkable. Appears as something. Examples of the hydrophobic treatment method include formation of a film made of a hydrophobic material (for example, the above-described material having liquid repellency).

The housing 31 may be connected to voltage application means 8 for applying a voltage. By applying a voltage having the same polarity as that of the granular dispersion 6 (toner particles 9) to the inner surface side of the housing 31 by the voltage application means 8, the following effects can be obtained.
Usually, the toner particles are positively or negatively charged. For this reason, when there is a charged substance charged with a polarity different from that of the toner particles, a phenomenon occurs in which the toner particles are electrostatically attracted and attached to the charged substance. On the other hand, if there is a charged material charged to the same polarity as the toner particles, the charged material and the toner particles repel each other, and the phenomenon that the toner adheres to the surface of the charged material can be effectively prevented. Therefore, by applying a voltage having the same polarity as that of the granular dispersion liquid 6 (toner particles 9) to the inner surface side of the housing 31, it is effective that the dispersion liquid 6 (toner particles 9) adhere to the inner surface of the housing 31. Can be prevented. As a result, the generation of irregularly shaped toner powder can be more effectively prevented, and the collection efficiency of the toner particles 9 can be improved. In particular, when used in combination with the above-described liquid repellent treatment (hydrophobization treatment), the effect can be further enhanced.

Further, in the illustrated configuration, the toner manufacturing apparatus 1 has an air intake unit 12. A gas flow can be formed in the transport unit 3 by the intake means 12. As a result, the finely divided dispersion liquid 6 (toner particles 9) can be smoothly transported in the transport section 3.
In the configuration shown in the figure, the intake means 12 is connected to the housing 31 by a connecting pipe 121. Further, an enlarged diameter portion 122 having an enlarged inner diameter is formed in the vicinity of the end portion of the connection pipe 121 connected to the housing 31, and a filter 123 for preventing the suction of the toner particles 9 and the like is further provided. ing.

As shown in FIG. 1, the toner manufacturing apparatus 1 includes a gas supply unit 10, and the dry gas supplied from the gas supply unit 10 is introduced into the heating region 331 via the duct 101. It is the composition which becomes.
A heat exchanger 11 is attached to the gas supply means 10. Thereby, the temperature of the dry gas injected from the gas injection port 14 can be set to a preferable value, and when the granular dispersion 6 discharged to the transport unit 3 passes through the heating region 331, the dispersion medium is changed. It can be removed efficiently.

  The humidity of the dry gas injected from the gas injection port 14 is, for example, preferably 50% RH or less, more preferably 30% RH or less, and even more preferably 20% RH or less. When the humidity of the dry gas ejected from the gas ejection port 14 is 50% RH or less, the dispersion medium 62 contained in the dispersion 6 can be efficiently removed in the heating region 331 described above, and toner production is performed. The nature is further improved.

  In addition, the temperature of the dry gas injected from the gas injection port 14 varies depending on the composition of the dispersoid 61 and the dispersion medium 62 contained in the dispersion 6, but is preferably 10 to 250 ° C. More preferably, it is -200 degreeC. When the temperature of the dry gas ejected from the gas ejection port 14 is within such a range, the dispersion medium 62 contained in the dispersion 6 can be efficiently dispersed while maintaining the uniformity of the shape of the toner particles 9 obtained. The toner productivity can be made particularly excellent.

Further, when such a gas supply means 10 is provided, the removal rate of the dispersion medium 62 of the dispersion 6 in the heating region 331 can be easily controlled by adjusting the gas supply amount.
Although the shape of the discharge part 23 is not specifically limited, It is preferable that it is a substantially circular shape. Thereby, the circularity of the discharged dispersion liquid 6 and the formed toner particles 9 can be increased. Further, the clogging of the dispersion 6 at the discharge unit 23 can be more reliably prevented.

  When the discharge part 23 is a substantially circular shape, the diameter (nozzle diameter) is preferably 1 to 500 μm, and more preferably 3 to 200 μm, for example. By adopting the configuration of the present invention, it is possible to effectively prevent clogging or the like of the discharge portion 23 even with such a relatively small nozzle diameter. On the other hand, if the diameter of the discharge portion 23 is less than the lower limit value, in order to obtain toner particles 9 having a desired size, the content rate of the toner constituents in the dispersion 6 must be increased. No longer. As a result, depending on the composition of the dispersion 6 and the like, the viscosity of the dispersion 6 may increase, and it may be difficult to discharge the droplet-like dispersion 6. Further, when the diameter of the discharge section 23 is less than the lower limit value, the dispersion 6 is likely to be clogged, and the dispersion of the discharged dispersion 6 may increase in size. The tendency as described above becomes more prominent as the diameter of the discharge section 23 becomes smaller. When the diameter of the discharge portion 23 exceeds the upper limit, depending on the viscosity of the dispersion 6 and the like, the stability of the shape of the discharged droplet-like dispersion 6 is lowered, and finally obtained toner particles 9 also has a large variation in shape, and the circularity tends to decrease. If the opening area of the discharge part 23 exceeds the upper limit, the discharged dispersion liquid 6 may entrap bubbles depending on the force relationship between the negative pressure of the dispersion liquid storage part 21 and the surface tension of the nozzle. There is.

  Further, the vicinity of the discharge portion 23 of the head portion 2 (particularly, the inner surface of the opening of the discharge portion 23 and the surface on the side where the discharge portion 23 of the head portion 2 is provided (the lower surface in the drawing)) are described above. Like the part of the inner wall surface of the housing 31, it is preferable that the dispersion liquid 6 has liquid repellency. Thereby, it can prevent effectively that the dispersion liquid 6 adheres to the discharge part vicinity. As a result, it is possible to effectively prevent a so-called poor liquid runout or a discharge failure of the dispersion 6. Further, by effectively preventing the dispersion liquid 6 from adhering to the vicinity of the discharge portion, the stability of the shape of the discharged droplets is improved (the variation in shape and size between the droplets is small). The variation in the shape and size of the toner particles finally obtained is also reduced.

  Further, the vicinity of the discharge portion 23 of the head portion 2 (particularly, the inner surface of the opening of the discharge portion 23 and the surface on the side where the discharge portion 23 of the head portion 2 is provided (the lower surface in the drawing)) are described above. Like the part of the inner wall surface of the housing 31, it is preferable that the hydrophobic treatment is performed. Thereby, for example, when the dispersion medium 62 of the dispersion 6 is mainly composed of water, the above-described liquid repellency can be more suitably exhibited, and the above effects are more remarkable. Appears as something. Examples of the hydrophobic treatment method include formation of a film made of a hydrophobic material (for example, the above-described material having liquid repellency). By the way, water has a relatively high viscosity among various liquids, but even if such water is used as a constituent material of the dispersion medium 62, the disadvantage is caused by the dispersion 6 adhering to the vicinity of the discharge portion. Is effectively prevented from occurring. Therefore, when the hydrophobic treatment is performed in the vicinity of the discharge portion 23 of the head portion 2, the dispersion liquid 6 substantially not containing or hardly containing an organic solvent can be suitably used. The toner can be produced by a method that hardly causes an adverse effect.

As shown in FIG. 2, the piezoelectric element 22 includes a lower electrode (first electrode) 221, a piezoelectric body 222, and an upper electrode (second electrode) 223 that are stacked in this order. In other words, the piezoelectric element 22 has a configuration in which the piezoelectric body 222 is interposed between the upper electrode 223 and the lower electrode 221.
The piezoelectric element 22 functions as a vibration source, and the diaphragm 24 vibrates due to the vibration of the piezoelectric element (vibration source) 22 and has a function of instantaneously increasing the internal pressure of the dispersion liquid storage unit 21. It is.

  The head unit 2 is in a state where a predetermined ejection signal is not input from a piezoelectric element driving circuit (not shown), that is, a state where no voltage is applied between the lower electrode 221 and the upper electrode 223 of the piezoelectric element 22. Then, the piezoelectric body 222 is not deformed. For this reason, the diaphragm 24 is not deformed and the volume of the dispersion liquid storage unit 21 is not changed. Therefore, the dispersion 6 is not discharged from the discharge unit 23.

  On the other hand, in a state where a predetermined ejection signal is input from the piezoelectric element driving circuit, that is, in a state where a predetermined voltage is applied between the lower electrode 221 and the upper electrode 223 of the piezoelectric element 22, the piezoelectric body 222 is deformed. Arise. As a result, the diaphragm 24 is greatly deflected (bends downward in FIG. 2), and the volume of the dispersion liquid storage unit 21 is reduced (changed). At this time, the pressure in the dispersion liquid storage unit 21 increases instantaneously, and the granular dispersion liquid 6 is discharged from the discharge unit 23.

  When one discharge of the dispersion liquid 6 is completed, the piezoelectric element driving circuit stops applying the voltage between the lower electrode 221 and the upper electrode 223. Thereby, the piezoelectric element 22 returns almost to its original shape, and the volume of the dispersion liquid storage unit 21 increases. At this time, a pressure (pressure in the positive direction) acting from the dispersion liquid supply unit 4 to the discharge unit 23 acts on the dispersion liquid 6. For this reason, air is prevented from entering the dispersion liquid storage part 21 from the discharge part 23, and an amount of the dispersion liquid 6 corresponding to the discharge amount of the dispersion liquid 6 is supplied from the dispersion liquid supply part 4 to the dispersion liquid storage part 21. The

By applying the voltage as described above at a predetermined cycle, the piezoelectric element 22 vibrates and the granular dispersion liquid 6 is repeatedly discharged.
In this way, by performing discharge (injection) of the dispersion liquid 6 with the pressure pulse generated by the vibration of the piezoelectric body 222, the dispersion liquid 6 can be intermittently discharged one by one, and the discharged dispersion liquid 6 can be discharged. The shape of is stable. As a result, resin particles (toner) with small variations in shape and size between the particles (each toner particle) can be obtained, and the produced toner particles can be highly spherical (geometrically). It is relatively easy to achieve a shape close to a perfect sphere.

  Further, by discharging (injecting) the dispersion liquid as described above, the vibration frequency of the piezoelectric body, the opening area (nozzle diameter) of the discharge portion, the temperature / viscosity of the dispersion liquid, the discharge amount of one drop of the dispersion liquid, The content of the dispersoid in the dispersion and the particle size of the dispersoid in the dispersion can be controlled relatively accurately, making it easy to control the toner to be manufactured to the desired shape and size. it can. Further, by controlling these conditions and the like, for example, the production amount of toner and the like can be easily and reliably managed.

Further, by using the vibration of the piezoelectric body for discharging the dispersion liquid, the dispersion liquid can be discharged more reliably at a predetermined interval. For this reason, it can prevent effectively that the granular dispersion liquid discharged collides and aggregates, and can prevent the formation of irregular-shaped powder more effectively.
The piezoelectric element 22 ′ has the same configuration as the piezoelectric element 22. That is, the piezoelectric element 22 ′ is configured by laminating a lower electrode (first electrode) 221 ′, a piezoelectric body 222 ′, and an upper electrode (second electrode) 223 ′ in this order. In other words, the piezoelectric element 22 ′ is configured such that the piezoelectric body 222 ′ is interposed between the upper electrode 223 ′ and the lower electrode 221 ′.

The piezoelectric element 22 ′ functions as a vibration source, and the diaphragm 24 ′ vibrates due to the vibration of the piezoelectric element (vibration source) 22 ′, and instantaneously increases the internal pressure of the wetting liquid reservoir 21 ′. It has a function.
The initial velocity of the dispersion 6 discharged from the head unit 2 to the transport unit 3 is, for example, preferably 0.1 to 10 m / sec, and more preferably 2 to 8 m / sec. When the initial speed of the dispersion liquid 6 is less than the lower limit, the productivity of the toner decreases. On the other hand, when the initial velocity of the dispersion 6 exceeds the upper limit, the sphericity of the toner particles 9 obtained tends to decrease.

  Moreover, the viscosity of the dispersion 6 discharged from the head part 2 is not particularly limited, but is preferably 0.5 to 200 [mPa · s], for example, 1 to 25 [mPa · s]. Is more preferable. When the viscosity of the dispersion liquid 6 is less than the lower limit, it is difficult to sufficiently control the size of the discharged particles (granular dispersion liquid 6), and the variation of the obtained toner particles 9 may increase. is there. On the other hand, when the viscosity of the dispersion 6 exceeds the upper limit, the diameter of the formed particles increases, the discharge speed of the dispersion 6 decreases, and the amount of energy required for discharging the dispersion 6 tends to increase. Show. In addition, when the viscosity of the dispersion liquid 6 is particularly large, the dispersion liquid 6 cannot be discharged as droplets.

Further, the discharge amount of one drop of the dispersion 6 is slightly different depending on the content of the dispersoid 61 in the dispersion 6, but is preferably 0.05 to 500 pl, and more preferably 0.5 to 5 pl. Is more preferable. By setting the discharge amount of one drop of the dispersion 6 within such a range, the toner particles 9 can be made to have an appropriate particle size.
Incidentally, the granular dispersion liquid 6 discharged from the head unit 2 is generally sufficiently larger than the dispersoid 61 in the dispersion liquid 6. That is, a large number of dispersoids 61 are dispersed in the granular dispersion liquid 6. For this reason, even if the dispersion of the particle size of the dispersoid 61 is relatively large, the ratio of the dispersoid 61 in the discharged granular dispersion liquid 6 is almost uniform for each droplet. Therefore, even when the particle size variation of the dispersoid 61 is relatively large, the toner particles 9 have a small particle size variation by making the discharge amount of the dispersion 6 substantially uniform. Such a tendency becomes more remarkable. For example, when the average particle diameter of the discharged dispersion liquid 6 is Dd [μm] and the average particle diameter of the dispersoid 61 in the dispersion liquid 6 is Dm [μm], the relationship of Dm / Dd <0.5 is satisfied. It is preferable to satisfy the relationship of Dm / Dd <0.2.

  Further, when the average particle size of the discharged dispersion 6 is Dd [μm] and the average particle size of the manufactured toner particles is Dt [μm], a relationship of 0.05 ≦ Dt / Dd ≦ 1.0 is established. It is preferable to satisfy, and it is more preferable to satisfy the relationship of 0.1 ≦ Dt / Dd ≦ 0.8. By satisfying such a relationship, it is possible to relatively easily obtain toner particles 9 that are sufficiently fine, have a high degree of circularity, and have a sharp particle size distribution.

  The frequency of the piezoelectric element 22 is not particularly limited, but is preferably 1 kHz to 500 MHz, and more preferably 5 kHz to 200 MHz. When the vibration frequency of the piezoelectric element 22 is less than the lower limit value, toner productivity decreases. On the other hand, when the vibration frequency of the piezoelectric element 22 exceeds the upper limit, the discharge of the granular dispersion liquid 6 cannot follow, and there is a possibility that the dispersion of the size of one drop of the dispersion liquid 6 becomes large.

In the illustrated configuration, the head unit 2 includes a plurality of droplet discharge heads 27 each having a discharge unit 23. And the granular dispersion liquid 6 is each discharged from these discharge parts 23 to the conveyance part 3. FIG.
Each discharge portion 23 may discharge the dispersion liquid 6 almost simultaneously, but it is preferable that at least two adjacent head portions are controlled so that the discharge timing of the dispersion liquid 6 is different. . Thereby, before the granular dispersion liquid 6 discharged from the adjacent head part 2 solidifies, it can prevent more effectively that a granular dispersion liquid collides and aggregates.

  Further, as shown in FIG. 2, the toner manufacturing apparatus 1 has a gas supplied from a gas supply unit (not shown) from each gas ejection port 7 provided between the droplet discharge head 27 and the droplet discharge head 27. In this configuration, injection is performed with a substantially uniform pressure. Such a gas preferably contains the same composition as that of the dispersion medium 62. Thereby, it is possible to more effectively suppress the dispersion medium 62 from voluntarily evaporating from the dispersion liquid 6 in the vicinity of the head portion 2, and to more reliably prevent various problems such as clogging. . Thereby, the dispersion liquid 6 can be conveyed and solidified while maintaining the interval of the granular dispersion liquid 6 intermittently ejected from the ejection section 23. As a result, collision and aggregation between the discharged granular dispersions 6 are more effectively prevented.

Further, by injecting the gas from the gas injection port 7, it is possible to form a gas flow that flows in substantially one direction (downward in the drawing) in the transport unit 3. When such a gas flow is formed, the granular dispersion 6 (toner particles 9) in the transport unit 3 can be transported more efficiently.
In addition, an air current curtain is formed between particles ejected from each head unit 2 by ejecting gas from the gas ejection port 7, for example, a collision between particles ejected from adjacent head units, Aggregation can be prevented more effectively.

  The content of the dispersion medium in the gas injected from the gas injection port 7 is not particularly limited. For example, the humidity of the gas when water containing water is used as the dispersion medium is 60% RH or more. Preferably, it is 70% RH or more. Thereby, it is possible to more effectively suppress the dispersion medium 62 from being voluntarily evaporated from the dispersion liquid 6 in the vicinity of the head portion 2.

  In addition, the toner manufacturing apparatus 1 includes a flow rate sensor 16 that measures the flow rate of the gas in the transport unit 3 and a gas flow control unit 15 that is electrically connected to the flow rate sensor 16 as illustrated in the drawing. is doing. The gas flow control means 15 is also electrically connected to the above-described gas supply means and the like, and by controlling each gas supply means based on the measurement result of the flow rate sensor 16, the granularity in the transport unit 3 is controlled. The dispersion liquid 6 (toner particles 9) can be conveyed more efficiently.

The granular dispersion 6 discharged from the head unit 2 becomes toner particles 9 by being solidified while being transported by the transport unit 3. Then, the toner particles 9 are collected by the collection unit 5.
As described above, the toner particles 9 are obtained by removing the dispersion medium 62 from the discharged granular dispersion liquid 6. In such a case, the dispersoid 61 contained in the dispersion 6 aggregates as the dispersion medium 62 in the discharged dispersion 6 is removed. As a result, the toner particles 9 are obtained as an aggregate of the dispersoid 61. In addition, when the above-mentioned solvent is contained in the dispersoid 61, the said solvent is also normally removed in the heating area | region 331.

The particle size of the dispersoid 61 contained in the dispersion liquid 6 is usually sufficiently smaller than the obtained toner particles 9 (the granular dispersion liquid 6 to be discharged). Therefore, the toner particles 9 obtained as an aggregate of the dispersoid 61 have a sufficiently large circularity.
Further, when the toner particles 9 are obtained by removing the dispersion medium 62, the obtained toner particles 9 are usually smaller than the dispersion liquid 6 discharged from the discharge unit 23. For this reason, even when the area (opening area) of the discharge portion 23 is relatively large, the size of the toner particles 9 obtained can be made relatively small. Therefore, in the present invention, sufficiently fine toner particles 9 are obtained even if the head portion 2 is not obtained by performing special precision processing (even if it can be manufactured relatively easily). be able to.

Further, as described above, since the area of the discharge section 23 does not need to be extremely small, the particle size distribution of the dispersion 6 discharged from each head section 2 is made sufficiently sharp. be able to. As a result, the toner particles 9 also have a small variation in particle size, that is, a sharp particle size distribution.
In the above description, the dispersion medium 62 is removed from the dispersion liquid 6 in the transport unit 3 (heating region 331), so that the dispersoid 61 in the granular dispersion liquid 6 aggregates (fuses), and the toner particles. However, the toner particles are not limited to those obtained in this way. For example, when the dispersoid 61 contains a precursor of a resin material (for example, a monomer, dimer, oligomer, or the like corresponding to the resin material), the toner particles 9 are obtained by advancing a polymerization reaction in the transport unit 3. Such a method may be used.

  The toner obtained as described above may be subjected to various kinds of treatment such as heat treatment as necessary. Thereby, the joining of the fine particles derived from the dispersoid constituting the toner particles 9 is advanced, and the mechanical strength (mechanical stability) of the toner particles 9 can be further improved. Further, by performing such a heat treatment, the circularity of the toner particles 9 can be made particularly large.

In addition, the toner as described above may be subjected to various processes such as a classification process and an external addition process as necessary.
For the classification treatment, for example, a sieve, an airflow classifier or the like can be used.
Examples of the external additive used for the external addition treatment include metal oxides such as silica, aluminum oxide, titanium oxide, strontium titanate, cerium oxide, magnesium oxide, chromium oxide, titania, zinc oxide, alumina, and magnetite. Fine particles composed of inorganic materials such as nitrides such as silicon nitride, carbides such as silicon carbide, calcium sulfate, calcium carbonate, aliphatic metal salts, acrylic resins, fluororesins, polystyrene resins, polyester resins, aliphatic metal salts Fine particles composed of organic materials such as these, and fine particles composed of a composite of these.

As the external additive, the surface of the fine particles as described above is subjected to a surface treatment with HMDS, a silane coupling agent, a titanate coupling agent, a fluorine-containing silane coupling agent, silicone oil or the like. It may be used.
The toner of the present invention produced as described above has a uniform shape and a sharp particle size distribution (small width).

Specifically, the toner (toner particles) preferably has an average circularity R represented by the following formula (I) of 0.96 or more, more preferably 0.97 or more, and 0.98. The above is more preferable. When the average circularity R is 0.96 or more, the toner transfer efficiency is further improved.
R = L ₀ / L ₁ (I)
(Where, L ₁ [μm] is the circumference of the projected image of the toner particles to be measured, and L ₀ [μm] is a perfect circle having an area equal to the area of the projected image of the toner particles to be measured (completely (Represents the perimeter of a geometric circle)

In addition, the toner preferably has a standard deviation of average circularity between particles of 0.015 or less, and more preferably 0.01 or less. When the standard deviation of the average circularity between the particles is 0.015 or less, variations such as charging characteristics and fixing characteristics are particularly reduced, and the reliability of the entire toner is further improved.
The volume-based average particle diameter of the toner obtained as described above is preferably 2 to 20 μm, and more preferably 4 to 10 μm. When the average particle size of the toner is less than the lower limit, it becomes difficult to uniformly charge, and the adhesion force to the surface of the electrostatic latent image carrier (for example, a photoreceptor) increases. As a result, There may be an increase in the residual toner. On the other hand, when the average particle size of the toner exceeds the upper limit, the reproducibility of the contour portion of an image formed using the toner, particularly a character image or a light pattern, tends to be lowered.
Further, the toner preferably has a standard deviation of the particle diameter between the particles of 1.3 μm or less, and more preferably 1.0 μm or less. When the standard deviation of the particle diameter between the particles is 1.3 μm or less, the variation in charging characteristics, fixing characteristics and the like is particularly small, and the reliability of the entire toner is further improved.

Next, a second embodiment of the present invention will be described. Hereinafter, the present embodiment will be described with a focus on differences from the above-described embodiments, and description of similar matters will be omitted.
FIG. 3 is a longitudinal sectional view schematically showing a second embodiment of the fine particle production apparatus of the present invention, and FIG. 4 is a sectional view taken along line XX in FIG.
As shown in FIG. 3, the toner manufacturing apparatus (fine particle manufacturing apparatus) 1 includes a wetting liquid spraying means 18 provided in the vicinity of the head portion 2, a cooling means 32 ′ provided in the head portion 2, and a housing 31. Except having the provided cooling means 34 and the dispersion medium collection | recovery part 35, it is the structure similar to 1st Embodiment mentioned above.

The wetting liquid spraying means (wetting means) 18 includes a wetting liquid storing section 181 that stores the wetting liquid 62 ′, an injection port 182 that sprays (discharges) the wetting liquid 62 ′ in an area near the head section 2, and a wetting liquid. A supply pipe 183 is connected to the reservoir 181 and supplies the wetting liquid 62 ′ to the injection port 182.
In the configuration shown in the drawing, the wetting liquid spraying means 18 sprays (discharges) the wetting liquid 62 ′ in a direction perpendicular to the discharge direction of the dispersion 6 discharged from the head unit 2.

In this way, by spraying the wetting liquid 62 ′ on the area near the head portion 2, the concentration of the wetting liquid 62 ′ can be made higher in the area near the head portion 2. As a result, the evaporation (volatilization) of the unintentional dispersion medium 62 from the dispersion liquid 6 in the vicinity of the head unit 2 can be more effectively suppressed, and problems such as clogging can be prevented more reliably. .
The wetting liquid 62 ′ is sprayed (discharged) so as not to hit the discharged dispersion liquid 6. For example, spraying may be performed between the plurality of dispersions 6 to be transported, or spraying may be performed while being shifted from the discharge timing of the dispersions 6.

  The cooling means 32 ′ is configured to cool the vicinity of the head portion 2 in the above-described embodiment, whereas in the present embodiment, the cooling means 32 ′ is configured to cool a region including the head portion 2. Thereby, since the dispersion liquid 6 can be discharged at a lower temperature, the evaporation (removal) of the unintentional dispersion medium 62 from the dispersion liquid 6 is more effectively suppressed in the vicinity of the head portion 2, Various problems such as clogging can be prevented more reliably.

As shown in FIG. 4, the cooling means 34 is provided at a part of the outer periphery of the housing 31.
The cooling means 34 has a function of selectively condensing (condensing) the dispersion medium 62 evaporated and vaporized from the dispersion 6 in the cooled portion by cooling a part of the housing 31. .
Further, the dispersion medium recovery unit 35 has a function of recovering the dispersion medium 62 condensed (condensed) by the cooling means 34.

  By the way, when the toner is continuously manufactured, the concentration of the dispersion medium 62 evaporated and vaporized from the dispersion 6 gradually increases in the transport unit 3 and the dispersion medium 62 may not be sufficiently removed. However, by collecting the dispersion medium 62 removed from the dispersion 6 while condensing it as in the present embodiment, it is possible to prevent the concentration of the evaporated dispersion medium 62 from increasing in the transport unit 3. The dispersion medium 62 can be more efficiently removed from the dispersion 6. As a result, it is possible to more effectively prevent the dispersion medium 62 from remaining in the manufactured toner.

In particular, when the inner wall surface of the housing 31 has liquid repellency as in the first embodiment described above, the condensed dispersion medium 62 flows downward in the housing 31 in the cooled portion of the housing 31. It becomes easy to go and can be more easily recovered in the dispersion medium recovery unit 35.
Further, by recovering the evaporated and vaporized dispersion medium 62 in this way, it is possible to sufficiently suppress the evaporated and vaporized dispersion medium 62 from being released to the outside of the apparatus, which is good for the environment.
In the configuration shown in the figure, the transport unit 3 is composed of the cooling region 321, the heating region 331, and other regions, but is not limited to this, and at least the cooling region 321 and the heating region are configured. What is comprised with the area | region 331 may be sufficient.

Next, a third embodiment of the present invention will be described. Hereinafter, the present embodiment will be described with a focus on differences from the above-described embodiments, and description of similar matters will be omitted.
The toner manufacturing apparatus 1 of the present embodiment has the same configuration as that of the second embodiment except that the configuration of the head unit is different.
FIG. 5 is a diagram schematically illustrating a structure in the vicinity of the head portion of the toner manufacturing apparatus according to the third embodiment.
As shown in FIG. 5, the toner manufacturing apparatus 1 of the present embodiment includes a head unit 28 having a plurality of head portions 2.

Each head portion 2 is partitioned by a partition wall 17 having a predetermined length in the discharge direction of the dispersion liquid 6. Thereby, the region 36 (region in the vicinity of the head unit 2) surrounded by the partition wall 17 is not easily affected by the temperature, gas flow, or the like of other regions.
The partition wall 17 includes an injection port 172 that sprays the wetting liquid 62 ′ on the region 36, and a supply pipe 171 that communicates with the injection port 172 and supplies the wetting liquid 62 ′ to the injection port 172 from a not-shown wetting liquid reservoir. have.
That is, in this embodiment, the partition wall 17 is provided with a wetting means.

The region 36 is a relatively narrow region, and therefore is not easily affected by the temperature and gas flow of other regions. Therefore, when the wetting liquid 62 ′ is sprayed toward the region 36 in this way, it is possible to easily maintain a high concentration (saturated state) of the wetting liquid 62 ′ in the region near the head portion 2. Thereby, the evaporation (volatilization) of the unintentional dispersion medium 62 from the dispersion liquid 6 in the vicinity of the head unit 2 can be more effectively suppressed, and problems such as clogging can be prevented more reliably. .
Note that the wetting liquid 62 ′ is sprayed between the plurality of dispersed liquids 6 so that the sprayed wetting liquid 62 ′ does not hit the discharged dispersion liquid 6.

Next, a fourth embodiment of the present invention will be described. Hereinafter, the present embodiment will be described with a focus on differences from the above-described embodiments, and description of similar matters will be omitted.
The toner manufacturing apparatus 1 of the present embodiment has the same configuration as that of the second embodiment except that the configuration of the wetting unit is different.
As shown in FIG. 6, the toner manufacturing apparatus 1 is provided with a wiping unit (wiping member) 19 for wiping the surface 29 on the ejection unit 23 side of the head unit 2 as a wetting unit.

The wiping means 19 includes a wiping head 191 and an operation unit 192.
The wiping head 191 contacts the surface 29 and is impregnated with the wetting liquid 62 ′.
The wiping means 19 operates the operation unit 192 to move the wiping head 191 on the surface 29 to wet the discharge unit 23 side of the head unit 2. At this time, it is possible to move the wiping head 191 in accordance with the discharge timing of the dispersion 6 and wipe it.
By adopting such a configuration, the evaporation (volatilization) of the unintentional dispersion medium 62 from the dispersion liquid 6 in the vicinity of the head unit 2 is more effectively suppressed, and clogging and the like are more reliably prevented. be able to.

Next, a fifth embodiment of the present invention will be described. Hereinafter, the present embodiment will be described with a focus on differences from the above-described embodiments, and description of similar matters will be omitted.
The toner manufacturing apparatus of this embodiment has the same configuration as that of the second embodiment except that the configuration of the head unit is different.
FIG. 7 is a diagram schematically illustrating a structure in the vicinity of the head portion of the toner manufacturing apparatus according to the fifth embodiment.

  As shown in FIG. 7, in the toner manufacturing apparatus 1 of the present embodiment, an acoustic lens (concave lens) 25 is installed in the head unit 2. By installing such an acoustic lens 25, for example, the pressure pulse (vibration energy) generated by the piezoelectric element 22 can be converged by the pressure pulse converging unit 26 in the vicinity of the ejection unit 23. As a result, vibration energy generated by the piezoelectric element 22 can be efficiently used as energy for discharging the dispersion liquid 6. Therefore, even if the dispersion liquid 6 stored in the dispersion liquid storage unit 21 has a relatively high viscosity, it can be reliably discharged from the discharge unit 23. In addition, even if the dispersion 6 stored in the dispersion storage unit 21 has a relatively large cohesive force (surface tension), it can be discharged as fine droplets. The particle diameter of the toner particles 9 can be controlled to a relatively small value.

Further, since the pressure pulse can be converged by the pressure pulse converging unit 26 in the vicinity of the ejection unit 23, even if the ejection unit 23 is likely to be blocked by evaporation of the dispersion medium 62 or the like, The attached deposit can be forced out. As a result, clogging and the like can be prevented more reliably.
As described above, in this embodiment, the toner particles 9 can be controlled to have a desired shape and size even when a material having a higher viscosity or a material having a high cohesive force is used as the dispersion liquid 6. Therefore, the range of material selection is particularly wide, and a toner having desired characteristics can be obtained more easily.

  In the present embodiment, since the dispersion liquid 6 is ejected by the converged pressure pulse, the size of the dispersion liquid 6 to be ejected is relatively large even when the area (opening area) of the ejection portion 23 is relatively large. Can be small. That is, even when it is desired to make the particle size of the toner particles 9 relatively small, the area of the discharge portion 23 can be increased. Thereby, even if the dispersion liquid 6 has a relatively high viscosity, the occurrence of clogging or the like in the discharge unit 23 can be more effectively prevented.

As mentioned above, although this invention was demonstrated based on suitable embodiment, this invention is not limited to this.
For example, each part constituting the fine particle production apparatus of the present invention can be replaced with any one that exhibits the same function, or other structures can be added.
In the above-described embodiment, the case where a part of a plurality of discharge units is used as the wetting unit has been described. However, the present invention is not limited to this, and a wet liquid jet nozzle or the like is provided between the plurality of discharge units. The above-described gas injection port 7 may be used for the wetting liquid injection.

In the above-described embodiment, the case where the fine particle manufacturing apparatus is applied to a toner manufacturing apparatus has been described. However, the present invention is not limited to toner, and can be applied to resin fine particles in general. Moreover, you may apply to manufacture of inorganic fine particles.
In the above-described embodiment, the case where the dispersion liquid 6 is discharged vertically downward has been described. However, the present invention is not limited to this. For example, as shown in FIG. 8, the dispersion liquid 6 is discharged vertically upward. It may be a thing. Thus, by discharging the dispersion liquid 6 vertically upward, the concentration of the dispersion medium 62 (wetting liquid 62 ′) in the vicinity of the head portion 2 can be made high, and as a result, clogging is more reliably performed. Etc. can be prevented.

In the above-described embodiment, some examples of the wetting means are described, but these wetting means may be used in combination.
In the above-described embodiment, the configuration in which the cooling region 321 and the heating region 331 are adjacent to each other has been described. However, the cooling region 321 and the heating region 331 may be separated from each other.
In the above-described embodiment, the cooling unit 32 ′ is described as cooling the region including the head unit 2. However, the cooling unit 32 ′ is provided separately for cooling the head unit 2 and for forming the cooling region 321. It may be a thing.

In the above-described embodiment, the case where the cooling unit 34 for cooling the housing 31 is provided on a part of the peripheral surface of the housing 31 has been described. However, the cooling unit 34 may be provided over the peripheral surface.
Further, in the above-described embodiment, it has been described that the evaporation of the dispersion medium is controlled by the temperature difference, but a pressure difference may be provided. For example, by configuring the pressure in the vicinity of the head portion to be high and the pressure in the heating region to be low, evaporation of the dispersion medium in the vicinity of the head portion can be suppressed, and the transport of the discharged dispersion liquid is also efficient. Can be done well.

In the above-described embodiment, the configuration using the concave lens as the acoustic lens has been described. However, the acoustic lens is not limited to this. For example, a Fresnel lens, an electronic scanning lens, or the like may be used as the acoustic lens.
Furthermore, in the above-described embodiment, the configuration in which only the dispersion liquid 6 is interposed between the acoustic lens 25 and the ejection unit 23 has been described. For example, as illustrated in FIGS. Between the discharge part 23, the throttle member 13 having a converging shape may be disposed toward the discharge part 23. Thereby, convergence of the pressure pulse (vibration energy) generated by the piezoelectric element 22 can be assisted, and the pressure pulse generated by the piezoelectric element 22 can be used more efficiently.

In the above-described embodiment, the toner component is described as a solid component contained in the dispersoid. However, at least a part of the toner component may be contained in the dispersion medium.
Moreover, although it demonstrated as what wiped off discharging a dispersion liquid in embodiment mentioned above, you may stop and wipe off.

  In the above-described embodiment, the dispersion liquid is intermittently ejected from the head portion by the piezoelectric pulse. However, other methods can be used as a dispersion liquid ejection method (injection method). For example, as a method for discharging (injecting) the dispersion liquid, a method such as a spray drying method or a so-called bubble jet (“Bubble Jet” is a registered trademark) method is used. A method of injecting a dispersion liquid in the form of droplets (as fine particles) using a nozzle that draws the thin layer flow into a thin laminar flow and injects the thin laminar flow away from the smooth surface as fine particles (Japanese Patent Application 2002-2002) The method as described in the specification of US Pat. No. 3,218,89) may be used. The spray drying method is a method of obtaining liquid droplets by spraying (spraying) a liquid (dispersion) using a high-pressure gas. Moreover, as a method to which a so-called bubble jet (“bubble jet” is a registered trademark) method is applied, a method described in the specification of Japanese Patent Application No. 2002-169348 can be cited. That is, as a method for ejecting (injecting) the dispersion liquid, a “method for intermittently ejecting the dispersion liquid from the head portion by a change in gas volume” can be applied.

[1] Production of toner particles (resin fine particles) (Example 1)
First, polyester resin as a binder resin (glass transition point Tg: 53 ° C., softening point Tf _1/2 : 105 ° C., weight average molecular weight Mw: 13000): 100 parts by weight, phthalocyanine pigment (manufactured by Dainichi Seika Co., Ltd.) as a colorant Phthalocyanine blue): 5 parts by weight, Cr-salicylic acid complex as a charge control agent (Bontron E-81, manufactured by Orient Chemical Industries): 1 part by weight, carnauba wax as wax: 3 parts by weight, tetrahydrofuran as a solvent (Wako Pure Chemicals) 300 parts by weight were prepared.
These components were mixed and dispersed with a ball mill for 10 hours to prepare a binder resin solution (resin solution).

On the other hand, an aqueous solution (aqueous solution) prepared by dissolving 10 parts by weight of sodium polyacrylate as a dispersant (manufactured by Wako Pure Chemical Industries, average polymerization degree n = 2700-7500) in 590 parts by weight of ion-exchanged water was prepared.
Next, 600 parts by weight of this aqueous solution is placed in a 3 liter round bottom stainless steel container, and a binder resin solution: 409 weights while stirring at a rotation speed of 4000 rpm using a TK homomixer (manufactured by Tokki Kako). The portion was gradually added dropwise over 10 minutes. At this time, the liquid temperature was kept at 70 ° C. The emulsion was further stirred for 10 minutes while maintaining the liquid temperature at 70 ° C. after the completion of the dropwise addition of the binder resin solution.

Next, under conditions of temperature: 45 ° C. and atmospheric pressure: 10 to 20 kPa, tetrahydrofuran in the emulsion (dispersoid) is removed, then cooled to room temperature, and further ion-exchanged water is added to form a solid. A binder resin suspension (dispersion) in which fine particles were dispersed was obtained.
Thereafter, the obtained binder resin suspension (dispersion) was degassed. The deaeration treatment was performed by placing the binder resin suspension (dispersion) in a stirred state in an atmosphere of 14 kPa for 10 minutes. The ambient temperature during the deaeration treatment was 25 ° C. The solid content (dispersoid) concentration in the binder resin suspension (dispersion) thus obtained was 10 wt%. The viscosity of the binder resin suspension (dispersion) at 25 ° C. was 2 mPa · s. Moreover, the average particle diameter Dm of the dispersoid constituting the binder resin suspension was 0.4 μm. The average particle size of the dispersoid was measured using a laser diffraction / scattering particle size distribution analyzer (LA-920, manufactured by Horiba, Ltd.).

  The degassed dispersion (binder resin suspension) was charged into the dispersion supply unit 4 of the toner manufacturing apparatus 1 as shown in FIGS. While the dispersion liquid in the dispersion liquid supply unit 4 was agitated by the agitation means 41, it was supplied to the dispersion liquid storage part 21 of the head part by the metering pump, and was discharged from the discharge part 23 to the transport part 3. The discharge part 23 shall have a circular shape with a diameter of 26 μm. Moreover, as the head part 2, the thing near which the hydrophobization process by the fluororesin (polytetrafluoroethylene) coating was performed in the discharge part 23 vicinity was used.

  At the time of discharging the dispersion liquid, the temperature of the dispersion liquid in the head unit 2 is 25 ° C., the frequency of the piezoelectric body is 10 kHz, the initial speed of the dispersion liquid discharged from the discharge unit 23 is 4 m / second, and the head part is discharged. It was performed in a state where the discharge amount for one drop of the dispersion was adjusted to 3 pl (particle diameter Dd: 18 μm, weight: about 3 ng). Further, the dispersion liquid was discharged so that the discharge timing of the dispersion liquid was shifted in at least adjacent head parts among the plurality of head parts. Further, among the plurality of discharge units, the ratio of the discharge unit 23 ′ that discharges the wetting liquid 62 ′ was 4%. Note that ion-exchanged water was used as the wetting liquid 62 '.

The dispersion was discharged in a state where the temperature of the cooling region 321 was 15 ° C., the temperature of the heating region 331 was 65 ° C., the length of the cooling region 321 was 10 cm, and the length of the heating region 331 was 30 cm.
At the time of discharging the dispersion, air having a temperature of 55 ° C., humidity of 27% RH, and a flow rate of 4 m / second is introduced into the heating region from the gas injection port 14, and the temperature: 10 ° C. from the gas injection port 7. , Humidity: 70% RH, flow rate: 4 m / sec. At this time, the pressure in the housing 31 (atmospheric pressure) was adjusted to atmospheric pressure by adjusting each gas supply unit and the intake unit 12.

In the transport unit 3, the dispersion medium was removed from the discharged dispersion, and particles as an aggregate of dispersoids were formed.
The particles formed in the transport unit 3 were collected with a cyclone. The recovered particles (toner particles) had an average circularity R of 0.974 and a circularity standard deviation of 0.012. The weight-based average particle diameter Dt was 6.4 μm. The particle size standard deviation based on weight was 0.8 μm. Further, the water content of the collected particles was 8 wt%. Then, it dried using the fluid-type dryer and made the water content 0.5 wt%. The circularity was measured in a water dispersion system using a flow particle image analyzer (manufactured by Toa Medical Electronics Co., Ltd., FPIA-2000). However, the circularity R is represented by the following formula (I).
R = L ₀ / L ₁ (I)
(Wherein, L ₁ [μm] is the circumference of the projected image of the particle to be measured, and L ₀ [μm] is the circumference of a perfect circle having an area equal to the area of the projected image of the particle to be measured. To express.)

(Example 2)
Toner particles were manufactured in the same manner as in Example 1 except that the toner manufacturing apparatus 1 shown in FIGS. 2 and 3 was used and the temperature of the cooling region 321 was set to 10 ° C. The water content of the collected particles was 7 wt%. The cooling by the cooling means 34 was set to 10 ° C.

Example 3
Toner particles were produced in the same manner as in Example 2 except that the head unit and the wetting means of the toner production apparatus shown in FIG. 3 were the same as those shown in FIG. In addition, ion-exchange water was used as the wetting liquid, and sprayed at a temperature of 15 ° C. and an injection speed of 0.5 m / second from an injection port 172.
(Examples 4 and 5)
Except that the temperature of the cooling region 321, the length of the cooling region 321, the temperature of the heating region 331, and the length of the heating region 331 at the time of discharging the dispersion liquid are as shown in Table 1, the same as in Example 3 above. Thus, toner particles were produced.

(Example 6)
Toner particles were produced in the same manner as in Example 3 except that the toner production apparatus 1 shown in FIG. 6 was used.
(Example 7)
Except that the temperature of the cooling region 321, the length of the cooling region 321, the temperature of the heating region 331, and the length of the heating region 331 at the time of discharging the dispersion liquid are as shown in Table 1, the same as in Example 6 above. Thus, toner particles were produced.

(Comparative Example 1)
A toner was produced in the same manner as in Example 1 except that the wetting means and the cooling area were not provided.
(Comparative Example 2)
First, polyester resin as a binder resin (glass transition point Tg: 53 ° C., softening point Tf _1/2 : 105 ° C., weight average molecular weight Mw: 13000): 100 parts by weight, phthalocyanine pigment (manufactured by Dainichi Seika Co., Ltd.) as a colorant Phthalocyanine blue): 5 parts by weight, a salicylic acid Cr complex (Bontron E-81, manufactured by Orient Chemical Co., Ltd.): 1 part by weight as a charge control agent, and 3 parts by weight of carnauba wax as a wax.
These components were mixed using a 20 L type Henschel mixer to obtain a raw material for preparing a kneaded product.

Next, this raw material (mixture) was kneaded using a twin-screw kneading extruder.
Next, the obtained kneaded material was coarsely pulverized to obtain a powder having an average particle size of 1.5 mm. A hammer mill was used for coarse pulverization of the kneaded product.
Next, the coarsely pulverized kneaded product was finely pulverized. A jet mill (200 AFG, manufactured by Hosokawa Micron Corporation) was used for finely pulverizing the kneaded product. The fine pulverization was performed at a pulverization air pressure: 500 [kPa] and a rotor rotational speed: 7000 [rpm].

The pulverized material thus obtained was classified with an airflow diverter (manufactured by Hosokawa Micron Corporation, 100 ATP).
Thereafter, the classified pulverized product (powder for toner production) was subjected to a thermal spheronization treatment. The thermal spheronization treatment was performed using a thermal spheronization apparatus (Nippon Pneumatic Co., Ltd., SFS3 type). The temperature of the atmosphere during the heat spheronization treatment was 270 ° C.
Thus, toner particles were obtained.
Table 1 shows the toner particle production conditions for each of the above Examples and Comparative Examples.
Table 1 also shows whether or not the ejection unit was clogged after operating continuously for 3 hours in the toner production apparatuses used in the examples and comparative examples.

[2] Evaluation Hydrophobic silica (manufactured by Nippon Aerosil Co., Ltd., R-972): 1.0 part by weight is added to 100 parts by weight of the toner particles obtained in the above Examples and Comparative Examples, and the final toner is prepared. Obtained. Each toner thus obtained was evaluated for durability and transfer efficiency.
[2.1] Durability The toner obtained in each of the above Examples and Comparative Examples was set in a developing machine of a color laser printer (manufactured by Seiko Epson Corporation: LP-2000C). Thereafter, the developing machine was continuously rotated so as not to print. After 12 hours, the developing machine was taken out, the uniformity of the toner thin layer on the developing roller was visually confirmed, and evaluated according to the following four criteria.
A: No disturbance is observed in the thin layer.
○: Disturbance is hardly observed in the thin layer.
Δ: Some disturbance is observed in the thin layer.
X: Streaky disturbance is clearly observed in the thin layer.

[2.2] Transfer efficiency Transfer efficiency of each toner obtained as described above was evaluated.
The transfer efficiency was evaluated as follows using a color laser printer (manufactured by Seiko Epson Corporation, LP-2000C).
The toner on the photoconductor immediately after the development process to the photoconductor (before transfer) and the toner on the photoconductor after transfer (after printing) were collected using different tapes, and their weights were measured. When the toner weight on the photoconductor before transfer is W _b [g] and the toner weight on the photoconductor after transfer is W _a [g], it is obtained as (W _b −W _a ) × 100 / W _b. The value was defined as transfer efficiency.

  Based on these results, the average circularity R, circularity standard deviation, weight-based average particle diameter Dt, particle diameter of particles (toner mother particles, toner particles before adding silica) manufactured using a toner manufacturing apparatus Table 2 shows the standard deviation, the average circularity R of the finally obtained toner, the circularity standard deviation, the weight-based average particle diameter Dt, and the particle diameter standard deviation. The average circularity R, the circularity standard deviation, the weight average particle diameter Dt, and the particle diameter standard deviation for the toners of Examples and Comparative Examples 1 were obtained by continuously operating the toner manufacturing apparatus for 10 hours. The numerical value of is shown.

As is clear from Table 2, the toners of the present invention (Examples 1 to 7) all had a large degree of circularity and a small width of the particle size distribution. Moreover, the variation in shape (standard deviation of circularity) was also small.
On the other hand, the toner of Comparative Example 1 has a small circularity, and the width of the particle size distribution is larger than that of the Example. This is because the wetting means and the cooling area are not provided, so that the drying of the dispersion liquid in the vicinity of the discharge part of the head part cannot be sufficiently suppressed, and the discharge part is clogged. it is conceivable that.

Further, the toner of Comparative Example 2 has a particularly small circularity, and many toner particles having relatively large convex portions were observed.
Further, as apparent from Table 2, the toner of the present invention was excellent in transfer efficiency. In contrast, the toner of the comparative example was inferior in transfer efficiency. This is because the toner of the comparative example has a large variation in shape, size, and characteristics among the particles, whereas the toner of the present invention has a variation in shape, size, and characteristics between the toner particles. This is probably due to being small enough. Further, the toner of the present invention had excellent durability, while the toner of the comparative example was inferior in durability.

In addition, after the toner was produced for 3 hours continuously, the discharge of the dispersion liquid was stopped for 3 hours. As a result, the toner obtained by the toner production apparatus of Comparative Example 1 had a variation in the shape and size between the particles. Was recognized. Further, when stopped for 24 hours, the toner production apparatus of Comparative Example 1 was unable to discharge.
In addition, as a result of manufacturing the toner in the same manner as described above using the toner manufacturing apparatus shown in FIGS. 7 to 11, the same result was obtained.

1 is a longitudinal sectional view schematically showing a first embodiment of a toner manufacturing apparatus of the present invention. FIG. 2 is an enlarged cross-sectional view of the vicinity of a head portion of the toner manufacturing apparatus shown in FIG. 1. FIG. 6 is a longitudinal sectional view schematically showing a second embodiment of the toner manufacturing apparatus of the present invention. It is sectional drawing in the XX line in FIG. FIG. 10 is a diagram schematically illustrating a structure near a head portion of a toner manufacturing apparatus according to a third embodiment. It is a longitudinal cross-sectional view which shows typically 4th Embodiment of the toner manufacturing apparatus of this invention. It is a figure which shows typically the structure of the head part vicinity of the toner manufacturing apparatus of 4th Embodiment. It is a figure which shows typically the structure of the toner manufacturing apparatus of other embodiment. It is a figure which shows typically the structure of the head part vicinity of the toner manufacturing apparatus of other embodiment. It is a figure which shows typically the structure of the head part vicinity of the toner manufacturing apparatus of other embodiment. It is a figure which shows typically the structure of the head part vicinity of the toner manufacturing apparatus of other embodiment.

Explanation of symbols

  DESCRIPTION OF SYMBOLS 1 ... Toner manufacturing apparatus 2 ... Head part 21 ... Dispersion liquid storage part 21 '... Wetting liquid storage part 22, 22' ... Piezoelectric element 221, 221 '... Lower electrode 222, 222' ... Piezoelectric body 223, 223 ′ …… Upper electrode 23, 23 ′ …… Discharge portion 24, 24 ′ …… Vibration plate 25 …… Acoustic lens 26 …… Pressure pulse converging portion 27, 27 ′ …… Droplet discharge head 28 …… Head Unit 3... Conveying section 31... Housing 32, 32 ′ Cooling means 321... Cooling area 33... Heating means 331 ... Heating area 34 ... Cooling means 35 ... Dispersing medium recovery section 36. …… Dispersion supply unit 41 …… Agitating means 5 …… Recovery unit 6 …… Dispersion 61 …… Dispersoid 62 …… Dispersion medium 62 ′ …… Liquid (wetting liquid) 7 …… Gas injection port 8 …… Voltage Application means 9 …… Toner particles 10 ...... Gas supply means 101 …… Duct 11 …… Heat exchanger 12 …… Intake means 121 …… Connecting pipe 122 …… Expanded diameter part 123 …… Filter 13 …… Restriction member 14 …… Gas injection port 15 ...... Gas flow control means 16 ...... Flow rate sensor 17 ...... Partition wall 171 ...... Supply pipe 172 ...... Injection port 18. ... Wiping means 191 ... Wiping head

Claims (33)

A production apparatus for producing fine particles using a dispersion in which a dispersoid containing a raw material for producing fine particles is finely dispersed in a dispersion medium,
A head unit including a discharge unit that discharges the dispersion liquid, and a transport unit that transports the dispersion liquid discharged from the head unit,
An apparatus for producing fine particles, comprising a wetting means for wetting the ejection unit side of the head unit.   2. The fine particle production according to claim 1, wherein the wet means for spraying a liquid that is mainly composed of a constituent material of the dispersion medium and does not contain the dispersoid is provided in a region in the vicinity of the discharge unit. apparatus.   The fine particle manufacturing apparatus according to claim 2, wherein the liquid is sprayed in a direction perpendicular to a discharge direction of the dispersion liquid discharged from the head unit. The head unit includes a plurality of the ejection units,
4. The wet means for discharging a liquid that is mainly composed of a constituent material of the dispersion medium and does not contain the dispersoid is provided between at least the plurality of discharge portions. The fine particle manufacturing apparatus described.   The fine particle manufacturing apparatus according to any one of claims 1 to 4, wherein the dispersion liquid discharged from the head part is configured to be discharged into a gas flow flowing in substantially one direction.   The fine particle manufacturing apparatus according to claim 5, wherein the humidity of the gas is 60% RH or more.   As the wetting means, there is provided a wiping member for wiping the surface of the head portion on the discharge portion side, which is mainly composed of a constituent material of the dispersion medium and impregnated with a liquid not containing the dispersoid. The fine particle production apparatus according to any one of claims 1 to 6.   The fine particle manufacturing apparatus according to claim 1, wherein the head portion discharges the dispersion liquid vertically upward.   The fine particle manufacturing apparatus according to claim 1, wherein a cooled cooling region is provided in the vicinity of the head portion.   The fine particle manufacturing apparatus according to claim 9, wherein a heated heating region is provided downstream of the cooling region in the transport direction of the discharged dispersion liquid.   The fine particle manufacturing apparatus according to claim 10, wherein the heating region is configured to have a temperature of 30 to 150 ° C.   The fine particle manufacturing apparatus according to claim 10 or 11, configured to introduce a dry gas into the heating region.   The fine particle production apparatus according to claim 12, wherein the humidity of the dry gas is 50% RH or less.   The fine particle manufacturing apparatus according to claim 1, wherein the fine particles are resin fine particles.   The apparatus for producing fine particles according to claim 1, wherein the fine particles are toner.   The fine particle manufacturing apparatus according to claim 1, wherein the dispersion liquid is intermittently ejected by a piezoelectric pulse.   The head unit stores a dispersion liquid storage unit that stores the dispersion liquid; a piezoelectric body that applies a piezoelectric pulse to the dispersion liquid stored in the dispersion liquid storage unit; and the discharge that discharges the dispersion liquid using the piezoelectric pulse. The fine particle production apparatus according to claim 1, wherein the fine particle production apparatus has a portion.   The fine particle manufacturing apparatus according to claim 16 or 17, wherein a frequency of the piezoelectric pulse is 1 kHz to 500 MHz.   A fine particle production method using the fine particle production apparatus according to claim 1. A method for producing fine particles using a dispersion in which a dispersoid containing a raw material for producing fine particles is finely dispersed in a dispersion medium,
A step of making the dispersion into fine particles and discharging it from a head unit having a discharge unit, solidifying while transporting the inside of the transport unit,
A method for producing fine particles, wherein fine particles are obtained by discharging the dispersion from the head portion while the discharge portion side of the head portion is wetted. The head unit includes a plurality of the ejection units,
21. The method for producing fine particles according to claim 20, wherein the liquid is wetted by discharging a liquid that is mainly composed of a constituent material of the dispersion medium and does not include the dispersoid from between at least a plurality of the discharge units.   The method for producing fine particles according to claim 20 or 21, wherein after the dispersion liquid is cooled in a region near the head part, the dispersion medium in the dispersion liquid is removed.   The method for producing fine particles according to claim 22, wherein the removal of the dispersion medium is mainly performed by heating.   The method for producing fine particles according to any one of claims 20 to 23, wherein the dispersion medium is mainly composed of water and / or a liquid having excellent compatibility with water.   The method for producing fine particles according to any one of claims 20 to 24, wherein the dispersion is a suspension.   The method for producing fine particles according to any one of claims 20 to 25, wherein the fine particles are resin fine particles.   27. The method for producing fine particles according to claim 20, wherein the fine particles are toner.   A fine particle produced by using the fine particle production apparatus according to claim 1.   Fine particles produced by the method according to any one of claims 19 to 27.   30. The fine particles according to claim 28 or 29, having an average particle diameter of 2 to 20 [mu] m.   The fine particles according to any one of claims 28 to 30, wherein the standard deviation of the particle size between the particles is 1.3 µm or less. 32. The fine particles according to claim 28, wherein an average circularity R represented by the following formula (I) is 0.96 or more.
R = L ₀ / L ₁ (I)
(Wherein, L ₁ [μm] is the peripheral length of the projected image of the fine particle to be measured, and L ₀ [μm] is the peripheral length of a perfect circle having an area equal to the area of the projected image of the fine particle to be measured. To express.)   The fine particles according to any one of claims 28 to 32, wherein the standard deviation of the average circularity between the particles is 0.015 or less.

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