WO2010035861A1 - 新規な銅フタロシアニン顔料及び銅フタロシアニン微粒子の製造方法 - Google Patents
新規な銅フタロシアニン顔料及び銅フタロシアニン微粒子の製造方法 Download PDFInfo
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- WO2010035861A1 WO2010035861A1 PCT/JP2009/066900 JP2009066900W WO2010035861A1 WO 2010035861 A1 WO2010035861 A1 WO 2010035861A1 JP 2009066900 W JP2009066900 W JP 2009066900W WO 2010035861 A1 WO2010035861 A1 WO 2010035861A1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0025—Crystal modifications; Special X-ray patterns
- C09B67/0026—Crystal modifications; Special X-ray patterns of phthalocyanine pigments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
- B01F27/271—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed radially between the surfaces of the rotor and the stator
- B01F27/2712—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed radially between the surfaces of the rotor and the stator provided with ribs, ridges or grooves on one surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
- B01F27/271—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed radially between the surfaces of the rotor and the stator
- B01F27/2714—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed radially between the surfaces of the rotor and the stator the relative position of the stator and the rotor, gap in between or gap with the walls being adjustable
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/40—Mixers with rotor-rotor system, e.g. with intermeshing teeth
- B01F27/41—Mixers with rotor-rotor system, e.g. with intermeshing teeth with the mutually rotating surfaces facing each other
- B01F27/412—Mixers with rotor-rotor system, e.g. with intermeshing teeth with the mutually rotating surfaces facing each other provided with ribs, ridges or grooves on one surface
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0002—Grinding; Milling with solid grinding or milling assistants
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0004—Coated particulate pigments or dyes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0017—Influencing the physical properties by treatment with an acid, H2SO4
- C09B67/0019—Influencing the physical properties by treatment with an acid, H2SO4 of phthalocyanines
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/322—Pigment inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/003—Pigment pastes, e.g. for mixing in paints containing an organic pigment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Definitions
- the present invention relates to a novel copper phthalocyanine pigment.
- a copper phthalocyanine pigment contains copper phthalocyanine (the following chemical formula) having crystal types represented by ⁇ , ⁇ , ⁇ , and ⁇ , and these crystal types are generally specified by powder X-ray diffraction.
- Ink for inkjet and color filters because each crystal type has different fastness such as heat resistance, water resistance, solvent resistance and light resistance, optical properties such as transmission spectrum and absorption spectrum, and physical properties such as appearance color appearance.
- a color filter uses a copper phthalocyanine pigment containing ⁇ -type crystalline copper phthalocyanine because of its transmission characteristics.
- the ⁇ -type copper phthalocyanine obtained by the acid pasting method is treated with a solvent and ⁇ ⁇ -type copper phthalocyanine is produced by a method of obtaining a copper phthalocyanine type (Patent Document 1) or a method of changing a copper phthalocyanine pigment to a ⁇ -type by treating with a solvent containing a salt (Patent Document 2). Yes.
- Patent Document 1 a method of obtaining a copper phthalocyanine type
- Patent Document 2 a method of changing a copper phthalocyanine pigment to a ⁇ -type by treating with a solvent containing a salt
- the present invention relates to a copper phthalocyanine pigment and a copper phthalocyanine fine particle having a wavelength ( ⁇ max) of less than 478 nm, which is copper phthalocyanine having a crystal form of ⁇ -type and having a maximum transmission spectrum transmittance at 380 to 780 nm. It is an object to provide a manufacturing method.
- copper phthalocyanine whose crystal form is ⁇ -type, and the wavelength ( ⁇ max) at which the transmittance of the transmission spectrum at 380 to 780 nm is maximum is less than 478 nm, and the transmission spectrum is the transmission spectrum at the wavelength of 400 to 450 nm. It is an object of the present invention to provide a copper phthalocyanine pigment containing copper phthalocyanine having a transmittance higher than the ⁇ -type copper phthalocyanine over the entire wavelength of 400 to 450 nm and a method for producing copper phthalocyanine fine particles.
- the invention according to claim 1 of the present application is a copper containing copper phthalocyanine having a crystal form of ⁇ -type and a wavelength ( ⁇ max) at which the transmittance of the transmission spectrum at 380 to 780 nm is maximum is less than 478 nm. It is a phthalocyanine pigment.
- the crystal type is ⁇ -type
- the wavelength ( ⁇ max) at which the transmittance of the transmission spectrum at 380 to 780 nm is maximum is less than 478 nm
- the wavelength is 400 to 450 nm.
- the fluid to be processed is supplied between the processing surfaces that can be approached / separated and relatively displaced, and between the supply pressure of the fluid and the processing surface that rotates.
- the distance between the processing surfaces is maintained at a minute interval by the balance between the force in the approaching direction including the pressure and the force in the separation direction, and the distance between the two processing surfaces maintained at the minute interval is covered.
- the copper phthalocyanine according to claim 1, wherein the fluid to be treated forms a thin film fluid by being used as a flow path of the treatment fluid, and is produced as fine particles in the thin film fluid.
- a copper phthalocyanine pigment A copper phthalocyanine pigment.
- the invention according to claim 4 of the present application is the copper phthalocyanine pigment containing copper phthalocyanine according to any one of claims 1 to 3, wherein the shape of the copper phthalocyanine fine particles is substantially spherical.
- the invention according to claim 5 of the present application is the copper phthalocyanine pigment containing copper phthalocyanine according to claim 4, wherein the volume average particle diameter of the copper phthalocyanine fine particles is 1 to 600 nm.
- the fluid to be processed is supplied between the processing surfaces that can be approached / separated and relatively displaced, and between the supply pressure of the fluid and the processing surface that rotates.
- the distance between the processing surfaces is maintained at a minute interval by the balance between the force in the approaching direction including the pressure and the force in the separation direction, and the distance between the two processing surfaces maintained at the minute interval is covered.
- a process for producing copper phthalocyanine fine particles is characterized by forming a thin film fluid by forming a flow path for the treatment fluid and depositing fine particles in the thin film fluid.
- a fluid pressure applying mechanism that applies pressure to the fluid to be processed, a first processing portion, and the first processing portion can be relatively approached and separated.
- the second processing unit includes at least two processing units, and a rotation drive mechanism that relatively rotates the first processing unit and the second processing unit.
- At least two processing surfaces, a first processing surface and a second processing surface are provided at opposing positions, and each of the processing surfaces is sealed so that the fluid to be processed having the pressure is flowed.
- at least the second processing portion of the first processing portion and the second processing portion includes a pressure receiving surface, and at least of the pressure receiving surface. Part of the surface is constituted by the second processing surface, and the pressure receiving surface is the fluid pressure applicator described above.
- the fluid to be treated having the pressure is passed between the surface and the second processing surface, whereby the fluid to be treated forms the thin film fluid, and fine particles are precipitated in the thin film fluid. It is a manufacturing method of the copper phthalocyanine microparticles
- a kind of fluid to be processed which is given pressure from the fluid pressure applying mechanism, is passed between the first processing surface and the second processing surface, An independent separate introduction path through which another kind of fluid to be treated different from the kind of fluid to be treated is passed is provided, and at least one opening leading to the introduction path has the first processing surface and the second treatment path.
- the other kind of fluid to be treated is introduced from the introduction path between the treatment surfaces, and the kind of fluid to be treated and the other kind of fluid are introduced.
- the present invention relates to copper phthalocyanine having an ⁇ -type crystal form in powder X-ray diffraction measurement, and a copper phthalocyanine containing copper phthalocyanine having a wavelength ( ⁇ max) of less than 478 nm at which the transmittance of the transmission spectrum at 380 to 780 nm is maximum.
- a phthalocyanine pigment could be provided. Since the crystal type is ⁇ -type, a process for changing the crystal type and a process requiring a lot of energy can be omitted, and the conventional problems mentioned above can be improved.
- the transmittance of the transmission spectrum at a wavelength of 400 to 450 nm is larger than that of copper phthalocyanine whose crystal type is ⁇ type over the entire wavelength.
- a copper phthalocyanine pigment containing copper phthalocyanine can be provided. That is, although it is a copper phthalocyanine whose crystal form is ⁇ -type, it has excellent characteristics under the above conditions than ⁇ -type copper phthalocyanine.
- FIG. 1 is a substantially longitudinal cross-sectional view which shows the concept of the apparatus used for implementation of this invention
- B is a general
- C is the said It is a schematic longitudinal cross-sectional view which shows the concept of other embodiment of an apparatus
- D is a general
- A) to (D) are schematic longitudinal sectional views showing the concept of still another embodiment of the apparatus shown in FIG.
- A) is the principal part schematic bottom view of the apparatus shown in FIG.2 (C)
- B) is the principal part schematic bottom view of other embodiment of the said apparatus
- C) is another implementation.
- FIG. 4D is a schematic bottom view showing the concept of still another embodiment of the apparatus
- FIG. 4E is a concept of still another embodiment of the apparatus
- (F) is a schematic bottom view showing the concept of still another embodiment of the above apparatus.
- A) to (D) are schematic longitudinal sectional views showing the concept of still another embodiment of the apparatus shown in FIG. (A) to (D) are schematic longitudinal sectional views showing the concept of still another embodiment of the apparatus shown in FIG. (A) to (D) are schematic longitudinal sectional views showing the concept of still another embodiment of the apparatus shown in FIG. (A) to (D) are schematic longitudinal sectional views showing the concept of still another embodiment of the apparatus shown in FIG. (A) to (D) are schematic longitudinal sectional views showing the concept of still another embodiment of the apparatus shown in FIG. (A) to (D) are schematic longitudinal sectional views showing the concept of still another embodiment of the apparatus shown in FIG.
- FIG. 1 to (C) are schematic longitudinal sectional views showing the concept of still another embodiment of the apparatus shown in FIG. (A) to (D) are schematic longitudinal sectional views showing the concept of still another embodiment of the apparatus shown in FIG. (A)
- FIG. 1 is a principal part outline of the apparatus shown in FIG. 1 (A). It is a bottom view.
- (A) is a principal part schematic longitudinal cross-sectional view which shows other embodiment about the pressure receiving surface of the apparatus shown to FIG. 1 (A)
- (B) is a principal part abbreviation of other embodiment of the said apparatus. It is a longitudinal cross-sectional view.
- (D) is a partially notch principal part schematic longitudinal cross-sectional view of other embodiment of the said apparatus. It is a principal part schematic longitudinal cross-sectional view of further another embodiment of the apparatus shown to FIG. 12 (A).
- (A) is a general
- (B) is a partial notch principal part explanatory drawing of the said apparatus.
- (A) is a top view of the 1st process part of the apparatus shown to FIG. 12 (A), (B) is the principal part longitudinal cross-sectional view.
- (A) is a longitudinal sectional view of the main part of the first and second processing parts of the apparatus shown in FIG. 12 (A), and (B) is a view of the first and second processing parts with a minute gap therebetween. It is a principal part longitudinal cross-sectional view.
- (A) is a top view of other embodiment of the said 1st process part,
- (B) is the principal part general
- (A) is a top view of further another embodiment of the said 1st process part, (B) is the principal part general
- (A) is a top view of other embodiment of the 1st processing part, (B) is a top view of other embodiment of the 1st processing part.
- FIG. 25 is a schematic plan view of a first processing surface of the apparatus shown in FIG. 25, and (B) is an enlarged view of a main part of the first processing surface of the apparatus shown in FIG. (A) is sectional drawing of a 2nd introduction path, (B) is a principal part enlarged view of the processing surface for demonstrating a 2nd introduction path.
- A) And (B) is a principal part expanded sectional view for demonstrating the inclined surface provided in the part for a process, respectively.
- FIG. 1 is a powder X diffraction pattern of copper phthalocyanine obtained in Example 1.
- FIG. 2 is a transmission spectrum (solid line) of ⁇ -type copper phthalocyanine and a transmission spectrum (dashed line) of copper phthalocyanine obtained in Example 1.
- FIG. 2 is a transmission electron microscope (TEM) photograph of copper phthalocyanine fine particles obtained in Example 1.
- FIG. 1 is a powder X diffraction pattern of copper phthalocyanine obtained in Example 1.
- FIG. 2 is a transmission spectrum (solid line) of ⁇ -type copper phthalocyanine and a transmission spectrum (dashed line) of copper phthalocyanine obtained in Example 1.
- FIG. 2 is a transmission electron microscope (TEM) photograph of copper phthalocyanine fine particles obtained in Example 1.
- (A) is a scanning electron microscope (SEM) photograph of copper phthalocyanine fine particles produced by FTFR (Example 6)
- (B) is a photograph of copper phthalocyanine particles produced by the batch method (Comparative Example 2). It is. It is a figure which shows the particle size distribution of the (Example 6) copper phthalocyanine microparticles produced by FTFR and the copper phthalocyanine particle produced by the batch method (Comparative Example 2).
- (Example 6) It is a transmission electron microscope (TEM) photograph of the copper phthalocyanine fine particle produced by FTFR.
- Example 4 is a graph showing infrared absorption spectra of copper phthalocyanine fine particles according to Examples 7 to 10. It is a figure which shows the transmission spectrum of the 0.0050% dispersion liquid of the copper phthalocyanine particle
- the black line shows the transmission spectrum of Example 7, and the gray line shows the transmission spectrum of Example 10.
- the crystal form is copper phthalocyanine shown by the powder X-ray diffraction pattern shown in FIG. 30, and the transmission spectrum shown by the broken line in FIG. 31 or the solid line (FTFR ( ⁇ )) in FIG.
- the copper phthalocyanine pigment in the present invention includes a copper phthalocyanine derivative such as a sulfonated product or hydroxide of copper phthalocyanine. It can also be carried out by including a copper phthalocyanine pigment having a functional group such as a hydroxyl group or a sulfo group introduced on the surface of the copper phthalocyanine fine particles.
- the crystal type of copper phthalocyanine in the present invention can be determined to be ⁇ -type.
- the wavelength ( ⁇ max) at which the transmittance of the transmission spectrum at 380 to 780 nm is maximum is less than 478 nm, and the transmittance of the transmission spectrum at the wavelength of 400 to 450 nm is over the entire wavelength of 400 to 450 nm.
- the copper phthalocyanine is larger than the ⁇ -type copper phthalocyanine.
- the method for measuring the transmission spectrum in the present invention is not particularly limited.
- Examples thereof include a method for measuring a transmission spectrum of an aqueous solution or an organic solvent-based dispersion of a copper phthalocyanine pigment, and a method for measuring a dispersion applied to glass, a transparent electrode, or a film.
- the method for producing the copper phthalocyanine pigment obtained in the present invention is not particularly limited.
- the break-down method represented by the pulverization method can be used, and the build-up method can also be used. It can also be carried out by newly synthesizing.
- a fluid containing a copper phthalocyanine solution in which copper phthalocyanine is dissolved in a solvent and a fluid containing a solvent that has a lower solubility in copper phthalocyanine than the copper phthalocyanine solution and can be a poor solvent
- copper phthalocyanine is precipitated to produce copper phthalocyanine fine particles.
- a method for producing copper phthalocyanine fine particles which mixes the fluid as a thin film fluid between the surfaces and deposits copper phthalocyanine fine particles in the thin film fluid, can be used.
- This manufacturing method will be described below. However, this manufacturing method is only an example, and the present invention is not limited to this manufacturing method.
- the crystal form of copper phthalocyanine before being dissolved in the solvent is not limited, and various crystal forms of copper phthalocyanine can be used as well as typical ⁇ -type, ⁇ -type, and ⁇ -type.
- copper phthalocyanine containing copper phthalocyanine before the pigmentation step or amorphous copper phthalocyanine can also be used.
- the particle diameter is not particularly limited.
- this apparatus includes first and second processing units 10 and 20 that face each other, and at least one processing unit rotates.
- the opposing surfaces of the processing parts 10 and 20 are processed surfaces 1 and 2, respectively, and the processing target fluid is processed between the processing surfaces.
- the first processing unit 10 includes a first processing surface 1
- the second processing unit 20 includes a second processing surface 2. Both processing surfaces 1 and 2 are connected to the flow path of the fluid to be processed and constitute a part of the flow path of the fluid to be processed. More specifically, this apparatus constitutes at least two flow paths for the fluid to be processed and joins the flow paths together.
- this apparatus is connected to the flow path of the first fluid to be treated, forms a part of the flow path of the first fluid to be treated, and is separate from the first fluid to be treated. 2 A part of the flow path of the fluid to be treated is formed. And this apparatus makes both flow paths merge, mixes both fluids between the processing surfaces 1 and 2, and makes it react when a reaction is accompanied.
- each of the above-mentioned flow paths is sealed, and is liquid-tight (when the fluid to be treated is liquid) or air-tight (when the fluid to be treated is gas). It is said that.
- this apparatus includes a first processing unit 10, a second processing unit 20, and a first processing unit 10 that holds the first processing unit 10.
- the rotation drive unit is not shown in the figure.
- At least one of the first processing unit 10 and the second processing unit 20 can be approached / separated from at least either one, and both processing surfaces 1 and 2 can be approached / separated.
- the second processing unit 20 approaches and separates from the first processing unit 10.
- the first processing unit 10 may approach or separate from the second processing unit 20, and both processing units 10 and 20 may approach or separate from each other. It may be.
- the second processing unit 20 is disposed above the first processing unit 10, and the lower surface of the second processing unit 20, that is, the lower surface is the second processing surface 2, and
- the first processing surface 1 is an upper surface, that is, an upper surface of the first processing portion 10.
- the first processing unit 10 and the second processing unit 20 are each an annular body, that is, a ring.
- the first processing unit 10 is referred to as a first ring 10
- the second processing unit 20 is referred to as a second ring 20 as necessary.
- both the rings 10 and 20 are members whose one end made of metal is mirror-polished, and the mirror surfaces are defined as a first processing surface 1 and a second processing surface 2. That is, the upper end surface of the first ring 10 is mirror-polished as the first processing surface 1, and the lower end surface of the second ring 20 is mirror-polished as the second processing surface 2.
- At least one of the holders can be rotated relative to the other holder by the rotation driving unit.
- Reference numeral 50 in FIG. 1A denotes a rotation shaft of the rotation drive unit.
- An electric motor can be adopted as the rotation drive unit.
- the processing surface of the other ring can be rotated relative to the processing surface of the one ring.
- the first holder 11 receives the driving force from the rotation driving unit at the rotation shaft 50 and rotates with respect to the second holder 21.
- the integrated first ring 10 rotates with respect to the second ring 20.
- the rotation shaft 50 is provided in the first holder 11 so as to be concentric with the center of the circular first ring 10 in plan view.
- the rotation of the first ring 10 is centered on the axis of the first ring 10.
- the axis indicates the center line of the first ring 10 and is an imaginary line.
- each of the first and second holders 11 and 21 includes a concave ring housing portion.
- the first ring 10 is fixed to the ring housing portion so that the first ring 10 fits into the ring housing portion of the first holder 11 and does not protrude from the ring housing portion of the first holder 11. ing.
- the material of the first ring 10 is not only metal, but also ceramic, sintered metal, wear-resistant steel, other metal that has been subjected to hardening treatment, or hard material that has been subjected to lining, coating, plating, or the like. .
- it since it rotates, it is desirable to form the 1st process part 10 with a lightweight raw material. What is necessary is just to employ
- the ring accommodating part 41 with which the 2nd holder 21 is provided accommodates the processing surface 2 of the 2nd ring 20 so that it can protrude and retract.
- the ring holder 41 included in the second holder 21 is a recess that mainly stores a portion of the second ring 20 on the side opposite to the processing surface 2 side.
- the ring holder 41 has a circular shape in plan view, that is, is formed in an annular shape. It is a groove.
- the ring accommodating portion 41 is formed larger than the size of the second ring 20 and accommodates the second ring 20 with a sufficient clearance between the ring accommodating portion 41 and the second ring 20.
- the second ring 20 can be displaced in the ring accommodating portion 41 in the axial direction of the annular ring accommodating portion 41 and in the direction intersecting with the axial direction.
- the second ring 20 can be displaced with respect to the ring housing part 41 so that the center line of the second ring 20 breaks the parallel relationship with the axial direction of the ring housing part 41.
- a portion of the second holder 21 surrounded by the second ring 20 is referred to as a central portion 22.
- the second ring 20 is further decentered with respect to the thrust direction of the ring accommodating portion 41, that is, the direction in which the second ring 20 protrudes and retracts, with respect to the center of the ring accommodating portion 41. Is accommodated so that it can be displaced. Further, the second ring 20 can be displaced so that the width of the protrusions and depressions from the ring accommodating portion 41 is different at each position in the circumferential direction of the second ring 20 with respect to the ring accommodating portion 41, that is, the second center can be swung. The ring 20 is accommodated.
- the second ring 20 includes the first ring 10 while having the above three degrees of freedom of freedom, that is, the degree of freedom of the second ring 20 with respect to the ring accommodating portion 41 in the axial direction, the eccentric direction, and the center deflection direction. Is held by the second holder 21 so as not to follow the rotation.
- this point may be implemented by providing each ring accommodating portion 41 and the second ring 20 with an appropriate contact that restricts the ring accommodating portion 41 from rotating in the circumferential direction. However, the hit must not impair the three degrees of freedom of displacement.
- Said contact surface pressure provision mechanism 4 provides the processing part with a force that causes the first processing surface 1 and the second processing surface 2 to approach each other.
- the contact pressure applying mechanism 4 is provided in the second holder 21 and biases the second ring 20 toward the first ring 10.
- the contact surface pressure application mechanism 4 urges each position in the circumferential direction of the second ring 20, that is, each position of the second processing surface 2, evenly toward the first ring 10.
- a specific configuration of the contact surface pressure imparting mechanism 4 will be described in detail later.
- the case 3 is arranged outside the outer peripheral surfaces of both the rings 10 and 20 and is generated between the processing surfaces 1 and 2. Contains the product discharged to the outside. As shown in FIG.
- the case 3 is a liquid-tight container that houses the first holder 11 and the second holder 21.
- the 2nd holder 21 can be implemented as what was formed integrally with case 3 as a part of the case 3 concerned.
- the second holder 21 when the second holder 21 is formed as a part of the case 3 or formed separately from the case 3, the second holder 21 has a space between the rings 10 and 20, that is, both processing surfaces 1. It is not movable so as to affect the distance between the two. In other words, the second holder 21 does not affect the distance between the processing surfaces 1 and 2.
- the case 3 is provided with a discharge port 32 for discharging the product outside the case 3.
- the first introduction part d1 supplies the first fluid to be processed between the processing surfaces 1 and 2.
- the fluid pressure applying mechanism p1 is connected to the first introduction part d1 directly or indirectly and applies a fluid pressure to the first fluid to be treated.
- a compressor or other pump can be employed for the fluid pressure imparting mechanism p1.
- the first introduction portion d1 is a fluid passage provided inside the central portion 22 of the second holder 21, and one end of the first introduction portion d1 is a flat surface of the second holder 21 and the second ring 20 is flat. An opening is made at the center position of the circle presented in the view.
- the other end of the first introduction part d1 is connected to the fluid pressure applying mechanism p1 outside the second holder 21, that is, outside the case 3.
- the second introduction part d2 supplies the second fluid to be mixed with the first fluid to be treated between the processing surfaces 1 and 2.
- the second introduction part is a fluid passage provided inside the second ring 20, one end of which opens at the second processing surface 2, and the other end has a second The fluid supply part p2 is connected.
- a compressor and other pumps can be adopted for the second fluid supply part p2.
- the first fluid to be treated which is pressurized by the fluid pressure imparting mechanism p1
- the first introduction part d1 into the space inside both the rings 10 and 20, and the first treatment surface 1 and the first 2 Passes between the processing surfaces 2 and tries to pass outside the rings 10 and 20.
- the second ring 20 that has received the pressure of the first fluid to be treated moves away from the first ring 10 against the urging force of the contact surface pressure imparting mechanism 4, and a minute amount between both treatment surfaces. Open a large interval. The distance between both surfaces 1 and 2 due to the approach and separation of both processing surfaces 1 and 2 will be described in detail later.
- the second fluid to be treated is supplied from the second introduction part d ⁇ b> 2, merges with the first fluid to be treated, and mixing (reaction) is caused by the rotation of the processing surface. Promoted. And the product by mixing (reaction) of both fluids is discharged
- the mixing and reaction of the fluid to be processed (when accompanied by a reaction) is performed by rotating the first processing surface 1 and the second processing by the rotation of the driving unit 5 of the first processing unit 10 with respect to the second processing unit 20. This is done with the working surface 2.
- the downstream side of the opening m2 of the second introduction portion d2 mixes the first fluid to be treated and the second fluid to be treated. It becomes a room.
- the second introduction is performed in the inner and outer direction r ⁇ b> 1 of the diameter of the second ring 20, which is indicated by diagonal lines.
- the opening m2 of the part that is, the region H outside the second opening m2 functions as the processing chamber. Therefore, this processing chamber is located downstream of both openings m1 and m2 of the first introduction part d1 and the second introduction part d2 between the processing surfaces 1 and 2.
- the processing surfaces 1 and 2 With respect to the first fluid to be processed introduced from the first opening m1 to the space between the processing surfaces 1 and 2 through the space inside the ring, the processing surfaces 1 and 2 from the second opening m2.
- the second fluid to be treated introduced between them is mixed in the region H serving as the treatment chamber, and when the reaction is involved, both fluids to be treated react.
- the fluid is supplied by the fluid pressure applying mechanism p1 and the fluid tries to move outside the ring through a minute gap between the processing surfaces 1 and 2, but the first ring 10 is rotating. Therefore, in the region H, the mixed fluid does not move linearly from the inside to the outside in the inner and outer directions of the diameter of the ring, but is centered on the rotation axis of the ring in a state where the processing surface is viewed in plan view. As a result, the ring moves from the inside of the ring to the outside. In this way, in the region H where mixing (reaction) is performed, the section required for sufficient mixing (reaction) at a minute interval between the processing surfaces 1 and 2 by moving spirally from the inside to the outside. Can be ensured, and uniform mixing can be promoted.
- a product generated by mixing becomes a homogeneous product between the minute first and second processing surfaces 1 and 2, and in particular, fine particles in the case of crystallization and precipitation.
- the distance between the processing surfaces 1 and 2 can be balanced between the processing surfaces 1 and 2, which can balance the interval to a preferable minute interval, and further receive the pressure applied by the fluid pressure applying mechanism p 1 and the centrifugal force due to the rotation of the ring Mixing (reaction) is promoted by moving the minute gap in a spiral.
- the above-mentioned mixing (reaction) is forcibly performed by the pressure feeding applied by the fluid pressure applying mechanism p1 and the rotation of the ring. That is, mixing (reaction) is forcedly and uniformly performed between the processing surfaces 1 and 2 that are disposed so as to be able to approach and separate from each other and at least one rotates relative to the other. Therefore, in particular, the crystallization or precipitation of the product due to the reaction is performed by a method that is relatively easy to control, such as adjustment of the feed pressure applied by the fluid pressure imparting mechanism p1, and adjustment of the rotation speed of the ring, that is, the rotation speed of the ring. Can be controlled.
- this fluid processing apparatus can control the distance between the processing surfaces 1 and 2 that affect the size of the product by adjusting the feeding pressure and the centrifugal force. This is excellent in that the distance traveled in the region H that affects generation can be controlled.
- said process is not restricted to what a product precipitates, but includes the case of a liquid.
- the product when the product is a fine mass such as fine particles, the product may be precipitated in the treated fluid, and is in a dispersion state in which a dispersed phase exists in the continuous phase. It may be a thing.
- the rotating shaft 50 is not limited to the one arranged vertically, but may be arranged in the horizontal direction or may be arranged inclined.
- the 1st introduction part d1 has corresponded with the axis of the 2nd ring 20 in the 2nd holder 21, and has shown what was extended vertically.
- the first introduction part d1 is not limited to the one that coincides with the axis of the second ring 20, and the first fluid to be treated is supplied to the space surrounded by the rings 10 and 20. As long as it is possible, it may be provided at other positions of the central portion 22 of the second holder 21, and may extend obliquely rather than vertically.
- FIG. 12A shows a more preferable embodiment of the above apparatus.
- the second processing section 20 includes the second processing surface 2 and a pressure receiving surface 23 located inside the second processing surface 2 and adjacent to the second processing surface 2.
- the pressure receiving surface 23 is also referred to as a separation adjusting surface 23.
- the separation adjusting surface 23 is an inclined surface.
- the ring holder 41 is formed at the bottom or lower part of the second holder 21, and the second processing member 20 is received in the ring holder 41.
- the second processing unit 20 is received so as not to rotate with respect to the second holder 21 by being prevented from rotating.
- the second processing surface 2 is exposed from the second holder 21.
- the inside of the first processing part 10 and the second processing part 20 between the processing surfaces 1 and 2 is an inflow part of the workpiece, and the first processing part 10 and the second processing part 20
- the outside of the processing portion 20 is an outflow portion of the object to be processed.
- the contact surface pressure applying mechanism 4 presses the second processing surface 2 against the first processing surface 1 in a pressure contact state or a close state, and both processes such as the contact surface pressure and the fluid pressure are performed.
- a thin film fluid having a predetermined thickness is formed by balance with the force separating the working surfaces 1 and 2. In other words, the distance between the processing surfaces 1 and 2 is kept at a predetermined minute distance by the balance of the forces.
- the contact surface pressure applying mechanism 4 includes the ring accommodating portion 41 and the ridge receiving portion 42 provided at the back of the ring accommodating portion 41, that is, at the deepest portion of the ring accommodating portion 41. And a spring 43 and an air introduction portion 44.
- the contact surface pressure imparting mechanism 4 only needs to include at least one of the ring accommodating portion 41, the sway receiving portion 42, the spring 43, and the air introducing portion 44.
- the ring accommodating portion 41 loosely fits the second processing portion 20 so that the position of the second processing portion 20 in the ring accommodating portion 41 can be displaced deeply or shallowly, that is, vertically. .
- One end of the spring 43 is in contact with the back of the sway receiving portion 42, and the other end of the spring 43 is in contact with the front portion, that is, the upper portion of the second processing portion 20 in the ring housing portion 41.
- the plurality of springs 43 press each part of the second processing unit 20. That is, by increasing the number of springs 43, a more uniform pressing force can be applied to the second processing unit 20. Therefore, the second holder 21 is preferably a multi-type in which several to several tens of springs 43 are attached.
- the air introduction part 44 can introduce air into the ring housing part 41 from others.
- the space between the ring accommodating portion 41 and the second processing portion 20 can be used as a pressurizing chamber, and the air pressure can be given to the second processing portion 20 together with the spring 43 as a pressing force. Therefore, it is possible to adjust the contact pressure of the second processing surface 2 with respect to the first processing surface 1 during operation by adjusting the air pressure introduced from the air introducing portion 44. It is also possible to use a mechanism that generates a pressing force with another fluid pressure such as a hydraulic pressure instead of the air introduction portion 44 that uses the air pressure.
- the contact surface pressure imparting mechanism 4 supplies and adjusts a part of the pressing force, that is, the contact surface pressure, and also serves as a displacement adjustment mechanism and a buffer mechanism.
- the contact surface pressure applying mechanism 4 is a displacement adjusting mechanism, and can follow the axial displacement due to the elongation or wear in the axial direction at the start or during operation by adjusting the air pressure, and can maintain the initial pressing force.
- the contact surface pressure applying mechanism 4 also functions as a buffer mechanism for fine vibration and rotational alignment by adopting a floating mechanism that holds the second processing member 20 in a displaceable manner.
- the first fluid to be processed is introduced from the first introduction part d1 into the internal space of the sealed case under pressure supplied from the fluid pressure imparting mechanism p1.
- the first processing unit 10 is rotated by the rotation of the rotating shaft 50 by the rotation driving unit.
- the 1st processing surface 1 and the 2nd processing surface 2 rotate relatively in the state where a minute interval was maintained.
- the first fluid to be processed becomes a thin film fluid between the processing surfaces 1 and 2 with a very small interval
- the second fluid to be processed introduced from the second introduction part d2 is the both processing surfaces 1. 2 is joined with the thin film fluid to form a part of the thin film fluid.
- the first and second fluids to be treated are mixed to form a product.
- both fluids react to promote a uniform reaction and form a reaction product.
- This makes it possible to produce relatively uniform and fine particles in the case of precipitation, and even in the case of no precipitation, a uniform mixed state (a uniform reaction in the case of reaction). ) Is realized.
- the precipitated product may be further refined by being sheared with the second processing surface 2 by the rotation of the first processing surface 1.
- the first processing surface 1 and the second processing surface 2 are adjusted to a minute interval of 1 ⁇ m to 1 mm, particularly 1 ⁇ m to 10 ⁇ m, so that a uniform mixed state (in the case involving reaction) (Uniform reaction) and ultrafine particles of several nanometers can be generated.
- the product exits between the processing surfaces 1 and 2 and is discharged from the discharge port 32 of the case 3 to the outside of the case.
- the discharged product is atomized in a vacuum or a reduced-pressure atmosphere by a known decompression device, and the product that has fallen as a fluid by hitting the other in the atmosphere is recovered as a liquid after degassing can do.
- the processing apparatus is provided with a case.
- the processing apparatus may be implemented without providing such a case.
- a depressurization tank that is, a vacuum tank for degassing may be provided, and a processing apparatus may be disposed inside the tank.
- the above-described discharge port is not provided in the processing apparatus.
- the first processing surface 1 and the second processing surface 2 can be adjusted to a minute interval of ⁇ m, which is impossible by setting a mechanical clearance.
- the first processing surface 1 and the second processing surface 2 are relatively close to and away from each other and rotate relatively.
- the first processing surface 1 rotates and the second processing surface 2 approaches and separates from the first processing surface 1 with a structure (floating structure) that can move in the axial direction. Therefore, in this example, the axial position of the second processing surface 2 is set with an accuracy in units of ⁇ m by the force, that is, the balance between the contact surface pressure and the separation force described above, whereby both processing surfaces 1, A minute interval between the two is set.
- examples of the contact pressure include the pressure when air pressure, that is, positive pressure is applied from the air introduction portion 44 in the contact pressure applying mechanism 4, and the pressing force of the spring 43. .
- the second introduction part d2 is omitted in order to avoid complication of the drawings. This may be considered as a cross section at a position where the second introduction part d2 is not provided.
- U indicates the upper side
- S indicates the lower side.
- the separation force the fluid pressure acting on the separation-side pressure receiving surface, that is, the second processing surface 2 and the separation adjusting surface 23, the centrifugal force due to the rotation of the first processing unit 10, and the air introduction unit 44.
- the negative pressure when a negative pressure is applied to can be mentioned.
- the processing surfaces 1 and 2 can be separated greatly, and cleaning can be performed easily. Then, due to the balance between these forces, the second processing surface 2 is stabilized at a predetermined distance from the first processing surface 1 so that setting with an accuracy of ⁇ m is realized. .
- the second processing unit 20 in the sealed flow path receives the feeding pressure of the fluid to be processed, that is, the fluid pressure, from the fluid pressure applying mechanism p1.
- the surface opposite to the first processing surface in the flow path that is, the second processing surface 2 and the separation adjusting surface 23 become the separation pressure receiving surface, and fluid pressure acts on the pressure receiving surface to Separation force due to pressure is generated.
- the centrifugal force when the first processing unit 10 rotates at a high speed, the centrifugal force acts on the fluid, and a part of the centrifugal force acts in a direction to move the processing surfaces 1 and 2 away from each other. It becomes power.
- the negative pressure acts as a separation force.
- the force that separates the first and second processing surfaces 1 and 2 from each other is described as a separation force, and the above-described force is not excluded from the separation force.
- the separation force and the contact surface pressure exerted by the contact surface pressure applying mechanism 4 are balanced through the fluid to be processed between the processing surfaces 1 and 2.
- a uniform mixed state is realized between the processing surfaces 1 and 2
- a uniform reaction is realized, and a fine product is crystallized / Form a thin film fluid suitable for performing the deposition.
- this apparatus forces a thin space between the processing surfaces 1 and 2 by passing a thin film fluid between them. In this way, it was possible to maintain the fine particles as a product with high accuracy.
- the thickness of the thin film fluid between the processing surfaces 1 and 2 is adjusted to a desired thickness by adjusting the above-described separation force and contact surface pressure, and the required uniform mixed state (in the case where there is a reaction). Can achieve a uniform reaction) and can produce fine products. Therefore, when trying to reduce the thickness of the thin film fluid, the contact surface pressure or the separation force may be adjusted so that the contact surface pressure is relatively increased with respect to the separation force. In this case, the separation force or the contact surface pressure may be adjusted so that the separation force is relatively increased with respect to the contact surface pressure.
- the contact surface pressure applying mechanism 4 may apply air pressure, that is, positive pressure from the air introduction portion 44, or the spring 43 may be changed to one having a large pressing force or the number thereof may be increased.
- the feeding pressure of the fluid pressure applying mechanism p1 is increased, or the areas of the second processing surface 2 and the separation adjusting surface 23 are increased, and in addition to this, the first processing unit 10
- the centrifugal force may be increased by adjusting the rotation of the air or the pressure from the air introduction part 44 may be reduced. Alternatively, negative pressure may be applied.
- the spring 43 is a pushing ridge that generates a pressing force in the extending direction, but can be a part or all of the configuration of the contact surface pressure applying mechanism 4 as a pulling ridge that generates a force in the contracting direction.
- the feeding pressure of the fluid pressure imparting mechanism p1 is decreased, or the areas of the second processing surface 2 and the separation adjusting surface 23 are decreased, and in addition to this, the first processing unit 10
- the centrifugal force may be reduced by adjusting the rotation of the air or the pressure from the air introduction part 44 may be increased. Alternatively, the negative pressure may be reduced.
- the properties of the fluid to be treated such as viscosity can be added as an element for increasing and decreasing the contact surface pressure and the separation force.
- the fluid pressure acting on the separation-side pressure receiving surface that is, the second processing surface 2 and the separation adjustment surface 23 is understood as a force constituting an opening force in the mechanical seal.
- the second processing unit 20 corresponds to a compression ring.
- this force is used as an opening force.
- the second processing portion 20 is provided with only the pressure-receiving surface on the separation side, that is, the second processing surface 2 and the separation adjustment surface 23. All of the infeed pressure constitutes the opening force.
- the pressure receiving surface is provided also in the back side of the 2nd process part 20, specifically in FIG.12 (B) and FIG.17 mentioned later, it is as separation force among sending pressure. The difference between what works and what works as contact pressure is the opening force.
- the second processing portion 20 is exposed from the ring accommodating portion 41 and has an inner peripheral surface side facing the opposite side, that is, the upper side, of the second processing surface 2.
- An adjustment surface 24 is provided.
- the contact surface pressure applying mechanism 4 includes a ring housing portion 41, an air introduction portion 44, and the approach adjustment surface 24.
- the contact surface pressure applying mechanism 4 includes at least one of the ring housing portion 41, the sway receiving portion 42, the spring 43, the air introduction portion 44, and the approach adjusting surface 24. If it is.
- the approach adjustment surface 24 receives a predetermined pressure applied to the fluid to be treated and generates a force for moving the first treatment surface 1 in the direction in which the second treatment surface 2 is brought closer to the approaching contact surface. As a part of the pressure application mechanism 4, it plays the role of the contact pressure supply side.
- the second processing surface 2 and the above-described separation adjusting surface 23 are moved in a direction to separate the second processing surface 2 from the first processing surface 1 under a predetermined pressure applied to the fluid to be processed. Force to generate, and to play the role of the supply side for a part of the separation force.
- the approach adjusting surface 24, the second processing surface 2 and the separation adjusting surface 23 are both pressure receiving surfaces that receive the pressure of the fluid to be processed, and the direction of the contact surface pressure is generated depending on the orientation thereof. It has a different effect of generating separation force.
- the area ratio A1 / A2 of the total area A2 of the projected areas of the second processing surface 2 and the separation adjusting surface 23 is called a balance ratio K and is important for adjusting the opening force.
- Both the tip of the approach adjustment surface 24 and the tip of the separation adjustment surface 23 are defined by the inner peripheral surface 25 of the annular second processing portion 20, that is, the tip line L ⁇ b> 1. For this reason, the balance ratio K is adjusted by determining where the base end line L2 of the approach adjustment surface 24 is placed.
- the total projected area of the second processing surface 2 and the separation adjusting surface 23 is determined by the approach adjusting surface 24. By making it larger than the projected area, an opening force according to the area ratio can be generated.
- the opening force can be adjusted by the pressure of the fluid to be treated, that is, the fluid pressure, by changing the balance line, that is, the area A1 of the approach adjustment surface 24.
- the sliding surface actual surface pressure P that is, the contact surface pressure due to the fluid pressure is calculated by the following equation.
- P1 represents the pressure of the fluid to be treated, that is, the fluid pressure
- K represents the balance ratio
- k represents the opening force coefficient
- Ps represents the spring and back pressure.
- the product can be made finer.
- the processing becomes rough and the processing amount per unit time increases. Therefore, by adjusting the sliding surface actual surface pressure P described above, the gap between the processing surfaces 1 and 2 is adjusted to obtain a desired uniform mixed state (a uniform reaction in the case where a reaction is involved). It can be realized and a fine product can be obtained.
- the actual sliding surface pressure P is referred to as a surface pressure P. To summarize this relationship, when the product is roughened, the balance ratio is reduced, the surface pressure P is reduced, the gap is increased, and the thickness is increased.
- the approach adjustment surface 24 is formed as a part of the contact surface pressure applying mechanism 4, and the contact surface pressure is adjusted at the balance line position, that is, the gap between the processing surfaces is adjusted. Can also be implemented.
- the clearance is adjusted in consideration of the pressing force of the spring 43 and the air pressure of the air introduction portion 44 as described above.
- adjustment of the fluid pressure that is, the feed pressure of the fluid to be processed
- the adjustment of the rotation of the first processing unit 10, that is, the first holder 11, which is an adjustment of the centrifugal force are also important adjustment factors.
- this apparatus uses the second processing unit 20 and the first processing unit 10 that rotates relative to the second processing unit 20 to feed the fluid to be processed and the rotational centrifugal force,
- the pressure is balanced by the contact surface pressure, and a predetermined thin film fluid is formed on both processing surfaces.
- at least one of the rings has a floating structure to absorb alignment such as runout and eliminate the risk of wear due to contact.
- the configuration other than the provision of the adjustment surface is the same as that of the embodiment shown in FIG. Further, in the embodiment shown in FIG. 12B, as shown in FIG. 17, it is possible to carry out without providing the separation adjusting surface 23 described above.
- the approach adjusting surface 24 is provided as in the embodiment shown in FIG. 12B or FIG. 17, the opening force is set by making the area A1 of the approach adjusting surface 24 larger than the area A2.
- the predetermined pressure applied to the fluid to be treated works as the contact pressure.
- the processing surfaces 1 and 2 can be balanced by increasing other separation force. With the above area ratio, the force that acts in the direction of separating the second processing surface 2 from the first processing surface 1 is determined as the resultant force of the force received from the fluid.
- the spring 43 is preferably attached in a larger number in order to apply a uniform stress to the sliding surface, that is, the processing surface.
- a single coil spring can be adopted as the spring 43. As shown in the figure, this is a single coil spring whose center is concentric with the annular second processing portion 20. A space between the second processing unit 20 and the second holder 21 is hermetically sealed, and well-known means can be employed for the seal.
- the second holder 21 is provided with a temperature adjustment jacket 46 capable of adjusting the temperature of the second processing unit 20 by cooling or heating.
- 3 of FIG. 14 has shown the above-mentioned case, This case 3 is also provided with the temperature-adjusting jacket 35 for the same purpose.
- the temperature adjustment jacket 46 of the second holder 21 is a water space formed in the side surface of the ring housing portion 41 in the second holder 21, and passages 47 and 48 that communicate with the outside of the second holder 21. I'm in touch.
- One of the passages 47 and 48 introduces a cooling or heating medium into the temperature adjusting jacket 46, and either one discharges the medium.
- the temperature adjusting jacket 35 of the case 3 allows heating water or cooling water provided between the outer peripheral surface of the case 3 and the covering portion 34 to pass through the covering portion 34 covering the outer periphery of the case 3. It is a passage.
- the second holder 21 and the case 3 are provided with the above-described temperature adjustment jacket.
- the first holder 11 can also be provided with such a jacket. is there.
- a cylinder mechanism 7 shown in FIG. 15 may be provided as a part of the contact surface pressure applying mechanism 4.
- the cylinder mechanism 7 includes a cylinder space portion 70 provided in the second holder 21, a communication portion 71 that connects the cylinder space portion 70 to the ring storage portion 41, and a communication portion 71 that is accommodated in the cylinder space portion 70.
- a pressing body 75 such as a ridge formed between the piston body 72 and the piston body 72 is provided.
- the piston body 72 can slide up and down in the cylinder space 70, and the second processing portion 20 slides up and down by the sliding of the piston body 72, and the first processing surface 1.
- the gap between the second processing surface 2 can be changed.
- a pressure source such as a compressor and the first nozzle 73 are connected, and air pressure, that is, positive pressure is applied from the first nozzle 73 to the piston body 72 in the cylinder space 70.
- the piston body 72 can be slid downward to narrow the gap between the first and second processing surfaces 1 and 2.
- a pressure source such as a compressor is connected to the second nozzle 74, and air pressure, that is, positive pressure is applied from the second nozzle 74 to the lower side of the piston body 72 in the cylinder space 70.
- the contact pressure can be adjusted by the air pressure obtained by the nozzles 73 and 74.
- the piston body 72 is set to abut on the uppermost part 70a of the cylinder space part 70.
- the uppermost portion 70a of the cylinder space 70 defines the upper limit of the width of the gap between the processing surfaces 1 and 2. That is, the piston body 72 and the uppermost portion 70a of the cylinder space 70 serve as a separation restraining portion that restrains the separation of the processing surfaces 1 and 2, and in other words, the maximum gap between the processing surfaces 1 and 2 is maximum. It functions as a mechanism that regulates the opening amount.
- the lowermost portion 70b of the cylinder space portion 70 is The lower limit of the width of the gap between the processing surfaces 1 and 2 is defined.
- the piston body 72 and the lowermost portion 70b of the cylinder space 70 serve as a proximity deterrence unit that deters the proximity of both processing surfaces 1 and 2, in other words, the minimum gap between the processing surfaces 1 and 2 It functions as a mechanism that regulates the opening amount.
- the gap z1 between the piston body 72 and the uppermost portion 70a of the cylinder space portion 70 in other words, between the piston body 72 and the lowermost portion 70b of the cylinder space portion 70, while restricting the maximum and minimum opening amounts of the gap.
- the interval z2 is adjusted by the air pressure of the nozzles 73 and 74.
- the nozzles 73 and 74 may be connected to separate pressure sources, or may be connected by switching or connecting one pressure source.
- the pressure source can be implemented by either a positive pressure supply or a negative pressure supply.
- a negative pressure source such as a vacuum is connected to the nozzles 73 and 74, the above operation is reversed.
- Such a cylinder mechanism 7 is provided in place of the other contact surface pressure applying mechanism 4 or as a part of the contact surface pressure applying mechanism 4 described above, and the nozzles 73 and 74 are provided depending on the viscosity and properties of the fluid to be processed.
- the pressure of the pressure source to be connected and the interval z1 and z2 are set, the thickness of the thin film fluid is set to the desired value, and a shearing force is applied to achieve a uniform mixed state (a uniform reaction if a reaction is involved). Particles can be generated.
- a cylinder mechanism 7 it is possible to forcibly open and close the sliding portion at the time of cleaning or steam sterilization to increase the reliability of cleaning and sterilization.
- the recesses 13... 13 can be implemented as curved or spirally extending on the first processing surface 1.
- the present invention can be carried out even if the individual concave portions 13 are bent in an L shape, and the concave portions 13 ... 13 extend straight radially as shown in FIG. 16 (C). Even if it is, it can be implemented.
- the recess 13 in FIGS. 16 (A) to 16 (C) is carried out with a gradient so as to become deeper toward the center side of the first processing surface 1.
- the groove-shaped recess 13 can be implemented even if it is continuous or intermittent. By forming such a concave portion 13, there are effects such as a response to an increase in the discharge amount of the fluid to be processed or a decrease in the heat generation amount, a cavitation control, and a fluid bearing effect.
- the recess 13 is formed on the first processing surface 1, but can also be formed on the second processing surface 2.
- the present invention can also be implemented by forming both the first and second processing surfaces 1 and 2.
- the influence of the surface roughness of the processing surfaces 1 and 2 on the fluid to be processed Is larger than that forming the recess 13. Therefore, in such a case, the smaller the particles of the fluid to be treated, the lower the surface roughness, that is, the finer the surface.
- the surface roughness of the processing surface should be the same as the above-described mirror surface, that is, the surface subjected to mirror finishing, in a uniform mixed state (in the case where reaction is accompanied).
- the inside of the case is all sealed. However, only the inside of the first processing unit 10 and the second processing unit 20 is sealed, and the outside is opened. It can also be implemented. That is, the flow path is sealed until it passes between the first processing surface 1 and the second processing surface 2, and the fluid to be processed receives all the pressure, but after passing, May be opened, and the treated fluid after treatment may not be subjected to pressure.
- the fluid pressure application mechanism p1 is preferably implemented by using a compressor as a pressurizing device. It can also be implemented using.
- the present invention can be implemented by constantly applying a constant pressure to the fluid to be treated by utilizing the weight of the fluid to be treated.
- a predetermined pressure is applied to the fluid to be processed, and the first processing is applied to the sealed fluid flow path through which the fluid to be processed that has received the predetermined pressure flows.
- the processing surface 1 and the second processing surface 2 are connected to each other at least two processing surfaces that can be moved toward and away from each other. 2
- a thin film fluid used for the seal in the mechanical seal is generated using the fluid to be processed, and reversely to the mechanical seal (the thin film fluid is used for the seal)
- the thin film fluid is intentionally leaked from between the first processing surface 1 and the second processing surface 2
- the processing of mixing reaction
- Realized and recovered between fluids A By such an epoch-making method, it is possible to adjust the distance between the processing surfaces 1 and 2 to be 1 ⁇ m to 1 mm, particularly 1 to 10 ⁇ m.
- the inside of the apparatus constitutes a closed fluid flow path, and the fluid pressure application mechanism p1 provided on the introduction part side (of the first fluid to be processed) of the processing apparatus, The fluid to be treated was pressurized.
- pressurization using such a fluid pressure applying mechanism p1 is not possible, and the flow path of the fluid to be processed can be opened even if it is open.
- 18 to 20 show an embodiment of such a processing apparatus.
- the processing apparatus an apparatus having a function of removing a liquid from a generated product and finally securing only a target solid (crystal) is illustrated.
- 18A is a schematic longitudinal sectional view of the processing apparatus
- FIG. 18B is a partially cutaway enlarged sectional view thereof.
- FIG. 19 is a plan view of the first processing unit 101 provided in the processing apparatus shown in FIG.
- FIG. 20 is a schematic vertical sectional view showing a part of the first and second processing parts 101 and 102 of the processing apparatus, partly cut away.
- the apparatus shown in FIGS. 18 to 20 is, as described above, charged with a fluid to be processed, that is, a fluid to be processed or a fluid that conveys the object to be processed under atmospheric pressure. .
- the second introduction part d2 is omitted and drawn (to be considered as a cross section at a position where the second introduction part d2 is not provided) in order to avoid complication of the drawings. ).
- the fluid processing apparatus includes a mixing apparatus G and a decompression pump Q.
- the mixing apparatus G includes a first processing unit 101 that is a rotating member, a first holder 111 that holds the processing unit 101, and a second processing unit 102 that is a member fixed to the case.
- the first processing unit 101 is moved together with the second holder 121 to which the second processing unit 102 is fixed, the urging mechanism 103, the dynamic pressure generation mechanism 104 (FIG. 19A), and the first holder 111.
- a drive unit that rotates, a housing 106, a first introduction part d1 that supplies (inputs) a first fluid to be processed, and a discharge part 108 that discharges fluid to the decompression pump Q are provided.
- the illustration of the drive unit is omitted.
- Each of the first processing unit 101 and the second processing unit 102 is an annular body formed by hollowing out the center of a cylinder. Both the processing parts 101 and 102 are members having the processing surfaces 110 and 120 as one bottom surface of a cylinder exhibited by each of the processing parts 101 and 102.
- the processing surfaces 110 and 120 have flat portions that are mirror-polished.
- the processing surface 120 of the second processing unit 102 is a flat surface in which the entire surface is mirror-polished.
- the processing surface 110 of the first processing unit 101 is entirely flat as in the second processing unit 102, but as shown in FIG. 19A, a plurality of grooves are formed in the flat surface. 112 ... 112.
- the surface roughness Ra is preferably set to 0.01 to 1.0 ⁇ m.
- Ra is more preferably 0.03 to 0.3 ⁇ m.
- the material of the processing parts 101 and 102 a hard material that can be mirror-polished is adopted.
- the hardness of the processing parts 101 and 102 at least a Vickers hardness of 1500 or more is preferable.
- SIC silicon carbide
- DLC diamond-like carbon
- the surface DLC coating is applied to the WC, ZrB 2 and BTC, boron ceramics with a Vickers hardness of 4000-5000 represented by B 4 C It is preferable to employ one.
- the housing 106 shown in FIG. 18 is a bottomed cylindrical body, although the illustration of the bottom is omitted, and the upper part is covered with the second holder 121.
- the second processing portion 102 is fixed to the lower surface, and the introduction portion d1 is provided above.
- the introduction part d1 includes a hopper 170 for introducing a fluid and an object to be processed from the outside.
- the drive unit includes a power source such as an electric motor and a shaft 50 that rotates upon receiving power from the power source.
- the shaft 50 is arranged inside the housing 106 and extends vertically.
- the first holder 111 is provided at the upper end of the shaft 50.
- the first holder 111 holds the first processing part 101, and is provided on the shaft 50 as described above, so that the processing surface 110 of the first processing part 101 is processed by the second processing part 102. It corresponds to the work surface 120.
- the first holder 111 is a cylindrical body, and the first processing portion 101 is fixed at the center of the upper surface.
- the first processing unit 101 is fixed so as to be integrated with the first holder 111 and does not change its position with respect to the first holder 111.
- a receiving recess 124 for receiving the second processing portion 102 is formed in the center of the upper surface of the second holder 121.
- the receiving recess 124 has an annular cross section.
- the second processing portion 102 is accommodated in the cylindrical receiving recess 124 so as to be concentric with the receiving recess 124.
- the structure of the receiving recess 124 is the same as that of the embodiment shown in FIG.
- the first processing portion 101 is the first ring 10
- the first holder 111 is the first holder 11
- the second processing is the second processing portion.
- the part 102 corresponds to the second ring 20 and the second holder 121 corresponds to the second holder 21).
- the second holder 121 includes the urging mechanism 103 described above.
- the urging mechanism 103 preferably uses an elastic body such as a spring.
- the urging mechanism 103 corresponds to the contact surface pressure applying mechanism 4 in FIG. 1A and adopts the same configuration. That is, the urging mechanism 103 presses the surface opposite to the processing surface 120 of the second processing portion 102, that is, the bottom surface, and positions each position of the second processing portion 102 on the first processing portion 101 side, that is, below. Energize evenly.
- the inner diameter of the receiving recess 124 is larger than the outer diameter of the second processing portion 102, so that when arranged concentrically as described above, the outer peripheral surface 102 b of the second processing portion 102 and the receiving recess 124.
- a gap t1 is set between the inner peripheral surface and the inner peripheral surface.
- a gap t2 is set between the inner peripheral surface 102a of the second processing portion 102 and the outer peripheral surface of the central portion 22 of the receiving recess 124 as shown in FIG.
- Each of the gaps t1 and t2 is for absorbing vibration and eccentric behavior, and is set to a size that can ensure the operating dimension or more and can be sealed.
- each of the gaps t1 and t2 is preferably 0.05 to 0.3 mm.
- the first holder 111 is integrally fixed to the shaft 50 and rotates together with the shaft 50.
- the second processing unit 102 does not rotate with respect to the second holder 121 due to the rotation stop.
- a clearance of 0.1 to 10 ⁇ m necessary for processing that is, a minute interval t shown in FIG. 20B, between both processing surfaces 110 and 120, as shown in FIG. 18B.
- a gap t3 is provided between the bottom surface of the receiving recess 124, that is, the top portion, and the top portion 124a of the second processing portion 102, that is, the top surface.
- the gap t3 is set in consideration of the deflection and elongation of the shaft 50 together with the clearance.
- the first processing unit 101 is variable in the direction z1 that approaches and separates from the second processing unit 102.
- the tilt direction z2 of the processing surface 110 is variable. That is, in this embodiment, the urging mechanism 103 and the gaps t1 to t3 constitute a floating mechanism, and at least the center and the inclination of the second processing unit 102 are several ⁇ m to several ⁇ m by this floating mechanism. A slight amount of about mm is variable. As a result, the center axis of the rotating shaft, the axial expansion, the surface deflection and vibration of the first processing unit 101 are absorbed.
- the groove 112 provided in the processing surface 110 of the first processing unit 101 will be described in more detail.
- the rear end of the groove 112 reaches the inner peripheral surface 101a of the first processing part 101, and the front end extends toward the outside y of the first processing part 101, that is, the outer peripheral surface side.
- the groove 112 has a cross-sectional area from the center x side of the annular first processing portion 101 toward the outer side y of the first processing portion 101, that is, the outer peripheral surface side. It is supposed to gradually decrease.
- the distance w1 between the left and right side surfaces 112a and 112b of the groove 112 decreases from the center x side of the first processing portion 101 toward the outside y of the first processing portion 101, that is, the outer peripheral surface side. Further, as shown in FIG. 19B, the depth w2 of the groove 112 decreases from the center x side of the first processing portion 101 toward the outside y of the first processing portion 101, that is, the outer peripheral surface side. Become. That is, the bottom 112c of the groove 112 becomes shallower from the center x side of the first processing part 101 toward the outer side y of the first processing part 101, that is, the outer peripheral surface side.
- the groove 112 gradually decreases in both the width and the depth toward the outer side y, assuming that both the width and the depth gradually decrease toward the outer side y, that is, the outer peripheral surface side.
- channel 112 is a dead end. That is, the tip of the groove 112, that is, the y side does not reach the outer peripheral surface 101b of the first processing portion 101, and the outer flat surface 113 is interposed between the tip of the groove 112 and the outer peripheral surface 101b.
- the outer flat surface 113 is a part of the processing surface 110.
- the left and right side surfaces 112a and 112b and the bottom 112c of the groove 112 constitute a flow path restricting portion.
- the flow path restricting portion, the flat portion around the groove 112 of the first processing portion 101, and the flat portion of the second processing portion 102 constitute a dynamic pressure generating mechanism 104.
- only one of the width and depth of the groove 112 may reduce the cross-sectional area by adopting the above configuration.
- a minute interval of 0.1 to 10 ⁇ m can be generated between the processing surfaces 110 and 120.
- Such a minute interval may be adjusted and selected according to the object of processing, but is preferably 1 to 6 ⁇ m, and more preferably 1 to 2 ⁇ m.
- this apparatus it is possible to realize an unprecedented uniform mixing state (a uniform reaction in the case where a reaction is involved) and generation of fine particles by the above-described minute intervals.
- Each of the grooves 112... 112 can be implemented even if it extends straight from the center x side to the outer side y. However, in this embodiment, as shown in FIG. 19A, the center x side of the groove 112 precedes the outer side y of the groove 112 in the rotational direction r of the first processing portion 101.
- the groove 112 is curved and extends so as to be positioned forward. In this way, the grooves 112... 112 are curved and extended, so that the separation force can be generated more effectively by the dynamic pressure generation mechanism 104.
- the first fluid R to be processed that is introduced from the hopper 170 and passes through the first introduction part d1 passes through the hollow part of the annular second processing part 102 and passes through the first part.
- the processing surface 110 of the first processing unit 101 and the processing surface 120 of the second processing unit 102 that enter and rotate between the processing units 101 and 102 under the centrifugal force due to the rotation of the processing unit 101 and the processing surface 120 of the second processing unit 102 In between, uniform mixing (reaction) and, in some cases, generation of fine particles are performed. Thereafter, the particles exit outside the processing units 101 and 102 and are discharged from the discharge unit 108 to the decompression pump Q side.
- the first treated fluid R is simply referred to as a fluid R as necessary).
- the fluid R that has entered the hollow portion of the annular second processing portion 102 first enters the groove 112 of the rotating first processing portion 101 as shown in FIG.
- both the processing surfaces 110 and 120 that are mirror-polished and are flat portions are kept airtight even through a gas such as air or nitrogen. Therefore, even if the centrifugal force due to the rotation is received, the fluid R cannot enter from the groove 112 between the processing surfaces 110 and 120 pressed together by the biasing mechanism 103.
- the fluid R gradually strikes the both side surfaces 112a, 112b and the bottom 112c of the groove 112 formed as the flow path restricting portion, and generates a dynamic pressure that works in a direction that separates both the processing surfaces 110, 120. As shown in FIG. 20B, this allows the fluid R to ooze out from the groove 112 to the flat surface, and to secure a minute interval t, that is, a clearance between the processing surfaces 110 and 120. Then, uniform mixing (reaction) and, in some cases, generation of fine particles are performed between such mirror-polished flat surfaces. In addition, the above-described curvature of the groove 112 more reliably causes the centrifugal force to act on the fluid, thereby making the generation of the dynamic pressure more effective.
- this fluid processing apparatus ensures a fine and uniform interval, that is, clearance, between both mirror surfaces, that is, the processing surfaces 110 and 120, by balancing the dynamic pressure and the urging force by the urging mechanism 103. It was possible. And by said structure, the said micro space
- the floating mechanism is a mechanism provided only in the second holder 121.
- a floating mechanism can be provided also in the first holder 111.
- FIGS. 21 to 23 show other embodiments of the groove 112 described above.
- the groove 112 can be implemented as having a flat wall surface 112d at the tip as a part of the flow path restricting portion.
- a step 112e is provided between the first wall surface 112d and the inner peripheral surface 101a in the bottom 112c, and this step 112e also forms a part of the flow path restricting portion.
- the groove 112 includes a plurality of branch portions 112f... 112f that branch into a plurality of portions, and each branch portion 112f includes a flow path restriction portion by narrowing the width thereof. It can also be implemented.
- configurations other than those specifically shown are the same as those of the embodiments shown in FIGS. 1 (A), 11 (C), and 18 to 20.
- the flow path restriction is achieved by gradually reducing the size of at least one of the width and the depth of the groove 112 from the inner side to the outer side of the first processing portion 101.
- the part was to be configured.
- the end surface 112f can be used as a flow path restriction unit.
- the generation of dynamic pressure is achieved by changing the width and depth of the groove 112 as described above so that the bottom and both side surfaces of the groove 112 are inclined surfaces.
- the end surface of the groove 112 serves as a pressure receiving portion for the fluid to generate dynamic pressure.
- the configuration of the groove 112 is not limited to that shown in FIGS. 19 and 21 to 23 described above, and the groove 112 can be implemented as having a channel restricting portion having another shape. For example, in the case shown in FIGS. 19 and 21 to 23, the groove 112 does not penetrate to the outside of the first processing portion 101.
- the outer flat surface 113 exists between the outer peripheral surface of the first processing unit 101 and the groove 112.
- the present invention is not limited to such an embodiment, and the groove 112 reaches the outer peripheral surface side of the first processing portion 101 as long as the above-described dynamic pressure can be generated.
- it can be implemented.
- a portion having a smaller cross-sectional area than other portions of the groove 112 is formed on the outer flat surface 113. Can do.
- the groove 112 is formed so that the cross-sectional area gradually decreases from the inside to the outside as described above, and the portion (terminal) of the groove 112 reaching the outer periphery of the first processing portion 101 has the largest cross-sectional area. It may be small (not shown). However, in order to effectively generate the dynamic pressure, it is preferable that the groove 112 does not penetrate to the outer peripheral surface side of the first processing portion 101 as shown in FIGS. 19 and 21 to 23.
- FIGS. 18 to 23 will be summarized.
- a rotating member having a flat processing surface and a fixing member having the same flat processing surface are concentrically opposed to each other by the flat processing surface, and the opening of the fixing member is rotated under the rotation of the rotating member.
- a pressure increasing mechanism is provided on the rotating member to generate the pressure.
- the rotating member and the fixed member have a flat processing surface on the outer peripheral portion thereof, and the flat processing surface has a sealing function on the surface, so that it is hydrostatic or hydrostatic. It is an object of the present invention to provide a fluid processing apparatus of a high-speed rotation type that generates a large force, a hydrodynamic or hydrodynamic force, or an aerostatic-aerodynamic force. The above force can generate a slight gap between the sealing surfaces, and can provide a fluid processing apparatus that is non-contact, mechanically safe, and has a function of highly uniform mixing (reaction).
- the decompression pump Q is connected to the discharge portion of the mixing apparatus G.
- the housing 106 is not provided, and the decompression pump Q is not provided.
- the processing apparatus can be a tank T for pressure reduction, and the mixing apparatus G can be disposed in the tank T. In this case, by reducing the pressure in the tank T to a vacuum or a state close to a vacuum, the object to be processed generated by the mixing device G is sprayed into the tank T in a mist form, and hits the inner wall of the tank T and flows down.
- the pressure reducing pump Q as shown in FIG. 24B, by connecting an airtight tank T to the mixing device G via the pressure reducing pump Q, processing is performed in the tank T.
- the object to be processed can be separated and extracted by atomizing the object to be processed later.
- the decompression pump Q is directly connected to the tank T, and the decompression pump Q and a discharge part of the fluid R different from the decompression pump Q are connected to the tank T.
- the target product can be separated. In this case, the vaporizing part is sucked by the decompression pump Q, and the liquid R (liquid part) is discharged from the discharging part separately from the vaporizing part.
- the first and second fluids to be treated are introduced from the second holders 21 and 121 and the second rings 20 and 102, respectively, and mixed (reacted). Indicated. Next, other embodiments relating to the introduction of the fluid to be processed into the apparatus will be described in order.
- the processing apparatus shown in FIG. 1 (A) is provided with a third introduction part d3 to introduce a third fluid to be processed between the processing surfaces 1 and 2, Similar to the second fluid to be treated, the first fluid to be treated can be mixed (reacted).
- the third introduction part d3 supplies the third processed fluid to be mixed with the first processed fluid between the processing surfaces 1 and 2.
- the third introduction part d3 is a fluid passage provided inside the second ring 20, one end of which opens at the second processing surface 2, and the other end has a third fluid.
- the supply part p3 is connected. A compressor and other pumps can be employed for the third fluid supply part p3.
- the opening in the second processing surface 2 of the third introduction part d3 is located outside the center of rotation of the first processing surface 1 relative to the opening of the second introduction part d2. That is, on the second processing surface 2, the opening of the third introduction part d3 is located on the downstream side of the opening of the second introduction part d2. A gap is provided between the opening of the third introduction part d3 and the opening of the second introduction part d2 in the inner and outer directions of the diameter of the second ring 20.
- the apparatus shown in FIG. 1 (B) is the same as the embodiment shown in FIG. 1 (A) except for the third introduction part d3. In FIG. 1B, and in FIGS.
- case 3 is omitted in order to avoid complication of the drawing.
- FIG. 9 (B) (C) FIG. 10, FIG. 11 (A) (B), a part of case 3 is drawn.
- the processing apparatus shown in FIG. 1B is provided with a fourth introduction part d4 to introduce the fourth fluid to be processed between the processing surfaces 1 and 2. And it can implement also as what is mixed (reacted) to the 1st to-be-processed fluid like the 2nd and 3rd to-be-processed fluid.
- the fourth introduction part d4 supplies the fourth processed fluid to be mixed with the first processed fluid between the processing surfaces 1 and 2.
- the fourth introduction part d4 is a fluid passage provided inside the second ring 20, one end of which opens at the second processing surface 2, and the other end has a fourth fluid.
- the supply part p4 is connected.
- a compressor or other pump can be employed.
- the opening in the second processing surface 2 of the fourth introduction part d4 is located outside the center of rotation of the first processing surface 1 relative to the opening of the third introduction part d3. That is, in the second processing surface 2, the opening of the fourth introduction part d4 is located on the downstream side of the opening of the third introduction part d3.
- the apparatus shown to this FIG.1 (C) about structure other than the 4th introduction part d4, it is the same as that of embodiment shown to FIG.1 (B).
- the second introduction part d2 is provided in the apparatus of FIG. 1A.
- the opening of the first introduction part d1 is located closer to the center of rotation, that is, the upstream side than the second introduction part d2.
- the opening of the second introduction part d2 and the opening of the third introduction part d3 are both arranged on the second processing surface 2 of the second ring 20. there were.
- the opening of the introduction part is not limited to such an arrangement with respect to the processing surface. In particular, as shown in FIG.
- the opening of the second introduction part d2 may be provided at a position adjacent to the second processing surface 2 on the inner peripheral surface of the second ring 20.
- the opening of the third introduction part d3 is arranged on the second processing surface 2 as in the apparatus shown in FIG. 1B, but the second introduction part d2
- the second fluid to be treated is immediately introduced into the processing surface by arranging the opening in the second processing surface 2 at a position adjacent to the second processing surface 2 in this manner. it can.
- the opening of the first introduction part d1 is provided in the second holder 21, and the opening of the second introduction part d2 is located inside the second processing surface 2 and adjacent to the second processing surface 2. (In this case, it is not essential to provide the third introduction part d3).
- the fluid to be treated introduced from the first introduction part d1.
- the to-be-processed fluid introduced from the second introduction part d2 can be introduced between the processing surfaces 1 and 2 in a state where they are not reacted, and both can be reacted for the first time between the processing surfaces 1 and 2. Therefore, the said structure is suitable especially when using the to-be-processed fluid with high reactivity.
- the “adjacent” described above is not limited to the case where the opening of the second introduction portion d2 is provided so as to contact the inner side surface of the second ring 20 as shown in FIG. .
- the distance from the second ring 20 to the opening of the second introduction part d2 is such that the mixing (reaction) is not completely performed before the plurality of fluids to be processed are introduced between the processing surfaces 1 and 2.
- it may be provided at a position close to the second ring 20 of the second holder 21.
- the apparatus shown in FIG. 1B there is an interval between the opening of the third introduction part d3 and the opening of the second introduction part d2 in the inner and outer directions of the diameter of the second ring 20. 2B.
- FIG. 2 (B) when the second and third fluids to be processed are introduced between the processing surfaces 1 and 2 without providing such an interval, It can also be implemented as a combination of fluids.
- Such an apparatus shown in FIG. 2B may be selected depending on the processing target.
- the distance between the opening of the first introduction part d1 and the opening of the second introduction part d2 is about the inner and outer directions of the diameter of the second ring 20.
- the first and second fluids to be treated are introduced between the processing surfaces 1 and 2, and both fluids can be immediately merged. (Not shown). What is necessary is just to select arrangement
- the opening of the third introduction part d3 on the second processing surface 2 is located downstream of the opening of the second introduction part d2.
- the second ring 20 is disposed outside the opening of the second introduction part d2 in the inner and outer directions of the diameter.
- the opening of the third introduction part d 3 is replaced with the opening of the second introduction part d 2 and the second ring 20. It can also be implemented as being arranged at different positions in the circumferential direction r0.
- m1 represents the opening of the first introduction part d1, that is, the first opening
- m2 represents the opening of the second introduction part d2
- m3 represents the opening of the third introduction part d3 (the first opening).
- r1 indicates the inner and outer directions of the ring diameter.
- the opening of the first introduction part d1 is formed on the second processing surface 2 with respect to the second introduction part d2. It can implement also as what arrange
- the processing surface 2 of the second ring 20 is shown in which the openings of the two introduction portions are arranged at different positions in the circumferential direction r0.
- the openings of the three introduction portions are arranged at different positions in the circumferential direction r0 of the ring, or four introduction portions are arranged at different positions in the circumferential direction r0 of the ring as shown in FIG. It can also be carried out by arranging openings.
- m4 represents the opening of the fourth introduction part
- m5 in FIG. 3C represents the opening of the fifth introduction part.
- the opening of the introduction part may be provided by providing five or more openings at different positions in the circumferential direction r0 of the ring.
- the second introduction unit to the fifth introduction unit can introduce different fluids to be treated, that is, second, third, fourth, and fifth fluids to be treated.
- the same kind of, that is, the second fluid to be processed can be introduced between the processing surfaces through the second to fifth openings m2 to m5.
- the second introduction unit to the fifth introduction unit communicate with each other inside the ring and can be implemented as being connected to one fluid supply unit, that is, the second fluid supply unit p2. .
- each of the outer openings may be provided at the same position as the inner opening in the circumferential direction r0 of the ring, but in consideration of the rotation of the ring, as shown in FIG. It can also be carried out by providing at different positions in the circumferential direction r0 of the ring.
- the opening is not limited to the arrangement and number shown in FIG.
- the radially outer opening is arranged at the vertex position of a polygon, that is, in this case, the vertex position of a quadrangle, and the radially inner opening is located on the side of the polygon. It can also arrange so that it may be located. Of course, other arrangements are possible.
- the openings for introducing each second fluid to be treated are treated.
- the circumferential direction r0 can be implemented as a continuous opening.
- the second introduction part d2 provided in the second ring 20 in the apparatus shown in FIG. 1 (A) is similar to the first introduction part d1. It can also be carried out by providing the central portion 22 of the second holder 21. In this case, the opening of the second introduction part d2 is positioned outside the opening of the first introduction part d1 located at the center of the second ring 20 with a gap therebetween.
- the 3rd introduction part d3 can also be provided in the 2nd ring 20, and it can implement.
- FIG. 4C in the apparatus shown in FIG.
- the present invention can be implemented even if both fluids merge immediately when the first and second fluids to be treated are introduced into the inner space.
- the third introduction part d3 is also provided in the second holder 21 in the same manner as the second introduction part d2. be able to.
- the fourth ring d4 is provided in the second ring 20, and the fourth fluid to be processed is subjected to both processing. It can also be implemented as an installation between the working surfaces 1 and 2.
- the second introduction part d2 is provided in the first ring 10, and the first processing surface 1 is provided with the opening of the second introduction part d2. It can also be implemented.
- the third introduction part d3 is provided in the first ring 10, and the opening of the third introduction part d3 is formed on the first processing surface 1. Further, the present invention can be carried out by disposing the opening of the second introduction part d2 and the circumferential position of the first ring 10 at different positions.
- FIG. 5 (D) in the apparatus shown in FIG.
- the first introduction part d1 is provided in the second ring 20, and second processing is performed. It can also be implemented by arranging the opening of the first introduction part d1 on the work surface 2. In this case, both openings of the first and second introduction portions d1 and d2 are arranged at the same position in the inner and outer directions of the diameter of the ring.
- the third introduction part d3 is provided in the first ring 10, and the opening of the third introduction part d3 is provided in the first processing surface 1. It can also be implemented as an arrangement. In this case, both openings of the second and third introduction portions d2 and d3 are arranged at the same position in the inner and outer directions of the diameter of the ring. However, it is good also as what arrange
- both the opening portions of the second and third introduction portions d2 and d3 are provided at the same position in the inner and outer directions of the diameter of the first ring 10, and the circumferential direction of the first ring 10 is provided. That is, although provided in different positions in the rotational direction, in the apparatus, as shown in FIG. 6B, both openings of the second and third introduction parts d2 and d3 are located at the same position in the circumferential direction of the first ring 10.
- the first ring 10 may be provided at different positions in the inner and outer directions of the diameter of the first ring 10. In this case, as shown in FIG.
- the second and third introduction portions d2 and d3 may be provided with an interval in the inner and outer directions of the diameter of the first ring 10 between the openings.
- the second treated fluid and the third treated fluid may be immediately joined without opening the interval.
- the first introduction part d1 instead of providing the first introduction part d1 in the second holder 21, the first introduction part d1 may be provided in the first ring 10 together with the second introduction part d2. it can.
- the opening of the first introduction part d ⁇ b> 1 is provided upstream of the opening of the second introduction part d ⁇ b> 2 (inside in the inner and outer directions of the diameter of the first ring 10).
- a gap is provided between the opening of the first introduction part d1 and the opening of the second introduction part d2 in the inner and outer directions of the diameter of the first ring 10.
- the present invention can be carried out without such an interval.
- the first introduction part d1 and the second introduction part 1 are located at different positions in the circumferential direction of the first ring 10 on the first processing surface 1 of the apparatus shown in FIG. 6 (C). It can be implemented as arranging the opening of each introduction part d2.
- three or more introduction portions are provided in the first ring 10, and the circumferential positions on the second processing surface 2 are different.
- each opening may be arranged at a different position in the inner and outer directions of the diameter of the ring.
- the arrangement of the openings shown in FIGS. 3B to 3F adopted in the second processing surface 2 can also be adopted in the first processing surface 1.
- the second introduction part d2 can be provided in the first holder 11 instead of being provided in the second ring 20.
- the opening of the second introduction part d2 is arranged at the center of the central axis of rotation of the first ring 10 in a portion surrounded by the first ring 10 on the upper surface of the first holder 11.
- the third introduction part d3 is provided in the second ring 20, and the opening of the third introduction part d3 is provided on the second processing surface. 2 can be arranged. Further, as shown in FIG.
- the first introduction part d ⁇ b> 1 can be provided in the first holder 11 instead of being provided in the second holder 21.
- the second introduction part d2 can be provided in the first ring 10 and the opening can be arranged in the first processing surface 1.
- the second introduction part d2 can be provided in the second ring 20, and the opening can be arranged in the second processing surface 2.
- FIG. 7D the second introduction part d2 shown in FIG.
- the opening of the second introduction part d2 is arranged at a part surrounded by the first ring 10 on the upper surface of the first holder 11.
- the second introduction part d2 provided in the second ring 20 may be the third introduction part d3.
- the first holder 11 and the first ring 10 are rotated with respect to the second holder 21 and the second ring 20.
- the second holder 2 is provided with a rotating shaft 51 that rotates by receiving a rotational force from the rotation driving unit, and the first holder 11 It can also be implemented as rotating the second holder 21 in the opposite direction.
- the rotation driving unit for the rotating shaft 51 may be provided separately from the rotating shaft 50 of the first holder 11 or the rotating shaft 50 of the first holder 11 is rotated by power transmission means such as a gear. It can also be implemented as receiving power from the drive unit.
- the second holder 21 is formed separately from the above-described case and is rotatably accommodated in the case like the first holder 11.
- the first holder 11 is provided in the same manner as in the apparatus of FIG. 7B.
- the second introduction part d2 can be provided in the embodiment.
- the second introduction part d ⁇ b> 2 can be provided in the second holder 21 instead of the first holder 11.
- the second introduction part d2 is the same as the apparatus of FIG.
- FIG. 8C in the apparatus shown in FIG.
- the second ring 20 is provided with the third introduction part d3, and the opening part of the introduction part d3 is arranged on the second processing surface 2. It can also be implemented. Further, as shown in FIG. 8D, the first holder 11 can be rotated without rotating the second holder 21 alone. Although not shown, the apparatus shown in FIGS. 1B to 7 can also be implemented by rotating the second holder 21 together with the first holder 11 or rotating only the second holder 21 alone.
- the second processing unit 20 is a ring
- the first processing unit 10 is not a ring, but a direct rotating shaft 50 similar to the first holder 11 of the other embodiments. It can be set as the member which rotates by providing.
- the upper surface of the first processing portion 10 is the first processing surface 1, and the processing surface is not an annular shape, that is, a flat surface having no hollow portion.
- the second introduction part d2 is provided in the second ring 20, and the opening is arranged in the second processing surface 2. ing.
- the second holder 21 is independent of the case 3, and the second ring 20 is interposed between the case 3 and the second holder 21.
- the contact surface pressure applying mechanism 4 such as an elastic body that approaches and separates from the first processing portion 10 provided with the above-described structure may be provided.
- the second processing portion 20 is not a ring but a member corresponding to the second holder 21, and the lower surface of the member is the second processing surface 2.
- the first processing unit 10 is not a ring, but is similar to the apparatus shown in FIGS. 9 (A) and 9 (B).
- the portion corresponding to the first holder 11 can be used as the first processing portion 10, and the upper surface thereof can be used as the first processing surface 1.
- At least the first fluid to be processed is supplied from the first processing part 10 and the second processing part 20, that is, from the central part of the first ring 10 and the second ring 20.
- the treatment with the fluid to be treated that is, mixing (reaction)
- the inside and outside directions of the diameter were discharged to the outside.
- FIG. 10 (B) it can implement also as what supplies a 1st to-be-processed fluid toward the inner side from the outer side of the 1st ring 10 and the 2nd ring 20.
- the outer sides of the first holder 11 and the second holder 21 are hermetically sealed with the case 3, and the first introduction part d1 is provided directly on the case 3 so that both the rings 10 are inside the case.
- the opening of the introduction part is arranged at a part corresponding to the butting position.
- the discharge part 36 is provided in the position used as the center of the ring 1 in the 1st holder 11, ie, the position where the 1st introduction part d1 was provided in the device of Drawing 1 (A).
- the opening of the second introduction part d2 is arranged on the opposite side of the opening of the case across the central axis of rotation of the holder.
- the opening of the second introduction part d2 may be located inside the case and at the part corresponding to the butting position of both the rings 10 and 20 like the opening of the first introduction part d1.
- the present invention is not limited to being formed on the opposite side of the opening of the first introduction part d1. In this case, the outside of the diameters of both rings 10 and 20 is upstream, and the inside of both rings 10 and 20 is downstream.
- the first processing portion 1 is formed on the first processing surface 1 of the first processing portion 10. It is also possible to carry out by forming groove-like recesses 13... 13 extending from the outer side of 10 toward the center side. By forming such recesses 13... 13, the balance ratio K is preferably an unbalanced type of 100% or more. As a result, dynamic pressure is generated in the groove-like recesses 13... 13 during rotation, and both the processing surfaces 1 and 2 can be reliably rotated without contact, and there is no danger of wear due to contact. In the embodiment shown in FIG. 16E, the separation force due to the pressure of the fluid to be processed is generated at the inner end 13 a of the recess 13.
- the second introduction part d2 provided in the side part of the case 3 is provided in the first ring 10 instead of the position, and the opening part is provided. Can also be carried out by arranging them on the first processing surface 1.
- the first processing unit 10 is not formed as a ring, but is similar to the apparatus shown in FIGS. 9A, 9B, and 10A.
- a portion corresponding to the first holder 11 is a first processing portion 10, an upper surface thereof is a first processing surface 1, and a second introduction portion is further provided in the first processing portion 10.
- d2 may be provided, and the opening may be disposed on the first processing surface 1.
- the second processing portion 20 is not formed as a ring, but a member corresponding to the second holder 21 in the other embodiment is used.
- the second processing unit 20 can be used, and the lower surface thereof can be used as the second processing surface 2.
- the second processing unit 20 is a member independent of the case 3, and between the case 3 and the second processing unit 20, the apparatus shown in FIGS. 9B, 9 C, and 10 A.
- the same contact pressure application mechanism 4 can be provided and implemented.
- the second introduction part d2 of the apparatus shown in FIG. 11A can be used as the third introduction part d3, and the second introduction part d2 can be provided separately.
- the opening of the second introduction part d2 is arranged on the downstream side of the opening of the third introduction part d3 on the second processing surface 2.
- the other fluid to be treated merges with the first fluid to be treated, and is not suitable for a material having a fast crystallization or precipitation reaction. However, such a device can also be employed for those having a slow reaction rate.
- the fluid processing apparatus includes a fluid pressure applying mechanism that applies a predetermined pressure to the fluid to be processed, and a first fluid channel that is provided in a sealed fluid flow path through which the fluid to be processed having the predetermined pressure flows.
- a fluid pressure applying mechanism that applies a predetermined pressure to the fluid to be processed
- a first fluid channel that is provided in a sealed fluid flow path through which the fluid to be processed having the predetermined pressure flows.
- At least two processing parts of the second processing part 20 that are relatively close to and away from the processing part 10 and the first processing part 10, and the processing parts 10 and 20, at positions facing each other.
- At least two processing surfaces of the first processing surface 1 and the second processing surface 2 provided, and a rotation drive mechanism that relatively rotates the first processing portion 10 and the second processing portion 20.
- At least the second processing unit 20 of the first processing unit 10 and the second processing unit 20 includes a pressure receiving surface, and at least a part of the pressure receiving surface is constituted by the second processing surface 2.
- the pressure receiving surface receives a pressure applied to at least one of the fluids to be processed by the fluid pressure applying mechanism and generates a force for moving the second processing surface 2 away from the first processing surface 1.
- this fluid processing apparatus it is preferable to employ a device provided with a buffer mechanism for adjusting fine vibration and alignment of at least one of the first processing surface 1 and the second processing surface 2.
- the thin film fluid between the processing surfaces 1 and 2 is adjusted by adjusting the axial displacement of one or both of the first processing surface 1 and the second processing surface 2 due to wear or the like. It is preferable to employ a mechanism having a displacement adjusting mechanism that can maintain the thickness.
- a pressurizing apparatus such as a compressor that applies a constant feeding pressure to the fluid to be processed can be employed as the fluid pressure applying mechanism.
- the separation between the first processing surface 1 and the second processing surface 2 is defined so as to prevent further separation between the processing surfaces 1 and 2.
- a thing provided with a deterrent part can be adopted.
- a minimum distance between the first processing surface 1 and the second processing surface 2 is defined, and further proximity of both processing surfaces 1 and 2 is suppressed.
- a thing provided with a proximity deterrent part can be adopted.
- the fluid processing apparatus may be one having a temperature adjusting jacket for adjusting the temperature of one or both of the first processing surface 1 and the second processing surface 2.
- At least a part of one or both of the first processing surface 1 and the second processing surface 2 is mirror-finished for the fluid processing apparatus.
- one or both of the first processing surface 1 and the second processing surface 2 may be provided with a recess.
- the fluid processing apparatus includes a separate introduction path that is independent from the passage of the one fluid to be treated, as supply means for the other fluid to be treated that is mixed (reacted) with one fluid to be treated.
- the at least one of the first processing surface and the second processing surface is provided with an opening that leads to the separate introduction path, and the other fluid to be processed that has been sent from the separate introduction path, It is preferable to employ one that can be introduced into the one fluid to be treated.
- a fluid pressure applying mechanism for applying a predetermined pressure to the fluid to be processed and a sealed fluid flow path through which the fluid to be processed having the predetermined pressure flows are connected. At least two processing surfaces that are relatively close to and away from the first processing surface 1 and the second processing surface 2, and a contact surface pressure applying mechanism that applies a contact pressure between the processing surfaces 1 and 2. And a rotational drive mechanism that relatively rotates the first processing surface 1 and the second processing surface 2, thereby providing at least two kinds of fluids to be processed between the processing surfaces 1 and 2. Between the first processing surface 1 and the second processing surface 2 that rotate relative to each other while the contact surface pressure is applied, pressure is applied from the fluid pressure application mechanism.
- At least one kind of fluid to be treated is passed, and another kind of fluid to be treated is passed.
- the one kind of fluid to be treated that has been pressurized by the fluid pressure imparting mechanism passes between the processing surfaces 1 and 2 while forming a thin film fluid having a predetermined thickness
- a material to be treated can be mixed and a desired mixed state (reaction) can be generated between the fluids to be treated.
- This contact surface pressure imparting mechanism can be implemented as a buffer mechanism or a displacement adjustment mechanism for adjusting fine vibrations and alignment in the above-described apparatus.
- a first introduction part for introducing at least one of the two treatment fluids to be mixed (reacted) into the apparatus, and a first introduction part A fluid pressure applying mechanism p that is connected to apply pressure to the one processed fluid, and a second introduction unit that introduces at least one of the two processed fluids to be mixed (reacted) into the apparatus.
- a first processing unit 10 and a second processing unit that are relatively close to and away from the first processing unit 10 provided in a sealed fluid flow path through which the one fluid to be processed flows.
- a holder 21 that receives the rotation, a rotational drive mechanism that relatively rotates the first processing unit 10 and the second processing unit 20, and the second processing surface 2 is pressed against the first processing surface 1.
- a contact surface pressure applying mechanism 4 that presses the second processing portion 20 in a close state, and performs a mixing (reaction) process between the fluids to be processed between the processing surfaces 1 and 2. 21 is provided with the opening of the first introduction part and is not movable so as to affect the gap between the processing surfaces 1 and 2, the first treatment part 10 and the second introduction part 20.
- At least one includes the opening of the second introduction portion, the second processing portion 20 is an annular body, and the second processing surface 2 slides with respect to the holder 21 so that the first processing surface 1
- the second processing unit 20 includes a pressure receiving surface, and the pressure receiving surface is formed by the fluid pressure applying mechanism p and the fluid to be processed. In response to the applied pressure, a force for moving the second processing surface 2 away from the first processing surface 1 is generated, and at least a part of the pressure receiving surface is configured by the second processing surface 2.
- One of the fluids to be treated is passed between the first processing surface 1 and the second processing surface 2 that can move toward and away from each other, and the other one of the processing surfaces.
- the fluids to be processed pass between the processing surfaces 1 and 2 while forming a thin film fluid having a predetermined thickness.
- desired mixing between the fluids to be processed is promoted, and the contact surface pressure of the contact surface pressure applying mechanism 4 and the fluid applied by the fluid pressure applying mechanism p.
- the thin film fluid having a predetermined thickness is balanced by the balance between the pressure and the force separating the processing surfaces 1 and 2. It is possible to employ one that keeps a minute interval between the two processing surfaces 1 and 2 to generate the.
- the second introduction unit can also be implemented by being connected to a separate fluid pressure imparting mechanism similar to that connected to the first introduction unit and pressurized.
- the fluid to be treated introduced from the second introduction part is not pressurized by a separate fluid pressure applying mechanism, but by the fluid pressure of the fluid to be treated introduced by the first introduction part.
- the present invention can also be implemented by sucking and supplying between the processing surfaces 1 and 2 due to the negative pressure generated in the second introduction part.
- the other fluid to be processed can be implemented by moving in the second introduction portion by its own weight, that is, flowing downward from above and supplied between the processing surfaces 1 and 2.
- the opening of the first introduction part that serves as a supply port for one of the fluids to be processed is not limited to the one provided in the second holder, but the opening of the first introduction part. May be provided on the first holder.
- transducing part can also be formed and formed in at least one of both processing surfaces.
- the opening of the second introduction part that serves as a supply port needs to be arranged downstream of the opening of the first introduction part on any of the processing surfaces.
- the fluid processing apparatus includes a plurality of introduction units that separately introduce two or more types of fluids to be mixed (reacted), and a fluid pressure that applies pressure to at least one of the two or more types of fluids to be processed.
- the second processing unit that is relatively close to and away from the first processing unit 10 and the first processing unit 10 provided in the sealed fluid flow path through which the fluid to be processed flows. At least two processing surfaces of the unit 20, and at least two processing surfaces 1 of the first processing surface 1 and the second processing surface 2 provided at positions facing each other in the processing units 10 and 20.
- the second processing portion 20 includes a pressure receiving surface, and at least a part of the pressure receiving surface is constituted by the second processing surface 2, and the fluid pressure applying mechanism is a fluid to be processed. In response to the pressure applied to the first processing surface 1, a force is generated to move the second processing surface 2 away from the first processing surface 1, and the second processing portion 20 is opposite to the second processing surface 2.
- the approaching adjustment surface 24 faces the side, and the approaching adjustment surface 24 receives a predetermined pressure applied to the fluid to be treated and causes the second processing surface 2 to approach the first processing surface 1.
- the resultant force of the total pressure received from the fluid to be treated is generated by the area ratio between the projected area in the approaching / separating direction of the approach adjusting surface 24 and the projected area in the approaching / separating direction of the pressure receiving surface.
- the second processing surface 2 moves away from the first processing surface 1.
- the fluid to be treated is passed between the first processing surface 1 and the second processing surface 2 that are capable of approaching, separating, and relatively rotating, and the processed fluid.
- the other fluids to be mixed (reacted) with the body are mixed between the processing surfaces, and the mixed fluid passes between the processing surfaces 1 and 2 while forming a thin film fluid having a predetermined thickness. By doing so, a desired product is obtained while passing between the processing surfaces.
- a predetermined pressure is applied to the first fluid to be processed, and the fluid to be processed that has received the predetermined pressure is sealed.
- the contact surface pressure that connects at least two processing surfaces that are relatively close to and away from each other, that is, the first processing surface 1 and the second processing surface 2, to the two fluid flow paths.
- the first processing surface 1 and the second processing surface 2 are relatively rotated, and a fluid to be processed is introduced between the processing surfaces 1 and 2.
- a second treated fluid to be mixed (reacted) with the body is introduced between the processing surfaces 1 and 2 through the above-described and separate flow paths, and both treated fluids are mixed (reacted).
- At least the predetermined pressure applied to the first fluid to be processed is separated from both processing surfaces 1 and 2.
- the processing surfaces 1 and 2 are maintained at a predetermined minute interval.
- the fluid to be treated is passed between the treatment surfaces 1 and 2 as a fluid film having a predetermined thickness, and the fluids to be treated are uniformly mixed (reaction) during the passage, thereby causing a reaction involving precipitation.
- a desired reaction product is crystallized or precipitated.
- FIG. 25 is a schematic cross-sectional view of a fluid processing apparatus that processes an object to be processed between processing surfaces in which at least one of the approachable / separable members rotates relative to the other.
- 26A is a schematic plan view of the first processing surface of the apparatus shown in FIG. 25, and FIG. 26B is an enlarged view of a main part of the processing surface of the apparatus shown in FIG.
- FIG. 27A is a cross-sectional view of the second introduction path, and FIG. 27B is an enlarged view of a main part of the processing surface for explaining the second introduction path.
- U indicates the upper side
- S indicates the lower side.
- R indicates the rotation direction.
- C indicates the centrifugal force direction (radial direction).
- This apparatus uses at least two kinds of fluids, of which at least one kind of fluid contains at least one kind of object to be processed, and is disposed so as to be able to approach and separate from each other, and at least One of the above-mentioned fluids joins between the processing surfaces rotating with respect to the other to form a thin film fluid, and is an apparatus for processing the object to be processed in the thin film fluid.
- the “treatment” is not limited to a form in which an object to be treated reacts, but includes a form in which only mixing and dispersion are performed without causing a reaction.
- this apparatus includes a first holder 11 and a second holder 21 disposed above the first holder 11 and a fluid pressure application mechanism P and a contact pressure application mechanism.
- the contact surface pressure applying mechanism includes a spring 43 and an air introduction portion 44.
- the first holder 11 is provided with a first processing part 10 and a rotating shaft 50.
- the first processing unit 10 is an annular body called a maining ring, and includes a first processing surface 1 that is mirror-finished.
- the rotary shaft 50 is fixed to the center of the first holder 11 by a fixing tool 81 such as a bolt, and the rear end thereof is connected to a rotary drive device 82 (rotary drive mechanism) such as an electric motor.
- a driving force is transmitted to the first holder 11 to rotate the first holder 11.
- the first processing unit 10 rotates integrally with the first holder 11.
- the upper part of the first holder 11 is provided with a receiving part capable of receiving the first processing part 10.
- the first processing part to the first holder 11 is fitted into the receiving part.
- Ten of the above attachments have been made.
- the first processing portion 10 is fixed by a rotation preventing pin 83 so as not to rotate with respect to the first holder 11.
- the rotation prevention pin 83 instead of the rotation prevention pin 83, it may be fixed so as not to rotate by a method such as shrink fitting.
- the first processing surface 1 is exposed from the first holder 11 and faces the second holder 21.
- ceramic, sintered metal, anti-abrasion steel, or other metal subjected to hardening treatment, or hard material subjected to lining, coating, plating, or the like is employed.
- the second holder 21 is provided with a second processing portion 20, a first introduction portion d1 into which a fluid is introduced from the inside of the processing portion, a spring 43 as the contact surface pressure applying mechanism, and an air introduction portion 44. It has been.
- the second processing unit 20 is an annular body called a compression ring, and is located on the inner side of the second processing surface 2 that is mirror-finished and adjacent to the second processing surface 2.
- Pressure receiving surface 23 (hereinafter referred to as separation adjusting surface 23).
- the separation adjusting surface 23 is an inclined surface.
- the mirror finishing applied to the second processing surface 2 employs the same method as the first processing surface 1 described above. Further, the same material as that of the first processing unit 10 is also used for the material of the second processing unit 20.
- the separation adjusting surface 23 is adjacent to the inner peripheral surface 25 of the annular second processing portion 20.
- a ring accommodating portion 41 is formed at the bottom (lower portion) of the second holder 21, and the second processing portion 20 is received in the ring accommodating portion 41 together with the O-ring. Further, the second processing unit 20 is received by the rotation stopper 84 so as not to rotate with respect to the second holder 21. The second processing surface 2 is exposed from the second holder 21. In this state, the second processing surface 2 faces the first processing surface 1 of the first processing unit 10.
- the ring holder 41 included in the second holder 21 is a recess that mainly stores a portion of the second ring 20 on the side opposite to the processing surface 2 side, and is a groove formed in an annular shape in plan view.
- the ring accommodating portion 41 is formed larger than the size of the second ring 20 and accommodates the second ring 20 with a sufficient clearance between the ring accommodating portion 41 and the second ring 20.
- the second processing portion 20 is accommodated in the ring accommodating portion 41 so as to be displaced in the axial direction of the accommodating portion 41 and further in the direction intersecting the axial direction. Further, the second processing portion 20 is accommodated such that the center line (axial direction) of the second processing portion 20 can be displaced relative to the ring accommodating portion 41 so as not to be parallel to the axial direction of the ring accommodating portion 41. Yes.
- At least the ring accommodating portion 41 of the second holder 21 is provided with a spring 43 as a processing portion biasing portion. The spring 43 urges the second processing unit 20 toward the first processing unit 10.
- the second processing unit 20 held by the second holder 21 using the pressurizing means for supplying air pressure or other fluid pressure such as the air introduction unit 44 is transferred to the first processing unit 10.
- a method of biasing in the approaching direction may be used.
- the contact surface pressure applying mechanism such as the spring 43 and the air introduction part 44 urges each position in the circumferential direction of the second processing part 20 (each position on the processing surface) equally toward the first processing part 10.
- the first introduction part d1 is provided in the center of the second holder 21, and the fluid that is pumped from the first introduction part d1 to the outer periphery of the processing part is first held by the second holder 21.
- the fluid pressure applying mechanism P is applied to the pressure receiving surface 23 provided in the second processing portion 20 in a direction in which the second processing portion 20 is separated from the first processing portion 10 against the urging force of the urging portion. Receives the fluid pressure (supply pressure).
- supply pressure the fluid pressure
- the introduction effect (micropump effect) of the fluid to be processed between the working surfaces may be used.
- the micropump effect means that the fluid in the recess advances at a speed toward the tip in the outer circumferential direction of the recess 13 by the rotation of the first processing surface 1 and then the fluid fed to the tip of the recess 13 This is an effect of receiving pressure from the inner peripheral direction of the recess 13 and finally becoming pressure in a direction to separate the processing surface, and simultaneously introducing the fluid between the processing surfaces.
- the pressure received by the fluid in the recess 13 provided in the first processing surface 1 finally acts on the second processing surface 2 as a pressure receiving surface that acts on the separation side.
- the pressure receiving surface 23 and the recess 13 can be provided together in one apparatus.
- the concave portion 13 has a depth of 1 ⁇ m to 50 ⁇ m, more preferably 3 ⁇ m to 20 ⁇ m, and is a concave portion provided on the processing surface.
- the total area in the horizontal direction with respect to the processing surface is the processing surface. 5% to 50%, preferably 15% to 25% of the total, the number of which is 3 to 50, preferably 8 to 24, and the shape extends in a curved or spiral shape on the processing surface Or bent into an L-shape.
- the fluid can be stably introduced between the processing surfaces from a high viscosity region to a low viscosity region, and even when the fluid introduced using the micropump effect contains a solid.
- the recess 13 provided in the processing surface may be connected to each other on the introduction side, that is, inside the processing surface, or may be divided.
- the pressure receiving surface 23 is an inclined surface.
- This inclined surface pressure-receiving surface 23
- the downstream end portion 60 of the inclined surface (pressure receiving surface 23) is placed on the axial projection surface of the concave portion 13.
- the angle ⁇ 1 of the inclined surface with respect to the second processing surface 2 is preferably in the range of 0.1 ° to 85 °, more preferably in the range of 10 ° to 55 °, and still more preferably in the range of 15 ° to 45 °. .
- This angle ⁇ 1 can be appropriately changed depending on the properties of the workpiece before processing.
- the downstream end portion 60 of the inclined surface has a downstream end portion 13 from a position that is 0.01 mm downstream from the upstream end portion 13-b of the concave portion 13 provided in the first processing surface 1.
- the position of the downstream end 60 can be appropriately changed according to the properties of the object to be processed.
- the inclined surface pressure receiving surface 23
- the workpieces can be introduced more uniformly.
- the recess 13 can be implemented even if it is intermittent as well as continuous as described above.
- the upstream end of the intermittent recess 13 on the innermost peripheral side of the first processing surface 1 becomes the above-mentioned 13-b, and also the upstream of the first processing surface 1 on the outermost peripheral side.
- the side end becomes 13-c.
- the concave portion 13 is formed on the first processing surface 1 and the pressure receiving surface 23 is formed on the second processing surface 2. Conversely, the concave portion 13 is formed on the second processing surface 2. It is also possible to form the pressure receiving surface 23 on the first processing surface 1.
- the recesses 13 are formed on both the first processing surface 1 and the second processing surface 2, and the recesses 13 and the pressure receiving surfaces 23 are alternately provided in the circumferential direction of the processing surfaces 1 and 2, thereby
- the concave portion 13 formed on the first processing surface 1 and the pressure receiving surface 23 formed on the second processing surface 2 face each other, and at the same time, the pressure receiving surface 23 formed on the first processing surface 1 and the second processing surface 2 It is also possible that the formed recess 13 is opposed.
- a groove different from the recess 13 can be formed on the processing surface. As a specific example, as shown in FIGS. 16 (F) and 16 (G), it extends radially outward (FIG. 16 (F)) or radially inward (FIG. 16 (G)) from the recess 13. A new recess 14 can be applied. This is advantageous when it is desired to extend the residence time between the processing surfaces or when processing a highly viscous fluid.
- the groove can be formed according to the purpose.
- the second processing portion 20 is formed with a second introduction portion d2 having an opening d20 that communicates between the processing surfaces independently of the flow path of the fluid introduced into the processing surface.
- the second introduction part d2 has a predetermined introduction direction from the opening d20 of the second processing surface 2 with respect to the second processing surface 2. Is inclined at an elevation angle ( ⁇ 1).
- the elevation angle ( ⁇ 1) is set to be more than 0 degrees and less than 90 degrees, and in the case of a reaction with a higher reaction rate, it is preferably set at 1 to 45 degrees.
- the introduction direction from the opening d20 of the second processing surface 2 has a directivity in a plane along the second processing surface 2. .
- the introduction direction of the second fluid is a component in the radial direction of the processing surface that is an outward direction away from the center and a component with respect to the rotation direction of the fluid between the rotating processing surfaces. Is forward.
- a line segment in the radial direction passing through the opening d20 and extending outward is defined as a reference line g and has a predetermined angle ( ⁇ 2) from the reference line g to the rotation direction R.
- This angle ( ⁇ 2) is also set to be greater than 0 ° and less than 90 °, and is discharged from the opening d20 toward the shaded portion in FIG.
- the angle ( ⁇ 2) may be small, and when the reaction rate is slow, the angle ( ⁇ 2) is preferably set to be large. This angle can be changed and implemented according to various conditions such as the type of fluid, reaction speed, viscosity, and rotational speed of the processing surface.
- the diameter of the opening d20 is preferably 0.2 ⁇ m to 3000 ⁇ m, more preferably 10 ⁇ m to 1000 ⁇ m.
- the diameter of the second introduction part d2 may be set within the range.
- the opening d20 in the separate flow path is a spiral laminar flow in which the flow direction when introduced by the micropump effect from the concave portion provided in the first processing surface 1 is formed between the processing surfaces. What is necessary is just to install in the outer diameter side rather than the point converted into a flow direction. That is, in FIG. 26B, it is preferable that the distance n from the radially outer side of the processing surface to the radially outer side of the recess 13 provided in the first processing surface 1 is 0.5 mm or more. Further, when a plurality of openings are provided for the same fluid, it is preferable to install them on concentric circles.
- reactions such as C + D ⁇ E are executed in order, and reactions such as A + B + C ⁇ F should not occur at the same time. It is effective in avoiding the problem that the reaction is not carried out without contact. Further, it can be carried out by immersing the processing part in a fluid and mixing (reacting) the processing part between the processing surfaces and directly putting it into a liquid outside the processing part or a gas other than air. . Furthermore, ultrasonic energy can be added to the workpiece between the processing surfaces or immediately after being discharged from the processing surface.
- the temperature control mechanism is not particularly limited, but when cooling is intended, the processing units 10 and 20 are provided with a cooling unit. Specifically, a cooling element capable of electrically or chemically cooling action such as piping for passing ice water or various refrigerants as a temperature control medium or a Peltier element is attached to the processing parts 10 and 20. When the purpose is heating, the processing parts 10 and 20 are provided with heating parts.
- a heating element that can generate heat electrically or chemically, such as steam as a temperature control medium, piping for passing various heating media, or an electric heater is attached to the processing units 10 and 20. .
- the temperature of the processing surface can be controlled using the heat conduction of the processing portion.
- a cooling element or a heating element in the processing parts 10 and 20 and energizing it or by embedding a passage for passing a cooling / heating medium and passing a temperature adjusting medium (cooling / heating medium) through the passage, it is used for processing from the inside.
- the surface can also be temperature controlled.
- the temperature control mechanisms J1 and J2 shown in FIG. 25 are examples thereof, and are pipes (jackets) through which the temperature control medium provided in the processing units 10 and 20 is passed.
- the temperature of one processing surface is higher than that of the other processing surface, and a temperature difference is generated between the processing surfaces.
- the first processing unit 10 is heated to 60 ° C. by any of the above methods
- the second processing unit 20 is set to 15 ° C. by any of the above methods.
- the temperature of the fluid introduced between the processing surfaces changes from 60 ° C. to 15 ° C. from the first processing surface 1 toward the second processing surface 2. That is, a temperature gradient is generated in the fluid between the processing surfaces.
- the fluid between the processing surfaces starts to convect due to the temperature gradient, and a flow in the direction perpendicular to the processing surface is generated.
- the “vertical flow” means that the flow direction component includes at least a component perpendicular to the processing surface.
- the temperature difference between the processing surfaces can be 1 to 400 degrees, preferably 5 to 100 degrees.
- the rotating shaft 50 in this apparatus is not limited to what is arrange
- position diagonally This is because the influence of gravity can be substantially eliminated by the fluid thin film formed between the processing surfaces 1 and 2 during processing.
- the first introduction part d1 coincides with the axial center of the second ring 20 in the second holder 21, and extends vertically.
- the first introduction part d1 is not limited to the one that coincides with the axis of the second ring 20, and the first fluid to be treated is supplied to the space surrounded by the rings 10 and 20.
- the central portion 22 of the second holder 21 may be provided at a position other than the axis, and may extend obliquely instead of vertically. In any of the arrangement angles, a flow perpendicular to the processing surface can be generated by the temperature gradient between the processing surfaces.
- the critical Rayleigh number at which Benard convection begins to occur is about 1700, although it depends on the nature of the interface between the processing surface and the workpiece fluid. Larger values cause Benard convection.
- the Rayleigh number Ra is a value larger than around 10 10 , the fluid becomes a turbulent state. In other words, the temperature difference ⁇ T between the processing surfaces or the distance L between the processing surfaces is adjusted so that the Rayleigh number Ra is 1700 or more, so that the processing surface is adjusted between the processing surfaces.
- a vertical flow can be generated, and the above mixing (reaction) operation can be performed.
- Benard convection hardly occurs at a distance between processing surfaces of about 1 to 10 ⁇ m. Strictly speaking, when the Rayleigh number is applied to a fluid in an interval of 10 ⁇ m or less and the Benard convection generation conditions are examined, the temperature difference in the case of water needs to be several thousand degrees Celsius or more. difficult. Benard convection is convection due to density difference in the temperature gradient of the fluid, that is, convection related to gravity. There is a high possibility of a microgravity field between the processing surfaces of 10 ⁇ m or less, and buoyancy convection is suppressed in such a place. That is, Benard convection actually occurs in this apparatus when the distance between the processing surfaces exceeds 10 ⁇ m.
- the critical Marangoni number at which Marangoni convection begins to occur is around 80, and Marangoni convection occurs under conditions that are larger than that value.
- the temperature difference ⁇ T between the processing surfaces or the distance L between the processing surfaces is adjusted so that the Marangoni number Ma is 80 or more, so that even if the flow path is 10 ⁇ m or less.
- a flow in a direction perpendicular to the processing surface can be generated between the surfaces, and the above mixing (reaction) operation can be performed.
- the method for maintaining the gap between the processing surfaces of the fluid processing apparatus is not limited to the method using pressure balance.
- the distance between the processing surfaces may be set mechanically, or the distance between the processing surfaces may be maintained using principles such as magnetic repulsion, magnetic levitation, and electromagnetic repulsion.
- the material of the processing surfaces 1 and 2 that are arranged so as to be able to approach and separate from each other and at least one rotates with respect to the other is not particularly limited, but ceramic, sintered metal, wear-resistant steel, and other metals Alternatively, it can be made of a metal that has been hardened or a hard material that has been constructed by lining, coating, plating, or the like.
- the distance between the processing surfaces 1 and 2 that are arranged so as to be able to approach and separate from each other and at least one of which rotates with respect to the other is 0.1 ⁇ m to 100 ⁇ m, particularly 1 to 10 ⁇ m. Is preferred.
- reactions such as precipitation / precipitation or crystallization are arranged opposite to each other so as to be able to approach and separate, and at least one of the processing surfaces 1 and 2 rotates with respect to the other. Occurs with forcible uniform mixing.
- Control of the particle size and monodispersity of the copper phthalocyanine fine particles can be adjusted by appropriately adjusting the rotational speed and flow rate of the processing units 10 and 20, the distance between the processing surfaces, the raw material concentration, the dispersion medium, and the like. it can.
- a fluid containing a solvent that can be a poor solvent for the copper phthalocyanine solution is disposed as a first fluid from the first introduction part d1 that is one channel so as to be able to approach and separate from each other. Is introduced between the processing surfaces 1 and 2 rotating with respect to the other to form a thin film fluid composed of the first fluid between the processing surfaces.
- a fluid containing a copper phthalocyanine solution in which copper phthalocyanine, which is a reactant, is dissolved is directly introduced as a second fluid into the thin film fluid composed of the first fluid from the second introduction part d2 that is another flow path.
- the first fluid and the second fluid are thin films between the processing surfaces 1 and 2 whose distance is fixed by the pressure balance between the fluid supply pressure and the pressure applied between the rotating processing surfaces. While maintaining the state, it is possible to carry out a reaction that is instantaneously mixed to produce copper phthalocyanine fine particles.
- the second fluid is introduced from the first introduction part d 1 and the first fluid is introduced from the second introduction part d 2. May be introduced.
- the expressions “first” and “second” in each solvent only have a meaning for identification that they are the n-th of a plurality of solvents, and third or more solvents may exist.
- the combination of the first fluid and the second fluid is not particularly limited, and any fluid that contains a copper phthalocyanine solution and a solvent that has a lower solubility in copper phthalocyanine than the copper phthalocyanine solution and can be a poor solvent can be used.
- the solvent for dissolving copper phthalocyanine is not particularly limited.
- sulfuric acid, hydrochloric acid, nitric acid, trifluoroacetic acid, phosphoric acid and the like can be used.
- a strong acid, particularly 95% or more of concentrated sulfuric acid can be used.
- fuming sulfuric acid or fuming nitric acid can be used.
- fuming sulfuric acid or fuming nitric acid is preferably used.
- Examples of the alkali added to the organic solvent include sodium hydroxide, potassium hydroxide, sodium methoxide, sodium ethoxide and the like.
- Examples of the acid include sulfuric acid, hydrochloric acid, nitric acid, trifluoroacetic acid, phosphoric acid and the like as described above.
- the solvent that can be a poor solvent for precipitating copper phthalocyanine is not particularly limited. It can carry out using the solvent whose solubility with respect to copper phthalocyanine is lower than the solvent which melt
- water, alcohol solvent, ketone solvent, ether solvent, aromatic solvent, carbon disulfide, aliphatic solvent, nitrile solvent, sulfoxide solvent, halogen solvent, ester solvent, ionic solution Or it is preferable to select from these 2 or more types of mixed solvents.
- the first fluid and the second fluid are disposed between the processing surfaces 1 and 2 whose distance is controlled by the pressure balance between the fluid supply pressure and the pressure applied between the rotating processing surfaces 1 and 2.
- first fluid or the second fluid may contain a dispersing agent such as a block copolymer, a polymer, or a surfactant.
- a dispersing agent such as a block copolymer, a polymer, or a surfactant.
- surfactant and dispersant various commercially available products used for pigment dispersion can be used. Although not particularly limited, for example, sodium dodecyl sulfonate or dodecylbenzenesulfonic acid type such as Neogen RK (Daiichi Kogyo Seiyaku), Solsperse 20000, Solsperse 24000, Solsperse 26000, Solsperse 27000, Solsperse 28000, Solsperse 41090 ( Dispersic 160 ⁇ , Dispersic 161, Dispersic 162, Dispersic 163, Dispersic 166, Dispersic 170, Dispersic 180, Dispersic 181, Dispersic 182, Dispersic 183, Dispersic 184 , Disperbic 190, Disperbic 191 ⁇ , Disperbic 192, Disperbic 2000, Dispersic 2001 (above, manufactured by BYK Chemie), Polymer 1 00, Polymer 120, Polymer 150, Polymer 400, Polymer 401, Polymer 402, Poly
- mixing in the mixing channel can be performed under laminar flow control or turbulent flow control.
- the thin film fluid can be heated and cooled ( FIG. 25).
- the processing fluid is heated and the reaction is accelerated by providing a microwave generator such as a magnetron for irradiating at least one or both of the processing units 10 and 20 with microwaves.
- a microwave generator such as a magnetron for irradiating at least one or both of the processing units 10 and 20 with microwaves.
- an element such as a lamp that irradiates ultraviolet rays is provided on at least one or both of the processing units 10 and 20, and ultraviolet rays (UV) are applied to the thin film fluid from the corresponding processing surfaces.
- At least one or both of the processing units 10 and 20 can be provided with an ultrasonic oscillator, and mixing and reaction between the processing surfaces can be performed in an ultrasonic atmosphere. It can also be carried out in a container.
- the deposition is performed in a container capable of securing a reduced pressure or a vacuum state, and at least the secondary side from which the fluid is discharged after the treatment is set to a reduced pressure or a vacuum state, whereby the gas generated during the precipitation reaction and the fluid are contained in the fluid.
- the contained gas can be degassed or the fluid can be desolvated.
- the third introduction part d3 can be provided in the processing apparatus.
- an aqueous solvent is used from each of the introduction parts.
- the fourth or more introduction portions are provided, and the fluid to be introduced into the processing apparatus can be subdivided in this way.
- the surface treatment by introducing a modifying group on at least the surface of the copper phthalocyanine fine particles can be performed by including a surface modifier in the fluid introduced between the treatment surfaces 1 and 2.
- the surface modifier may be contained in either the pigment solution (first fluid) or the poor solvent (second fluid), or both, or in a third fluid different from the pigment solution and the poor solvent. It may be included. Further, the combination of the first fluid and the second fluid is not particularly limited to the above.
- the type of the modifying group introduced at least on the pigment surface as the surface modifying group is not particular limitation.
- a solvent for dispersion or a dispersion What is necessary is just to use properly according to a kind.
- polar groups such as acidic groups and basic groups, salt structures of the polar groups, highly polar atoms such as oxygen and sulfur, and / or structures with large polarizability introduced with aromatic rings, hydrogen bonding groups, hetero groups
- polar groups such as acidic groups and basic groups, salt structures of the polar groups, highly polar atoms such as oxygen and sulfur, and / or structures with large polarizability introduced with aromatic rings, hydrogen bonding groups, hetero groups
- polar groups such as acidic groups and basic groups, salt structures of the polar groups, highly polar atoms such as oxygen and sulfur, and / or structures with large polarizability introduced with aromatic rings, hydrogen bonding groups, hetero groups
- polar groups such as acidic groups and basic groups, salt structures of the polar groups, highly polar
- Examples of the acidic group include a hydroxyl group (hydroxy group), a sulfonic acid group (sulfo group), a carboxylic acid group, a phosphoric acid group, and a boric acid group.
- An amino group etc. are mentioned as a basic group.
- Examples of the hydrogen bonding group include a urethane moiety, a thiourethane moiety, a urea moiety, and a thiourea moiety.
- the purpose of the surface treatment is other than the improvement of dispersibility
- the surface of the copper phthalocyanine fine particles is made water repellent, lipophilic, or oleophilic, it is oleophilic to the first fluid or the second fluid.
- a lipophilic functional group can be introduced as a modifying group on the surface of the copper phthalocyanine fine particles discharged from between the processing surfaces 1 and 2 to perform lipophilic treatment.
- the above surface treatment is not limited to the case where the surface modification of the copper phthalocyanine fine particles is performed between the processing surfaces 1 and 2 as described above, and is performed even after the copper phthalocyanine fine particles are discharged from between the processing surfaces 1 and 2 it can.
- the substance used for the surface treatment of the copper phthalocyanine fine particles is added to the discharged liquid, stirred, etc.
- the surface treatment of the copper phthalocyanine fine particles can be performed.
- impurities can be removed from the fluid containing the copper phthalocyanine fine particles by a dialysis tube or the like, and then a substance for surface treatment can be added. Further, the surface treatment can be performed after drying the liquid component of the fluid containing the copper phthalocyanine fine particles discharged from between the processing surfaces 1 and 2 to obtain a copper phthalocyanine fine particle powder. Specifically, the obtained copper phthalocyanine fine particle powder is dispersed in a target solvent, and the above-described surface treatment target substance is added and subjected to a treatment such as stirring.
- the copper phthalocyanine pigment fine particle production method (forced ultrathin film rotary reaction method) can freely change the Reynolds number of the microchannel, so that the particle diameter, particle shape, crystal type, etc.
- fine particles of copper phthalocyanine that are monodispersed and have good redispersibility can be produced.
- due to its self-discharging properties there is no clogging of the product even in the case of a reaction involving precipitation, and a large pressure is not required. Therefore, copper phthalocyanine fine particles can be stably produced, and the safety is excellent, the impurities are hardly mixed, and the cleaning property is good.
- it can be scaled up according to the target production volume, it is possible to provide a method for producing copper phthalocyanine pigment fine particles with high productivity.
- the copper phthalocyanine pigment according to the present invention is blue, and is suitable as a color filter for use in a liquid crystal color display, but is not limited thereto, and is not limited thereto. Paint, dye, inkjet ink, thermal transfer ink, toner It can be used for various applications such as colored resins.
- Copper phthalocyanine having a wavelength ( ⁇ max) at which the spectral transmittance is maximum is less than 478 nm, and the transmittance of the same transmission spectrum at a wavelength of 400 to 450 nm is larger than the ⁇ -type copper phthalocyanine over the entire wavelength of 400 to 450 nm.
- the manufactured Example is shown.
- the present invention is not limited to the following examples.
- Example 1 As shown in FIG. 1 (A), they are arranged so as to be able to approach and separate from each other, and at least one of them is formed between processing surfaces 1 and 2 that rotate with respect to the other. Then, copper phthalocyanine is dissolved, and a copper phthalocyanine solution is combined with an aqueous solvent in a thin film fluid, and uniformly mixed in the thin film fluid to precipitate copper phthalocyanine.
- “from the center” means “from the first introduction part d1” of the processing apparatus shown in FIG. 1A, and the first fluid is the above-mentioned first fluid. 1 refers to the fluid to be treated, and the second fluid refers to the above-described second fluid to be treated that is introduced from the second introduction portion d2 of the treatment apparatus illustrated in FIG.
- “part” here means “part by weight”.
- the particle size distribution was measured using a Nanotrac particle size distribution analyzer UPA-EX150 (manufactured by Nikkiso Co., Ltd.), and the volume average particle size was adopted.
- the transmission spectrum was measured from 380 nm to 780 nm using an ultraviolet-visible spectrophotometer (UV-2450) manufactured by Shimadzu Corporation.
- UV-2450 ultraviolet-visible spectrophotometer
- the characteristic that the transmittance of the transmission spectrum of copper phthalocyanine at a wavelength of 400 to 450 nm is larger than that of the conventionally used ⁇ -type copper phthalocyanine over the entire wavelength of 400 to 450 nm is 380 to Confirmed as an evaluation criterion that the ratio (T425 / Tmax) ⁇ 0.70 of the transmittance (T425) at the wavelength 425 nm to the transmittance (Tmax) at the wavelength ( ⁇ max) at which the transmittance of the transmission spectrum at 780 nm is maximum did.
- an aqueous solvent at 25 ° C 1% sodium dodecyl sulfate aqueous solution
- the crystal form is ⁇ -form (crystal form) Is confirmed by powder X-ray diffraction
- a concentrated sulfuric acid solution of copper phthalocyanine in which 98% concentrated sulfuric acid is dissolved in 98% concentrated sulfuric acid is introduced between the processing surfaces 1 and 2 at 10 ml / min, and the discharge flow rate becomes 150 g / min.
- a copper phthalocyanine particle dispersion having a substantially spherical shape and a volume average particle diameter of 14.2 nm was obtained.
- a TEM photograph of the obtained copper phthalocyanine fine particles is shown in FIG.
- the obtained copper phthalocyanine fine particle dispersion was dialyzed with pure water for 24 hours using a dialysis tube to remove sulfuric acid and the like, and the result of measuring the transmission spectrum is shown in FIG.
- FIG. 30 shows a powder X-ray diffraction pattern of the copper phthalocyanine powder obtained by drying the copper phthalocyanine dispersion.
- Example 2 to 5 Example 2 to 5 were carried out by changing the amount of copper phthalocyanine introduced between the processing surfaces, the rotational speed of the processing surface, or the discharge flow rate. The results are shown in Table 1 below.
- copper phthalocyanine whose crystal type is ⁇ -type, and as shown in FIG. 31 and Table 1, the wavelength ( ⁇ max) at which the transmittance of the transmission spectrum at 380 to 780 nm is maximum is less than 478 nm.
- a copper phthalocyanine having a transmission spectrum having a transmission spectrum having a transmittance of 400 to 450 nm and a transmittance greater than the ⁇ -type copper phthalocyanine over the entire wavelength of 400 to 450 nm could be produced. .
- the acid pasting method in which copper phthalocyanine is dissolved in concentrated sulfuric acid and diluted with pure water to precipitate copper phthalocyanine fine particles, is a common purification method for crude pigments and is also known as a method for producing ⁇ -type copper phthalocyanine. It has been.
- the acid pasting method is performed by an apparatus (Forced thin film reactor, manufactured by M Technique Co., Ltd. ULREA (hereinafter abbreviated as “FTFR”).
- FTFR Form thin film reactor, manufactured by M Technique Co., Ltd. ULREA
- the shape confirmation and particle diameter measurement of the produced copper phthalocyanine fine particles were confirmed by an electron microscope (transmission type and scanning type) and a particle size distribution meter.
- ⁇ -type copper phthalocyanine (trade name: PV FAST BLUE BG, manufactured by Clariant Japan Co., Ltd.) was used.
- Concentrated sulfuric acid for dissolving copper phthalocyanine was 98% concentrated sulfuric acid (special grade reagent) manufactured by Kishida Chemical Co., Ltd.
- As the surfactant for dispersing the fine particles sodium dodecyl sulfate (first grade reagent, hereinafter abbreviated as “SDS”) manufactured by Kanto Chemical Co., Inc. was used.
- SDS sodium dodecyl sulfate
- the aqueous sodium hydroxide solution used for pH adjustment was prepared by dissolving sodium hydroxide (special grade reagent) manufactured by Kanto Chemical Co., Ltd. in pure water.
- a copper phthalocyanine concentrated sulfuric acid solution in which copper phthalocyanine was dissolved in concentrated sulfuric acid was prepared.
- FTFR processing section started to rotate (rotation speed 1700rpm), while pure water was fed from the center as the first fluid at a feed temperature of 20 ° C and a feed flow rate of 400ml / min., While copper phthalocyanine as the second fluid
- the concentrated sulfuric acid solution was directly introduced between the processing surfaces 1 and 2 at a flow rate of 3 ml / min.
- the copper phthalocyanine concentrated sulfuric acid solution was diluted with pure water between the processing surfaces 1 and 2 to precipitate copper phthalocyanine fine particles, and discharged from between the processing surfaces 1 and 2 as a dilute sulfuric acid aqueous dispersion of copper phthalocyanine fine particles.
- the pH of the discharged copper phthalocyanine fine particle diluted sulfuric acid aqueous solution was 0.81.
- This dilute sulfuric acid aqueous dispersion was adjusted to pH 7.01 using a 3 mol / L aqueous sodium hydroxide solution and allowed to stand in a constant temperature room at 25 ° C. for 22 hours.
- Comparative Example 2 copper phthalocyanine fine particles were prepared by a batch method.
- the batch method used in this comparative example is a method in which copper phthalocyanine concentrated sulfuric acid solution is dropped to precipitate copper phthalocyanine fine particles while stirring pure water using a beaker and a magnetic stirrer.
- the copper phthalocyanine fine particles were washed and dried under the same conditions as in the experiment using the FTFR.
- a dynamic light scattering type particle size distribution measuring device Microtrac UPA-150 manufactured by Nikkiso Co., Ltd. was used.
- the measurement conditions of the particle size distribution are a particle refractive index of 1.51, a particle specific gravity of 1.0 g / cm 3 , a measurement solvent of pure water, and a measurement time of 3 min.
- An ultraviolet-visible spectrophotometer UV-2450 manufactured by Shimadzu Corporation was used for spectrum measurement of the dispersion.
- the measurement conditions for the spectrum are a quartz cell, a sampling rate of 0.2 nm, and a low measurement speed.
- a transmission electron microscope HF-2000 (TEM, manufactured by Hitachi, Ltd.) and a scanning electron microscope S-4800 (SEM, manufactured by Hitachi High-Technologies Corporation) were used.
- a powder X-ray diffractometer X'Pert PRO MPD (Spectris Co., Ltd. PANalytical Division) was used to identify the crystal form of the powder.
- the measurement conditions are a Cu counter cathode, a tube voltage of 45 kV, a tube current of 40 mA, and a scanning speed of 1.6 ° / min.
- TG / DTA simultaneous differential thermogravimetric measurement
- TG / DTA6300 manufactured by Seiko Instruments Inc.
- the measurement conditions are an alumina powder as a reference and a heating rate of 20 ° C./min.
- the infrared absorption spectrum (FT-IR) was measured using FT / IR-4100 type A (manufactured by JASCO Corporation).
- the measurement conditions are ATR method, resolution 4.0 cm ⁇ 1 , number of integrations, 16 times. All the evaluations of the results by the above measurements were performed using the average value of the measurement results obtained three times for the same object. The evaluation and discussion of the results are described below.
- FIG. 33 shows the FTFR
- FIG. 33B shows the batch method
- FIG. 35 shows a transmission electron microscope (TEM) photograph of copper phthalocyanine fine particles prepared by FTFR. It was found that the particles produced by the batch method are rod-like particles having a wide particle size distribution, whereas the fine particles produced using FTFR are spherical particles having a particle diameter of about 10 nm.
- FIG. 36 shows the results of X-ray diffraction measurement of copper phthalocyanine fine particles.
- the X-ray diffraction pattern of the copper phthalocyanine fine particles produced by FTFR has a diffraction peak at the same position as the copper phthalocyanine particles produced by the batch method. From this, it was found that the copper phthalocyanine fine particles prepared by FTFR were ⁇ -type crystal type. Moreover, the diffraction peak of the copper phthalocyanine fine particle produced by FTFR was broader than the diffraction peak of the copper phthalocyanine particle produced by the batch method. This is considered to be due to the fact that the half width of the peak is widened as the particle diameter is reduced.
- FIG. 37 shows an infrared absorption spectrum in the fingerprint region of the copper phthalocyanine fine particles ((A) in FIG. 37 is that of the copper phthalocyanine fine particles produced by FTFR, and (B) is the copper phthalocyanine particles produced by the batch method. ).
- (A) in FIG. 37 is that of the copper phthalocyanine fine particles produced by FTFR
- (B) is the copper phthalocyanine particles produced by the batch method. ).
- peak together due to vibration of the phthalocyanine skeleton approximately 1117-1118, 1089, 1066, 941-943, 863-864, 717 cm - 1 .
- the other peaks are consistent with previous reports (BN Achar, KS Lokesh: J. Solid State Chem., 117, 1987 (2004)), and it was found that there was no change in the molecular structure of copper phthalocyanine.
- the transmission spectrum of a 0.0050% aqueous dispersion of copper phthalocyanine particles in the wavelength region 350-800 nm is shown in FIG.
- the dispersion of copper phthalocyanine fine particles produced by FTFR is 360-550 nm
- the wavelength of the maximum transmittance of the transmission spectrum in the wavelength region shifted to the short wavelength side, and the area ratio was improved by 20-30% compared to the transmittance of the same ⁇ -type copper phthalocyanine.
- the wavelength ( ⁇ max) at which the transmittance of the transmission spectrum at 380 to 780 nm is the maximum is 465.degree. C. as shown in FIG. Since it is 8 nm, it is less than 478 nm, and as shown in FIG. 39, it is possible to produce copper phthalocyanine whose transmission spectrum transmittance at wavelengths of 400 to 450 nm is larger than ⁇ -type copper phthalocyanine over the entire wavelength of 400 to 450 nm. I understand that.
- FIG. 40 shows an absorption spectrum of a 0.0010% aqueous dispersion of copper phthalocyanine fine particles in the wavelength region of 300 to 800 nm. Peaks are observed around 330, 600, and 690 nm, respectively. The spectrum was ⁇ -shaped, but each peak was sharp and shifted to the short wavelength side. The peaks near 690 nm and 600 nm are attributed to the absorption of the monomer and dimer, respectively (JH Sharp, M. Abkowitz: J. Phys. Chem., 77, 477 (1972) H. Xia, M. Nogami: Opt. Mater., 15, 93 (2000)).
- the absorption maximum wavelength ( ⁇ [nm]) of phthalocyanine is calculated by the following equation.
- ⁇ (8mc / h) ( L 2 / [N + 1])
- m the electron mass
- c the speed of light
- h the Planck constant
- L the polymethine bond distance
- N the number of electrons.
- the two items in the equation are the reciprocal of the electron density, and the maximum wavelength shifts to the short wavelength side as the electron density increases.
- the shift of the absorption maximum to the short wavelength side in the copper phthalocyanine fine particle dispersion prepared by FTFR is thought to be due to the fact that the electron density on the particle surface increased due to the decrease in the particle diameter of the copper phthalocyanine fine particles.
- the absorption at 690 nm was shifted to the short wavelength side, it was considered that the absorption in the region of 550 to 700 nm was large and sharp peaks due to the transmission of red.
- Example 7 to 10 Next, another embodiment different from the above will be described.
- the experimental apparatus used in Examples 7 to 10 is the same as in Example 6 above.
- Example 6 As the raw material copper phthalocyanine, the same ⁇ -type copper phthalocyanine as in Example 6 (trade name: PV FAST BLUE BG, manufactured by Clariant Japan Co., Ltd.) was used. Concentrated sulfuric acid and fuming sulfuric acid for dissolving copper phthalocyanine are 98% concentrated sulfuric acid (special grade reagent, manufactured by Kishida Chemical Co., Ltd.) and fuming sulfuric acid (special grade reagent, 30% SO 3 concentration, manufactured by Yotsuhata Chemical Co., Ltd.) Was used. SO 3 concentration of 5% fuming sulfuric acid was prepared by mixing 98% concentrated sulfuric acid and SO 3 concentration of 30% fuming sulfuric acid under a nitrogen atmosphere.
- concentrated sulfuric acid and fuming sulfuric acid for dissolving copper phthalocyanine are 98% concentrated sulfuric acid (special grade reagent, manufactured by Kishida Chemical Co., Ltd.) and fuming sulfuric acid (special grade reagent, 30% SO 3 concentration, manufactured by Yotsuhata
- a surfactant for preparing an aqueous dispersion of copper phthalocyanine fine particles sodium dodecyl sulfate (reagent grade 1, manufactured by Kanto Chemical Co., Inc., hereinafter abbreviated as “SDS” as in Example 6) was used.
- organic solvents for preparing an organic solvent dispersion of copper phthalocyanine fine particles include propylene glycol monomethyl ether acetate (special grade reagent, manufactured by Kanto Chemical Co., Inc., hereinafter abbreviated as “PGMEA”) and propylene glycol monomethyl ether (special grade reagent). Manufactured by Kanto Chemical Co., Inc., hereinafter abbreviated as “PGME”).
- Disperbyk-2000 modified acrylic copolymer, amine value 4 mg KOH / g, active ingredient 40%, manufactured by Big Chemie Japan Co., Ltd.
- the aqueous sodium hydroxide solution used for pH adjustment was prepared by dissolving sodium hydroxide (special grade reagent, manufactured by Kanto Chemical Co., Inc.) in pure water.
- Example 7 is expressed as “Ex.1”
- Example 8 is expressed as “Ex.2”
- Example 9 is expressed as “Ex.3”.
- Example 10 is described as “Ex.4”.
- Copper phthalocyanine was dissolved in concentrated sulfuric acid (Examples 7 to 9) or fuming sulfuric acid having a SO 3 concentration of 5% (Example 10) to prepare a copper phthalocyanine solution.
- Rotation of the processing part is started while supplying pure water as the first fluid (“Fluid [A]” in Table 3) between the processing surfaces 1 and 2 of the FTFR from the center at a liquid supply temperature of 20 ° C.
- a copper phthalocyanine solution was introduced between the processing surfaces 1 and 2 as the second fluid (“Fluid [B]” in Table 3).
- the discharged copper phthalocyanine fine particle aqueous dispersion was allowed to stand in a thermostatic chamber at 25 ° C. for 22 hours (Example 9 (Ex. 3), Example 10 (Ex. 4)).
- Example 7 (Ex.1) and Example 8 (Ex.2) the discharged copper phthalocyanine fine particle aqueous dispersion (pH 1.58, Example 9 (Ex.3)) was added to 3 mol / L water. It adjusted to pH 7.01 (Example 8 (Ex.2)) and pH 12.55 (Example 7 (Ex.1)) using sodium oxide aqueous solution, and left still at 25 degreeC thermostat for 22 hours.
- a mixed solution of PGMEA and PGME and an active ingredient concentration of 2 wt% Disperbyk-2000 solution were added to the copper phthalocyanine fine particle dry powder to prepare a copper phthalocyanine fine particle organic solvent dispersion. (Prescription conditions: copper phthalocyanine fine particle solid concentration 2 wt%, Disperbyk-2000 active ingredient concentration 1 wt%).
- IR Infrared absorption spectrum
- FIG. 41 shows an infrared absorption spectrum in the fingerprint region of the copper phthalocyanine fine particles.
- peaks caused by vibrations of the phthalocyanine skeleton about 1117-1118, 1089-1090, 1065-1066, 943, 864-865, 717-719 cm -1 ) was confirmed.
- a shoulder peak peak marked with * in the figure was confirmed in the vicinity of 1388 cm ⁇ 1 and copper phthalocyanine fine particles prepared using fuming sulfuric acid as the second fluid. It was confirmed that a sulfo group was present and surface treatment was performed.
- FIG. 42 shows the transmission spectrum of 0.005 wt% -copper phthalocyanine particle dispersion in the wavelength region of 350-800 nm for the aqueous dispersion of Example 7 (Ex.1) and the organic solvent dispersion of Example 10 (Ex.4). Indicates.
- the black line shows the transmission spectrum of Example 7, and the gray line shows the transmission spectrum of Example 10. Also in Example 7 and Example 10, it turns out that the transmission spectrum similar to the said Example 6 (refer FIG. 39) is shown.
- Example 7 and Example 10 The spectral shapes of Example 7 and Example 10 are almost the same, and it is considered that the functional groups present on the surface of the copper phthalocyanine fine particles have little influence on the spectral characteristics. It was also found that the copper phthalocyanine fine particles showed the same transmission spectrum both in the aqueous solution system and in the organic solvent system.
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Abstract
Description
両処理用面1、2は、被処理流動体の流路に接続され、被処理流動体の流路の一部を構成する。
より詳しくは、この装置は、少なくとも2つの被処理流動体の流路を構成すると共に、各流路を、合流させる。
即ち、この装置は、第1の被処理流動体の流路に接続され、当該第1被処理流動体の流路の一部を形成すると共に、第1被処理流動体とは別の、第2被処理流動体の流路の一部を形成する。そして、この装置は、両流路を合流させて、処理用面1、2間において、両流動体を混合し、反応を伴う場合においては反応させる。図1(A)へ示す実施の形態において、上記の各流路は、密閉されたものであり、液密(被処理流動体が液体の場合)・気密(被処理流動体が気体の場合)とされている。
尚、回転駆動部は図示を省略する。
第1処理用部10と第2処理用部20とは、少なくとも何れか一方が、少なくとも何れか他方に、接近・離反可能となっており、両処理用面1、2は、接近・離反できる。
この実施の形態では、第1処理用部10に対して、第2処理用部20が接近・離反する。但し、これとは逆に、第1処理用部10が、第2処理用部20に対して接近・離反するものであってもよく、両処理用部10、20が互いに接近・離反するものであってもよい。
図1(A)へ示す通り、この実施の形態において、第1処理用部10及び第2処理用部20は、夫々環状体、即ちリングである。以下、必要に応じて第1処理用部10を第1リング10と呼び、第2処理用部20を第2リング20と呼ぶ。
この実施の形態において、両リング10、20は、金属製の一端が鏡面研磨された部材であり、当該鏡面を第1処理用面1及び第2処理用面2とする。即ち、第1リング10の上端面が第1処理用面1として、鏡面研磨されており、第2リング20の下端面が第2処理用面2として、鏡面研磨されている。
この実施の形態において、第1ホルダ11は、回転軸50にて、回転駆動部から駆動力を受けて、第2ホルダ21に対して回転するものであり、これにて、第1ホルダ11と一体となっている第1リング10が第2リング20に対して回転する。第1リング10の内側において、回転軸50は、平面視、円形の第1リング10の中心と同心となるように、第1ホルダ11に設けられている。
第1リング10の回転は、第1リング10の軸心を中心とする。図示はしないが、軸心は、第1リング10の中心線を指し、仮想線である。
具体的には、第1及び第2ホルダ11、21は、夫々は、凹状のリング収容部を備える。この実施の形態において、第1ホルダ11のリング収容部に、第1リング10が嵌合し、第1ホルダ11のリング収容部から出没しないように、第1リング10はリング収容部に固定されている。
第1リング10の材質は、金属の他、セラミックや焼結金属、耐磨耗鋼、その他金属に硬化処理を施したものや、硬質材をライニングやコーティング、メッキなどを施工したものを採用する。特に、回転するため、軽量な素材にて第1処理用部10を形成するのが望ましい。第2リング20の材質についても、第1リング10と同様のものを採用して実施すればよい。
この第2ホルダ21が備えるリング収容部41は、第2リング20の、主として処理用面2側と反対側の部位を収容する凹部であり、平面視において、円を呈する、即ち環状に形成された、溝である。
リング収容部41は、第2リング20の寸法より大きく形成され、第2リング20との間に十分なクリアランスを持って、第2リング20を収容する。
このクリアランスにより、当該第2リング20は、このリング収容部41内にて、環状のリング収容部41の軸方向について、更に、当該軸方向と交差する方向について、変位することができる。言い換えれば、このクリアランスにより、当該第2リング20は、リング収容部41に対して、第2リング20の中心線を、上記リング収容部41の軸方向と平行の関係を崩すようにも変位できる。
以下、第2ホルダ21の、第2リング20に囲まれた部位を、中央部分22と呼ぶ。
上記について、換言すると、当該第2リング20は、このリング収容部41内にて、リング収容部41のスラスト方向即ち上記出没する方向について、更に、リング収容部41の中心に対して偏心する方向について、変位することが可能に収容されている。また、リング収容部41に対して、第2リング20の周方向の各位置にて、リング収容部41からの出没の幅が夫々異なるようにも変位可能に即ち芯振れ可能に、当該第2リング20は収容されている。
接面圧付与機構4は、第2リング20の周方向の各位置即ち第2処理用面2の各位置を均等に、第1リング10へ向けて付勢する。接面圧付与機構4の具体的な構成については、後に詳述する。
図1(A)へ示す通り、上記のケース3は、両リング10、20外周面の外側に配置されたものであり、処理用面1、2間にて生成され、両リング10、20の外側に排出される生成物を収容する。ケース3は、図1(A)へ示すように、第1ホルダ11と第2ホルダ21を、収容する液密な容器である。但し、第2ホルダ21は、当該ケース3の一部としてケース3と一体に形成されたものとして実施することができる。
上記の通り、ケース3の一部とされる場合は勿論、ケース3と別体に形成される場合も、第2ホルダ21は、両リング10、20間の間隔、即ち、両処理用面1、2間の間隔に影響を与えるようには可動となっていない。言い換えると、第2ホルダ21は、両処理用面1、2間の間隔に影響を与えない。
ケース3には、ケース3の外側に生成物を排出するための排出口32が設けられている。
上記の流体圧付与機構p1は、直接或いは間接的に、この第1導入部d1に接続されて、第1被処理流動体に、流体圧を付与する。流体圧付与機構p1には、コンプレッサやその他のポンプを採用することができる。
この実施の形態において、第1導入部d1は、第2ホルダ21の上記中央部分22の内部に設けられた流体の通路であり、その一端が、第2ホルダ21の、第2リング20が平面視において呈する円の中心位置にて、開口する。また、第1導入部d1の他の一端は、第2ホルダ21の外部即ちケース3の外部において、上記流体圧付与機構p1と接続されている。
第2流体供給部p2には、コンプレッサ、その他のポンプを採用することができる。
このとき、第1被処理流動体の送圧を受けた、第2リング20は、接面圧付与機構4の付勢に抗して、第1リング10から遠ざかり、両処理用面間に微小な間隔を開ける。両処理用面1、2の接近・離反による、両面1、2間の間隔について、後に詳述する。
両処理用面1、2間において、第2導入部d2から第2の被処理流動体が供給され、第1の被処理流動体と合流し、処理用面の回転により、混合(反応)が促進される。そして、両流動体の混合(反応)による生成物が両処理用面1、2から、両リング10、20の外側に排出される。両リング10、20の外側に排出された生成物は、最終的に、ケース3の排出口32からケース3の外部に排出される(自己排出)。
上記の被処理流動体の混合及び反応(反応を伴う場合)は、第2処理用部20に対する第1処理用部10の駆動部5による回転にて、第1処理用面1と第2処理用面2とによって行われる。
第1及び第2の処理用面1、2間において、第2導入部d2の開口部m2の下流側が、上記の第1の被処理流動体と第2の被処理流動体とを混合させる処理室となる。具体的には、両処理用面1、2間において、第2リング20の底面を示す図11(C)にて、斜線で示す、第2リング20の径の内外方向r1について、第2導入部の開口部m2即ち第2開口部m2の外側の領域Hが、上記の処理室として機能する。従って、この処理室は、両処理用面1、2間において、第1導入部d1と第2導入部d2の両開口部m1、m2の下流側に位置する。
第1開口部m1からリングの内側の空間を経て両処理用面1、2間へ導入された第1の被処理流動体に対して、第2開口部m2から、両処理用面1、2間に導入された第2の被処理流動体が、上記処理室となる領域Hにて、混合され、反応を伴う場合においては両被処理流動体は反応する。流体圧付与機構p1により送圧を受けて、流動体は、両処理用面1、2間の微小な隙間にて、リングの外側に移動しようとするが、第1リング10は回転しているので、上記領域Hにおいて、混合された流動体は、リングの径の内外方向について内側から外側へ直線的に移動するのではなく、処理用面を平面視した状態において、リングの回転軸を中心として、渦巻き状にリングの内側から外側へ移動する。このように、混合(反応)を行う領域Hにて、渦巻状に内側から外側へ移動することによって、両処理用面1、2間の微小間隔にて、十分な混合(反応)に要する区間を確保することができ、均一な混合を促進することができる。
また、混合(反応)にて生ずる生成物は、上記の微小な第1及び第2の処理用面1、2間にて、均質な生成物となり、特に晶析や析出の場合微粒子となる。
少なくとも、上記の流体圧付与機構p1が負荷する送圧と、上記の接面圧付与機構4の付勢力と、リングの回転による遠心力のバランスの上に、両処理用面1、2間の間隔を好ましい微小な間隔にバランスさせることができ、更に、流体圧付与機構p1が負荷する送圧とリングの回転による遠心力を受けた被処理流動体が、上記の処理用面1、2間の微小な隙間を、渦巻き状に移動して、混合(反応)が促進される。
上記の混合(反応)は、流体圧付与機構p1が負荷する送圧やリングの回転により、強制的に行われる。即ち、混合(反応)は、接近・離反可能に互いに対向して配設され且つ少なくとも一方が他方に対して回転する処理用面1、2間で、強制的に、均一に起こる。
従って、特に、反応による生成物の晶出又は析出は、流体圧付与機構p1が負荷する送圧の調整や、リングの回転速度即ちリングの回転数の調整という、比較的コントロールし易い方法により、制御できる。
このように、この流体処理装置は、送圧や遠心力の調整にて、生成物の大きさに影響を与える処理用面1、2間の間隔の制御を行え、更に、生成物の均一な生成に影響を与える上記領域Hにて移動する距離の制御が行える点で優れたものである。
また、上記の処理は、生成物が析出するものに限らず、液体の場合も含む。また、生成物が微粒子などの微細な固まりである場合、生成物が処理後の流体中に沈殿するものであっても良く、また、連続相中に分散相が存在する分散液の状態にあるものであっても良い。
尚、回転軸50は、鉛直に配置されたものに限定されるものではなく、水平方向に配位されたものであってもよく、傾斜して配位されたものであってよい。処理中、両処理用面1、2間の微細な間隔にて混合(反応)がなされるものであり、実質的に重力の影響を排除できるからである。
図1(A)にあっては、第1導入部d1は、第2ホルダ21において、第2リング20の軸心と一致し、上下に鉛直に伸びたものを示している。但し、第1導入部d1は、第2リング20の軸心と一致しているものに限定されるものではなく、両リング10、20に囲まれた空間に、第1被処理流動体を供給できるものであれば、第2ホルダ21の中央部分22の他の位置に設けられていてもよく、更に、鉛直でなく、斜めに伸びるものであってもよい。
前述の通り、第2ホルダ21の底部即ち下部には、リング収容部41が形成され、そのリング収容部41内に、第2処理用部20が受容されている。また、図示はしないが、回り止めにて、第2処理用部20は、第2ホルダ21に対して回転しないよう、受容されている。上記の第2処理用面2は、第2ホルダ21から露出する。
この実施の形態において、処理用面1、2間の、第1処理用部10及び第2処理用部20の内側が、被処理物の流入部であり、第1処理用部10及び第2処理用部20の外側が、被処理物の流出部である。
具体的には、この実施の形態において、接面圧力付与機構4は、上記のリング収容部41と、リング収容部41の奥に即ちリング収容部41の最深部に設けられた発条受容部42と、スプリング43と、エア導入部44とにて構成されている。
但し、接面圧力付与機構4は、上記リング収容部41と、上記発条受容部42と、スプリング43と、エア導入部44の少なくとも、何れか1つを備えるものであればよい。
上記のスプリング43の一端は、発条受容部42の奥に当接し、スプリング43の他端は、リング収容部41内の第2処理用部20の前部即ち上部と当接する。図1において、スプリング43は、1つしか現れていないが、複数のスプリング43にて、第2処理用部20の各部を押圧するものとするのが好ましい。即ち、スプリング43の数を増やすことによって、より均等な押圧力を第2処理用部20に与えることができるからである。従って、第2ホルダ21については、スプリング43が数本から数十本取付けられたマルチ型とするのが好ましい。
接面圧力付与機構4は、上記の押圧力即ち接面圧力の一部を供給し調節する他、変位調整機構と、緩衝機構とを兼ねる。
詳しくは、接面圧力付与機構4は、変位調整機構として、始動時や運転中の軸方向への伸びや磨耗による軸方向変位にも、空気圧の調整によって追従し、当初の押圧力を維持できる。また、接面圧力付与機構4は、上記の通り、第2処理用部20を変位可能に保持するフローティング機構を採用することによって、微振動や回転アライメントの緩衝機構としても機能するのである。
まず、第1の被処理流動体が、流体圧付与機構p1からの送圧を受けて、密閉されたケースの内部空間へ、第1導入部d1より導入される。他方、回転駆動部による回転軸50の回転によって、第1処理用部10が回転する。これにより、第1処理用面1と第2処理用面2とは微小間隔を保った状態で相対的に回転する。
第1の被処理流動体は、微小間隔を保った両処理用面1、2間で、薄膜流体となり、第2導入部d2から導入された第2被処理流動体は、両処理用面1、2間において、当該薄膜流体と合流して、同様に薄膜流体の一部を構成する。この合流により、第1及び第2の被処理流動体が混合されて生成物が形成される。そして反応を伴う場合にあっては、両流動体が反応して、均一な反応が促進されて、その反応生成物が形成される。これにより、析出を伴う場合にあっては比較的均一で微細な粒子の生成が可能となり、析出を伴わない場合にあっても、均一な混合状態(反応を伴う場合にあっては均一な反応)が実現される。なお、析出した生成物は、第1処理用面1の回転により第2処理用面2との間で剪断を受けることにて、さらに微細化される場合もあると考えられる。ここで、第1処理用面1と第2処理用面2とは、1μmから1mm、特に1μmから10μmの微小間隔に調整されることにより、均一な混合状態(反応を伴う場合にあっては均一な反応)を実現すると共に、数nm単位の超微粒子の生成をも可能とする。
生成物は、両処理用面1、2間から出て、ケース3の排出口32からケース外部へ排出される。排出された生成物は、周知の減圧装置にて、真空或いは減圧された雰囲気内にて霧状にされ、雰囲気内の他に当たることによって流動体として流れ落ちたものが脱気後の液状物として回収することができる。
尚、この実施の形態において、処理装置は、ケースを備えるものとしたが、このようなケースを設けずに実施することもできる。例えば、脱気するための減圧タンク即ち真空タンクを設け、そのタンク内部に、処理装置を配置して、実施することが可能である。その場合、当然上記の排出口は、処理装置には備えられない。
第1処理用面1と第2処理用面2とは、相対的に接近離反可能であり、且つ相対的に回転する。この例では、第1処理用面1が回転し、第2処理用面2が軸方向に移動可能な構造(フローティング構造)を持って第1処理用面1に対して接近離反する。
よって、この例では、第2処理用面2の軸方向位置が、力即ち、前述の接面圧力と離反力のバランスによって、μm単位の精度で設定されることにより、両処理用面1、2間の微小間隔の設定がなされる。
尚、図12~15、17に示す実施の形態において、図面の煩雑を避けるため、第2導入部d2は、省略して描いてある。この点について、第2導入部d2が設けられていない位置の断面と考えればよい。また、図中、Uは上方を、Sは下方を、夫々示している。
他方、離反力としては、離反側の受圧面、即ち第2処理用面2及び離反用調整面23に作用する流体圧と、第1処理用部10の回転による遠心力と、エア導入部44に負圧を掛けた場合の当該負圧とを挙げることができる。
尚、装置を洗浄するに際して、上記のエア導入部44に掛ける負圧を大きくすることにより、両処理用面1、2を大きく離反させることができ、洗浄を容易に行うことができる。
そして、これらの力の均衡によって、第2処理用面2が第1処理用面1に対して所定の微小間隔を隔てた位置にて安定することにより、μm単位の精度での設定が実現する。
まず、流体圧に関しては、密閉された流路中にある第2処理用部20は、流体圧付与機構p1から被処理流動体の送り込み圧力即ち流体圧を受ける。その際、流路中の第1処理用面に対向する面、即ち第2処理用面2と離反用調整面23が離反側の受圧面となり、この受圧面に流体圧が作用して、流体圧による離反力が発生する。
次に、遠心力に関しては、第1処理用部10が高速に回転すると、流体に遠心力が作用し、この遠心力の一部は両処理用面1、2を互いに遠ざける方向に作用する離反力となる。
更に、上記のエア導入部44から負圧を第2処理用部20へ与えた場合には、当該負圧が離反力として作用する。
以上、本願の説明においては、第1第2の処理用面1、2を互いに離反させる力を離反力として説明するものであり、上記に示した力を離反力から排除するものではない。
接面圧力を増加させる場合、接面圧力付与機構4において、エア導入部44から空気圧即ち正圧を付与し、又は、スプリング43を押圧力の大きなものに変更或いはその個数を増加させればよい。
離反力を増加させる場合、流体圧付与機構p1の送り込み圧力を増加させ、或いは第2処理用面2や離反用調整面23の面積を増加させ、またこれに加えて、第1処理用部10の回転を調整して遠心力を増加させ或いはエア導入部44からの圧力を低減すればよい。もしくは負圧を付与すればよい。スプリング43は、伸びる方向に押圧力を発する押し発条としたが、縮む方向に力を発する引き発条として、接面圧力付与機構4の構成の一部又は全部とすることが可能である。
離反力を減少させる場合、流体圧付与機構p1の送り込み圧力を減少させ、或いは第2処理用面2や離反用調整面23の面積を減少させ、またこれに加えて、第1処理用部10の回転を調整して遠心力を減少させ或いはエア導入部44からの圧力を増加させれば良い。もしくは負圧を低減すればよい。
メカニカルシールにあっては、第2処理用部20がコンプレッションリングに相当するが、この第2処理用部20に対して流体圧が加えられた場合に、第2処理用部20を第1処理用部10から離反する力が作用する場合、この力がオープニングフォースとされる。
より詳しくは、上記の第1の実施の形態のように、第2処理用部20に離反側の受圧面即ち、第2処理用面2及び離反用調整面23のみが設けられている場合には、送り込み圧力の全てがオープニングフォースを構成する。なお、第2処理用部20の背面側にも受圧面が設けられている場合、具体的には、後述する図12(B)及び図17の場合には、送り込み圧力のうち、離反力として働くものと接面圧力として働くものとの差が、オープニングフォースとなる。
図12(B)に示す通り、この第2処理用部20のリング収容部41より露出する部位であり且つ内周面側に、第2処理用面2と反対側即ち上方側を臨む接近用調整面24が設けられている。
即ち、この実施の形態において、接面圧力付与機構4は、リング収容部41と、エア導入部44と、上記接近用調整面24とにて構成されている。但し、接面圧力付与機構4は、上記リング収容部41と、上記発条受容部42と、スプリング43と、エア導入部44と、上記接近用調整面24の少なくとも、何れか1つを備えるものであればよい。
接近用調整面24と、第2処理用面2及び離反用調整面23とは、共に前述の被処理流動体の送圧を受ける受圧面であり、その向きにより、上記接面圧力の発生と、離反力の発生という異なる作用を奏する。
接近用調整面24の先端と離反用調整面23の先端とは、共に環状の第2処理用部20の内周面25即ち先端線L1に規定されている。このため、接近用調整面24の基端線L2をどこに置くかの決定で、バランス比Kの調整が行われる。
即ち、この実施の形態において、被処理用流動体の送り出しの圧力をオープニングフォースとして利用する場合、第2処理用面2及び離反用調整面23との合計投影面積を、接近用調整面24の投影面積より大きいものとすることによって、その面積比率に応じたオープニングフォースを発生させることができる。
摺動面実面圧P、即ち、接面圧力のうち流体圧によるものは次式で計算される。
P=P1×(K-k)+Ps
ここでP1は、被処理流動体の圧力即ち流体圧を示し、Kは上記のバランス比を示し、kはオープニングフォース係数を示し、Psはスプリング及び背圧力を示す。
このバランスラインの調整により摺動面実面圧Pを調整することで処理用面1、2間を所望の微小隙間量にし被処理流動体による薄膜流体を形成させ、生成物を微細とし、また、均一な混合(反応)処理を行うのである。
この関係を纏めると、上記の生成物を粗くする場合、バランス比を小さくし、面圧Pを小さくし、上記隙間を大きくして、上記厚みを大きくすればよい。逆に、上記の生成物をより細かくする場合、バランス比Kを大きくし、面圧Pを大きくし、上記隙間を小さくし、上記厚みを小さくする。
このように、接面圧力付与機構4の一部として、接近用調整面24を形成して、そのバランスラインの位置にて、接面圧力の調整、即ち処理用面間の隙間を調整するものとしても実施できる。
上述の通り、この装置は、第2処理用部20と、第2処理用部20に対して回転する第1処理用部10とについて、被処理流動体の送り込み圧力と当該回転遠心力、また接面圧力で圧力バランスを取り両処理用面に所定の薄膜流体を形成させる構成にしている。またリングの少なくとも一方をフローティング構造とし芯振れなどのアライメントを吸収し接触による磨耗などの危険性を排除している。
また、図12(B)に示す実施の形態において、図17に示すように、上記の離反用調整面23を設けずに実施することも可能である。
図12(B)や図17に示す実施の形態のように、接近用調整面24を設ける場合、接近用調整面24の面積A1を上記の面積A2よりも大きいものとすることにより、オープニングフォースを発生させずに、逆に、被処理流動体に掛けられた所定の圧力は、全て接面圧力として働くことになる。このような設定も可能であり、この場合、他の離反力を大きくすることにより、両処理用面1、2を均衡させることができる。
上記の面積比にて、流体から受ける力の合力として、第2処理用面2を第1処理用面1から離反させる方向へ作用させる力が定まる。
第2処理用部20と第2ホルダ21との間は、気密となるようにシールし、当該シールには、周知の手段を採用することができる。
第2ホルダ21の温度調整用ジャケット46は、第2ホルダ21内において、リング収容部41の側面に形成された水回り用の空間であり、第2ホルダ21の外部に通じる通路47、48と連絡している。通路47、48は、何れか一方が温度調整用ジャケット46に、冷却用或いは加熱用の媒体を導入し、何れか他方が当該媒体を排出する。
また、ケース3の温度調整用ジャケット35は、ケース3の外周を被覆する被覆部34にて、ケース3の外周面と当該被覆部34との間に設けられた、加熱用水或いは冷却水を通す通路である。
この実施の形態では、第2ホルダ21とケース3とが、上記の温度調整用のジャケットを備えるものとしたが、第1ホルダ11にも、このようなジャケットを設けて実施することが可能である。
このシリンダ機構7は、第2ホルダ21内に設けられたシリンダ空間部70と、シリンダ空間部70をリング収容部41と連絡する連絡部71と、シリンダ空間部70内に収容され且つ連絡部71を通じて第2処理用部20と連結されたピストン体72と、シリンダ空間部70上部に連絡する第1ノズル73と、シリンダ空間部70下部に連絡する第2ノズル74と、シリンダ空間部70上部とピストン体72との間に介された発条などの押圧体75とを備えたものである。
図示はしないが、具体的には、コンプレッサなどの圧力源と第1ノズル73とを接続し、第1ノズル73からシリンダ空間部70内のピストン体72上方に空気圧即ち正圧を掛けることにて、ピストン体72を下方に摺動させ、第1及び第2処理用面1、2間の隙間を狭めることができる。また図示はしないが、コンプレッサなどの圧力源と第2ノズル74とを接続し、第2ノズル74からシリンダ空間部70内のピストン体72の下方に空気圧即ち正圧を掛けることにて、ピストン体72を上方に摺動させ、第2処理用部20を移動させて第1及び第2処理用面1、2間の隙間を広げる、即ち開く方向に移動させることができる。このように、ノズル73、74にて得た空気圧で、接面圧力を調整できるのである。
このように上記隙間の最大及び最小の開き量を規制しつつ、ピストン体72とシリンダ空間部70の最上部70aとの間隔z1、換言するとピストン体72とシリンダ空間部70の最下部70bとの間隔z2を上記ノズル73、74の空気圧にて調整する。
また圧力源は、正圧を供給するものでも負圧を供給するものでも何れでも実施可能である。真空などの負圧源と、ノズル73、74とを接続する場合、上記の動作は反対になる。
前述の他の接面圧力付与機構4に代え或いは前述の接面圧力付与機構4の一部として、このようなシリンダ機構7を設けて、被処理流動体の粘度や性状によりノズル73、74に接続する圧力源の圧力や間隔z1、z2の設定を行い薄膜流体の厚みを所望値にしせん断力をかけて均一な混合状態(反応を伴う場合にあっては均一な反応)を実現し、微細な粒子を生成させることができる。特に、このようなシリンダ機構7にて、洗浄時や蒸気滅菌時など摺動部の強制開閉を行い洗浄や滅菌の確実性を上昇させることも可能とした。
この様な凹部13を形成することにより被処理流動体の吐出量の増加または発熱量の減少への対応や、キャビテーションコントロールや流体軸受け効果などの効果がある。
上記の図16に示す各実施の形態において、凹部13は、第1処理用面1に形成するものとしたが、第2処理用面2に形成するものとしても実施可能であり、更には、第1及び第2の処理用面1、2の双方に形成するものとしても実施可能である。
図12乃至図17に示す実施の形態においても、特に明示した以外の構成については図1(A)又は図11(C)に示す実施の形態と同様である。
流体圧付与機構p1には、加圧装置として、既述のとおり、コンプレッサを用いて実施するのが好ましいが、常に被処理流動体に所定の圧力を掛けることが可能であれば、他の手段を用いて実施することもできる。例えば、被処理流動体の自重を利用して、常に一定の圧力を被処理流動体に付与するものとしても実施可能である。
このような画期的な方法により、両処理用面1、2間の間隔を1μmから1mmとする調整、特に、1~10μmとする調整を可能とした。
この他、このような流体圧付与機構p1を用いて加圧するものではなく、被処理流動体の流路は開放されたものであっても実施可能である。
図18乃至図20へ、そのような処理装置の一実施の形態を示す。尚、この実施の形態において、処理装置として、生成されたものから、液体を除去し、目的とする固体(結晶)のみを最終的に確保する機能を備えた装置を例示する。
図18(A)は処理装置の略縦断面図であり、図18(B)はその一部切欠拡大断面図である。図19は、図18に示す処理装置が備える第1処理用部101の平面図である。図20は、上記処理装置の第1及び第2処理用部101、102の一部切欠要部略縦断面図である。
尚、図18(B)及び図20において、図面の煩雑を避けるため、第2導入部d2は、省略して描いてある(第2導入部d2が設けられていない位置の断面と考えればよい)。
図18(A)に示す通り、この流体処理装置は、混合装置Gと、減圧ポンプQとを備えたものである。この混合装置Gは、回転する部材である第1処理用部101と、当該処理用部101を保持する第1ホルダ111と、ケースに対して固定された部材である第2処理用部102と、当該第2処理用部102が固定された第2ホルダ121と、付勢機構103と、動圧発生機構104(図19(A))と、第1ホルダ111と共に第1処理用部101を回転させる駆動部と、ハウジング106と、第1被処理流動体を供給(投入する)する第1導入部d1と、流体を減圧ポンプQへ排出する排出部108とを備える。駆動部については図示を省略する。
上記の処理用面110、120は、鏡面研磨された平坦部を有する。この実施の形態において、第2処理用部102の処理用面120は、面全体に鏡面研磨が施された平坦面である。また、第1処理用部101の処理用面110は、面全体を第2処理用部102と同様の平坦面とするが、図19(A)へ示す通り、平坦面中に、複数の溝112...112を有する。この溝112... 112は、第1処理用部101が呈する円柱の中心を中心側として円柱の外周方向へ、放射状に伸びる。
上記の第1及び第2の処理用部101、102の処理用面110、120についての、鏡面研磨は、面粗度Raを0.01~1.0μmとするのが好ましい。この鏡面研磨については、Raを0.03~0.3μmとするのがより好ましい。
処理用部101、102の材質については、硬質且つ鏡面研磨が可能なものを採用する。処理用部101、102のこの硬さについて、少なくともビッカース硬さ1500以上が好ましい。また、線膨張係数が小さい素材を、若しくは、熱伝導の高い素材を、採用するのが好ましい。処理にて熱を発する部分と他の部分との間で、膨張率の差が大きいと歪みが発生して、適正なクリアランスの確保に影響するからである。
このような処理用部101、102の素材として、特に、SIC即ちシリコンカーバイトでビッカース硬さ2000~2500のもの、表面にDLC即ちダイヤモンドライクカーボンでビッカース硬さ3000~4000のもの、コーティングが施されたSIC、WC即ちタングステンカーバイトでビッカース硬さ1800のもの、表面にDLCコーティングが施されたWC、ZrB2やBTC、B4Cに代表されるボロン系セラミックでビッカース硬さ4000~5000のものなどを採用するのが好ましい。
図示はしないが、上記の駆動部は、電動機などの動力源と、当該動力源から動力の供給を受けて回転するシャフト50とを備える。
図18(A)に示すように、シャフト50は、ハウジング106の内部に配され上下に伸びる。そして、シャフト50の上端部に上記の第1ホルダ111が、設けられている。第1ホルダ111は、第1処理用部101を保持するものであり、上記の通りシャフト50に設けられることにより、第1処理用部101の処理用面110を第2処理用部102の処理用面120に対応させる。
一方、第2ホルダ121の上面中央には、第2処理用部102を受容する受容凹部124が形成されている。
上記の受容凹部124は、環状の横断面を有する。第2処理用部102は、受容凹部124と、同心となるように円柱状の受容凹部124内に収容される。
この受容凹部124の構成は、図1(A)に示す実施の形態と同様である(第1処理用部101は第1リング10と、第1ホルダ111は第1ホルダ11と、第2処理用部102は第2リング20と、第2ホルダ121は第2ホルダ21と対応する)。
同様に、第2処理用部102の内周面102aと受容凹部124の中心部分22の外周面との間には、図18(B)に示すように、隙間t2が設定される。
上記隙間t1、t2の夫々は、振動や偏芯挙動を吸収するためのものであり、動作寸法以上確保され且つシールが可能となる大きさに設定する。例えば、第1処理用部101の直径が100mmから400mmの場合、当該隙間t1、t2の夫々は、0.05~0.3mmとするのが好ましい。
第1ホルダ111は、シャフト50へ一体に固定され、シャフト50と共に回転する。また、図示しないが、回り止めによって、第2ホルダ121に対して、第2処理用部102は回らない。しかし、両処理用面110、120間に、処理に必要な0.1~10μmのクリアランス、即ち図20(B)に示す微小な間隔tを確保するため、図18(B)に示すように、受容凹部124の底面、即ち天部と、第2処理用部102の天部124a、即ち上面との間に隙間t3が設けられる。この隙間t3については、上記のクリアランスと共に、シャフト50の振れや伸びを考慮して設定する。
即ち、この実施の形態において、付勢機構103と、上記隙間t1~t3とが、フローティング機構を構成し、このフローティング機構によって、少なくとも第2処理用部102の中心や傾きを、数μmから数mmの程度の僅かな量、可変としている。これにて、回転軸の芯振れ、軸膨張、第1処理用部101の面振れ、振動を吸収する。
溝112の左右両側面112a、112bの間隔w1は、第1処理用部101の中心x側から、第1処理用部101の外側y即ち外周面側に向かうにつれて小さくなる。また、溝112の深さw2は、図19(B)へ示すように、第1処理用部101の中心x側から、第1処理用部101の外側y即ち外周面側に向かうにつれて、小さくなる。即ち、溝112の底112cは、第1処理用部101の中心x側から、第1処理用部101の外側y即ち外周面側に向かうにつれて、浅くなる。
このように、溝112は、その幅及び深さの双方を、外側y即ち外周面側に向かうにつれて、漸次減少するものとして、その横断面積を外側yに向けて漸次減少させている。そして、溝112の先端即ちy側は、行き止まりとなっている。即ち、溝112の先端即ちy側は、第1処理用部101の外周面101bに達するものではなく、溝112の先端と外周面101bとの間には、外側平坦面113が介在する。この外側平坦面113は、処理用面110の一部である。
但し、溝112の幅及び深さの何れか一方についてのみ、上記の構成を採るものとして、断面積を減少させるものとしてよい。
上記の動圧発生機構104は、第1処理用部101の回転時、両処理用部101、102間を通り抜けようとする流体によって、両処理用部101、102の間に所望の微小間隔を確保することを可能とする、両処理用部101、102を離反させる方向に働く力を発生させる。このような動圧の発生により、両処理用面110、120間に、0.1~10μmの微小間隔を発生させることができる。このような微小間隔は、処理の対象によって、調整し選択すればよいのであるが、1~6μmとするのが好ましく、より好ましくは、1~2μmである。この装置においては、上記のような微小間隔による従来にない均一な混合状態(反応を伴う場合にあっては均一な反応)の実現と微細な粒子の生成が可能である。
このように溝112...112が湾曲して伸びることにより、動圧発生機構104による離反力の発生をより効果的に行うことができる。
図18(A)に示すように、ホッパ170から投入され、第1導入部d1を通ってくる第1被処理流動体Rは、環状の第2処理用部102の中空部を通り、第1処理用部101の回転による遠心力を受け、両処理用部101、102間に入り、回転する第1処理用部101の処理用面110と、第2処理用部102の処理用面120との間にて、均一な混合(反応)と、場合により微細な粒子の生成が行われ、その後、両処理用部101、102の外側に出て、排出部108から減圧ポンプQ側へ排出される(以下必要に応じて第1被処理流動体Rを単に流体Rと呼ぶ)。
上記において、環状の第2処理用部102の中空部に入った流体Rは、図20(A)へ示すように、先ず、回転する第1処理用部101の溝112に入る。一方、鏡面研磨された、平坦部である両処理用面110、120は、空気や窒素などの気体を通しても気密性が保たれている。従って、回転による遠心力を受けても、そのままでは、付勢機構103によって押し合わされた両処理用面110、120の間に、溝112から流体Rは入り込むことはできない。しかし、流路制限部として形成された溝112の上記両側面112a、112bや底112cに、流体Rは徐々に突き当たり、両処理用面110、120を離反させる方向に働く動圧を発生させる。図20(B)へ示すように、これによって、流体Rが溝112から平坦面に滲み出し、両処理用面110、120の間に微小間隔t即ちクリアランスを確保することができる。そして、このような鏡面研磨された平坦面の間で、均一な混合(反応)と、場合により微細な粒子の生成が行われる。また上述の溝112の湾曲が、より確実に流体へ遠心力を作用させ、上記動圧の発生をより効果的にしている。
このように、この流体処理装置は、動圧と付勢機構103による付勢力との均衡にて、両鏡面即ち処理用面110、120間に、微細で均一な間隔即ちクリアランスを確保することを可能とした。そして、上記の構成により、当該微小間隔は、1μm以下の超微細なものとすることができる。
また、上記フローティング機構の採用により、処理用面110、120間のアライメントの自動調整が可能となり、回転や発生した熱による各部の物理的な変形に対して、処理用面110、120間の各位置における、クリアランスのばらつきを抑制し、当該各位置における上記の微小間隔の維持を可能とした。
図21(A)(B)に示すように、溝112は、流路制限部の一部として、先端に平らな壁面112dを備えるものとして実施することができる。また、この図21に示す実施の形態では、底112cにおいて、第1壁面112dと、内周面101aとの間に段差112eが設けられており、この段差112eも流路制限部の一部を構成する。
図22(A)(B)に示すように、溝112は、複数に分岐する枝部112f...112fを備えるものとし、各枝部112fがその幅を狭めることにより流路制限部を備えるものとしても実施可能である。
図21及び図22の実施の形態においても、特に示した以外の構成については、図1(A)、図11(C)、図18乃至図20に示す実施の形態と同様である。
また、この図23(A)(B)に示す場合、溝112の幅及び深さの少なくとも何れか一方の寸法を漸次小さくすることも併せて実施することができる。
尚、溝112の構成について、上記の図19、図21乃至図23に示すものに限定されるものではなく、他の形状の流路制限部を備えたものとして実施することが可能である。
例えば、図19、図21乃至図23に示すものでは、溝112は、第1処理用部101の外側に突き抜けるものではなかった。即ち、第1処理用部101の外周面と、溝112との間には、外側平坦面113が存在した。しかし、このような実施の形態に限定されるものではなく、上述の動圧を発生されることが可能であれば、溝112は、第1処理用部101の外周面側に達するものであっても実施可能である。
例えば、図23(B)に示す第1処理用部101の場合、点線で示すように、溝112の他の部位よりも断面積が小さな部分を、外側平坦面113に形成して実施することができる。
また、溝112を、上記の通り内側から外側へ向けて漸次断面積を小さくするように形成し、溝112の第1処理用部101の外周に達した部分(終端)を、最も断面積が小さいものとすればよい(図示せず)。但し、動圧を効果的に発生させる上で、図19、図21乃至図23に示すように、溝112は、第1処理用部101の外周面側に突き抜けないほうが好ましい。
この流体処理装置は、平坦処理用面を有する回転部材と同じく平坦処理用面を有する固定部材とをそれらの平坦処理用面で同心的に相対向させ、回転部材の回転下に固定部材の開口部より被処理原料を供給しながら両部材の対向平面処理用面間にて処理する流体処理装置において機械的にクリアランスを調整するのではなく、回転部材に増圧機構を設けて、その圧力発生によりクリアランスを保持し、かつ、機械的クリアランス調整では不可能であった1~6μmの微小クリアランスを可能とし、混合(反応)の均一化及び、場合により生成粒子の微細化の能力が著しく向上出来たものである。
即ち、この流体処理装置は、回転部材と固定部材がその外周部に平坦処理用面を有しその平坦処理用面において、面上の密封機能を有することで、流体静力学的な即ちハイドロスタティックな力、流体動力学的な即ちハイドロダイナミックな力、或いは、エアロスタティック-エアロダイナミックな力を発生させる高速回転式の流体処理装置を提供しようとするものである。上記の力は、上記密封面間に僅かな間隙を発生させ、また非接触で機械的に安全で高度な混合(反応)の均一化の機能を有した流体処理装置を提供することができる。この僅かな隙間が形成されうる要因は、一つは、回転部材の回転速度によるものであり、もう一つは、被処理物(流体)の投入側と排出側の圧力差によるものである。投入側に圧力付与機構が付設されていない場合即ち大気圧下で被処理物(流体)を投入される場合、圧力差が無いわけであるから回転部材の回転速度だけで密封面間の分離を生じさせる必要がある。これは、ハイドロダイナミックもしくはエアロダイナミック力として知られている。
この場合、タンクT内を真空或いは真空に近い状態に減圧することにて、混合装置Gにて生成された被処理物をタンクT内に霧状に噴射せしめ、タンクTの内壁にぶつかって流れ落ちる被処理物を回収すること、或いはこのような流れ落ちる被処理物に対して気体(蒸気)として分離されタンクT内上部に充満するものを回収することにて、処理後の目的物を得ることができる。
また、減圧ポンプQを用いる場合も、図24(B)へ示すように、混合装置Gに、減圧ポンプQを介して、気密なタンクTを接続することにより、当該タンクT内にて、処理後の被処理物を霧状にして、目的物の分離・抽出を行うことができる。
更に、図24(C)へ示すように、減圧ポンプQを直接タンクTに接続し、当該タンクTに、減圧ポンプQと、減圧ポンプQとは別の流体Rの排出部とを接続して、目的物の分離を行うことができる。この場合、気化部については、減圧ポンプQに吸いよせられ、液体R(液状部)は排出部より、気化部とは別に排出される。
次に、装置への被処理流動体の導入に関する他の実施の形態について、順に説明する。
第3導入部d3は、第1の被処理流動体と混合させる第3の被処理流動体を処理用面1、2間へ供給する。この実施の形態において、第3導入部d3は、第2リング20の内部に設けられた流体の通路であり、その一端が第2処理用面2にて開口し、他の一端に第3流体供給部p3が接続されている。
第3流体供給部p3には、コンプレッサ、その他のポンプを採用することができる。
第3導入部d3の第2処理用面2における開口部は、第2導入部d2の開口部よりも、第1処理用面1の回転の中心の外側に位置する。即ち、第2処理用面2において、第3導入部d3の開口部は、第2導入部d2の開口部よりも、下流側に位置する。第3導入部d3の開口部と第2導入部d2の開口部との間には、第2リング20の径の内外方向について、間隔が開けられている。
この図1(B)へ示す装置も、第3導入部d3以外の構成については、図1(A)へ示す実施の形態と同様である。尚、この図1(B)、更に、以下に説明する、図1(C)、図1(D)、図2~図11において、図面の煩雑を避けるため、ケース3を省略する。尚、図9(B)(C)、図10、図11(A)(B)においては、ケース3の一部を描いてある。
第4導入部d4は、第1の被処理流動体と混合させる第4の被処理流動体を処理用面1、2間へ供給する。この実施の形態において、第4導入部d4は、第2リング20の内部に設けられた流体の通路であり、その一端が第2処理用面2にて開口し、他の一端に第4流体供給部p4が接続されている。
第4流体供給部p4には、コンプレッサ、その他のポンプを採用することができる。
第4導入部d4の第2処理用面2における開口部は、第3導入部d3の開口部よりも、第1処理用面1の回転の中心の外側に位置する。即ち、第2処理用面2において、第4導入部d4の開口部は、第3導入部d3の開口部よりも、下流側に位置する。
この図1(C)へ示す装置について、第4導入部d4以外の構成については、図1(B)へ示す実施の形態と同様である。
また、図示はしないが、更に、第5導入部や、第6導入部など、5つ以上の導入部を設けて、夫々5種以上の被処理流動体を、混合(反応)させるものとしても実施できる。
上記の図1(D)へ示す装置では、第2導入部d2の開口部と、第3導入部d3の開口部は、共に第2リング20の第2処理用面2に配置されるものであった。しかし、導入部の開口部は、このような処理用面に対する配置に限定されるものではない。特に、図2(A)へ示す通り、第2導入部d2の開口部を、第2リング20の内周面の、第2処理用面2に隣接する位置に設けて実施することもできる。この図2(A)へ示す装置において、第3導入部d3の開口部は、図1(B)へ示す装置と同様、第2処理用面2に配置されているが、第2導入部d2の開口部を、このように第2処理用面2の内側であって、第2処理用面2へ隣接する位置に配置することによって、第2の被処理流動体を処理用面に直ちに導入できる。
また、上記の図1(D)へ示す装置についても、第1導入部d1の開口部と第2導入部d2の開口部との間には、第2リング20の径の内外方向について、間隔が開けられていたが、そのような間隔を設けずに、両処理用面1、2間に第1及び第2の被処理流動体を導入すると直ちに両流動体が合流するものとしても実施できる(図示しない)。処理の対象によって、このような開口部の配置を選択すればよい。
上記の図1(B)及び図1(C)に示す実施の形態では、第2処理用面2において、第3導入部d3の開口部を、第2導入部d2の開口部の下流側、言い換えると、第2リング20の径の内外方向について第2導入部d2の開口部の外側に配置するものとした。この他、図2(C)及び図3(A)へ示す通り、第2処理用面2において、第3導入部d3の開口部を、第2導入部d2の開口部と、第2リング20の周方向r0について異なる位置に配置するものとしても実施できる。図3において、m1は第1導入部d1の開口部即ち第1開口部を、m2は第2導入部d2の開口部即ち第2開口部を、m3は第3導入部d3の開口部(第3開口部)を、r1はリングの径の内外方向を、夫々示している。
また、第1導入部d1を第2リング20に設ける場合も、図2(D)へ示す通り、第2処理用面2において、第1導入部d1の開口部を、第2導入部d2の開口部と、第2リング20の周方向について異なる位置に配置するものとしても実施できる。
上記に示す装置において、第2導入部乃至第5導入部は、夫々異なる被処理流動体即ち、第2、第3、第4、第5の被処理流動体を、導入することができる。一方、第2~第5の開口部m2~m5から、全て同種の即ち、第2被処理流動体を処理用面間に導入するものとしても実施できる。図示はしないが、この場合、第2導入部乃至第5導入部は、リング内部にて連絡しており、一つの流体供給部、即ち第2流体供給部p2に接続されているものとして実施できる。
また、リングの周方向r0の異なる位置に導入部の開口部を複数設けたものと、リングの径方向即ち径の内外方向r1の異なる位置に導入部の開口部を複数設けたものを、複合して実施することもできる。
例えば、図3(D)へ示す通り、第2処理用面2に8つの導入部の開口部m2~m9が設けられており、そのうち4つであるm2~m5は、リングの周方向r0の異なる位置であり且つ径方向r1について同じ位置に設けられたものであり、他の4つであるm6~m9はリングの周方向r0の異なる位置であり且つ径方向r1について同じ位置に設けられている。そして、当該他の開口部m6~m9は、径方向r1について、上記4つの開口部m2~m5の径方向の外側に配置されている。また、この外側の開口部は、夫々、内側の開口部と、リングの周方向r0について同じ位置に設けてもよいが、リングの回転を考慮して、図3(D)へ示すように、リングの周方向r0の異なる位置に設けて実施することもできる。また、その場合も、開口部について、図3(D)に示す配置や数に限定されるものではない。
例えば、図3(E)へ示す通り、径方向外側の開口部が多角形の頂点位置、即ちこの場合四角形の頂点位置に配置され、当該多角形の辺上に、径方向内側の開口部が位置するように配置することもできる。勿論この他の配置を採ることもできる。
また、第1開口部m1以外の開口部は、何れも第2被処理流動体を処理用面間に導入するものとした場合、各第2被処理流動体を導入する当該開口部を、処理用面の周方向r0について、点在させるのではなく、図3(F)へ示す通り、周方向r0について、連続する開口部として実施することもできる。
また、処理の対象によっては、図5(A)へ示す通り、図4(D)へ示す装置において、第2リング20に第4導入部d4を設けて第4の被処理流動体を両処理用面1、2間へ導入するものとしても実施できる。
図5(C)へ示す通り、図5(B)へ示す装置において、第1リング10に第3導入部d3を設けて、第1処理用面1において、第3導入部d3の開口部を、第2導入部d2の開口部と、第1リング10の周方向について異なる位置に配置するものとしても実施できる。
図5(D)へ示す通り、図5(B)へ示す装置において、第2ホルダ21へ第1導入部d1を設ける代わりに、第2リング20へ第1導入部d1を設け、第2処理用面2に、第1導入部d1の開口部を配置するものとしても実施できる。この場合、第1及び第2の導入部d1、d2の両開口部は、リングの径の内外方向について、同じ位置に配置されている。
図5(C)へ示す装置において、第2及び第3の導入部d2、d3の両開口部を、第1リング10の径の内外方向について同じ位置に設けると共に、第1リング10の周方向即ち回転方向について異なる位置に設けたが、当該装置において、図6(B)へ示す通り、第2及び第3導入部d2、d3の両開口部を、第1リング10の周方向について同じ位置に設けると共に、第1リング10の径の内外方向について異なる位置に設けて実施することができる。この場合図6(B)へ示す通り、第2及び第3導入部d2、d3の両開口部の間には、第1リング10の径の内外方向に間隔を開けておくものとしても実施でき、または図示はしないが、当該間隔を開けずに直ちに、第2被処理流動体と第3被処理流動体とが合流するものとしても実施できる。
また、図6(C)へ示す通り、第2ホルダ21へ第1導入部d1を設ける代わりに、第2導入部d2と共に、第1リング10へ第1導入部d1を設けて実施することもできる。この場合、第1処理用面1において、第1導入部d1の開口部を、第2導入部d2の開口部の、上流側(第1リング10の径の内外方向について内側)に設ける。第1導入部d1の開口部と第2導入部d2の開口部との間には、第1リング10の径の内外方向について、間隔を開けておく。但し図示はしないが、このような間隔を開けずに実施することもできる。
また、図6(D)へ示す通り、図6(C)へ示す装置の第1処理用面1にあって、第1リング10の周方向の異なる位置に、第1導入部d1と第2導入部d2夫々の開口部を配置するものとして実施することができる。
また、図示はしないが、図6(C)(D)へ示す実施の形態において、第1リング10へ3つ以上の導入部を設けて、第2処理用面2において、周方向の異なる位置に、或いは、リングの径の内外方向の異なる位置に、各開口部を配置するものとして実施することもできる。例えば、第2処理用面2において採った、図3(B)~図3(F)に示す開口部の配置を第1処理用面1においても採用することができる。
図7(B)へ示す通り、図7(A)へ示す実施の形態において、第3導入部d3を、第2リング20へ設けて、第3導入部d3の開口部を第2処理用面2へ配置することができる。
また、図7(C)へ示す通り、第1導入部d1を第2ホルダ21へ設ける代わりに、第1ホルダ11へ設けて実施することができる。この場合、第1ホルダ11上面の第1リング10に囲まれた部位において、第1リング10の回転の中心軸に第1導入部d1の開口部を配置するのが好ましい。また、この場合、図示の通り、第2導入部d2を第1リング10へ設けて、第1処理用面1へ、その開口部を配置することができる。また、図示はしないが、この場合、第2導入部d2を第2リング20へ設けて、第2処理用面2へ、その開口部を配置することができる。
更に、図7(D)へ示す通り、図7(C)へ示す第2導入部d2を、第1導入部d1と共に、第1ホルダ11へ設けて実施することもできる。この場合、第1ホルダ11上面の第1リング10に囲まれた部位において、第2導入部d2の開口部を配置する。また、この場合、図7(C)において、第2リング20へ設けた第2導入部d2を、第3導入部d3とすればよい。
また、図8(B)へ示す通り、図8(A)に示す装置において、第2リング20に第2導入部d2を設ける代わりに、図7(B)の装置と同様に第1ホルダ11に第2導入部d2を設けて実施することができる。
また、図示はしないが、図8(B)へ示す装置において、第2導入部d2を、第1ホルダ11に代え第2ホルダ21へ設けて実施することもできる。この場合、第2導入部d2は、図4(A)の装置と同様である。図8(C)へ示す通り、図8(B)へ示す装置において、第2リング20に第3導入部d3を設けて、当該導入部d3の開口部を、第2処理用面2に配置して実施することもできる。
更に、図8(D)へ示す通り、第1ホルダ11を回転させずに、第2ホルダ21のみを回転させるものとしても実施できる。図示はしないが、図1(B)~図7に示す装置においても、第1ホルダ11と共に第2ホルダ21を回転させるものや、或いは第2ホルダ21のみ単独で回転させるものとしても実施できる。
この他、図10(B)へ示す通り、第1リング10及び第2リング20の外側から、内側に向けて、第1の被処理流動体を供給するものとしても実施できる。この場合、図示の通り、第1ホルダ11及び第2ホルダ21の外側をケース3にて密閉し、第1導入部d1を当該ケース3に直接設けて、ケースの内側であって、両リング10、20の突合せ位置と対応する部位に、当該導入部の開口部を配置する。そして、図1(A)の装置において第1導入部d1が設けられていた位置、即ち第1ホルダ11におけるリング1の中心となる位置に、排出部36を設ける。また、ホルダの回転の中心軸を挟んで、ケースの当該開口部の反対側に、第2導入部d2の開口部を配置する。但し、第2導入部d2の開口部は、第1導入部d1の開口部と同様、ケースの内側であって、両リング10、20の突合せ位置と対応する部位に配置するものであればよく、上記のように、第1導入部d1の開口部の反対側に形成するのに限定されるものではない。
この場合、両リング10、20の径の外側が、上流となり、両リング10、20の内側が下流側となる。
また、図11(B)へ示す通り、図11(A)に示す装置の第2導入部d2を第3導入部d3とし、別途第2導入部d2を設けるものとしても実施できる。この場合、第2処理用面2において第2導入部d2の開口部を第3導入部d3の開口部よりも下流側に配置する。
前述の図4に示す各装置、図5(A)、図7(A)(B)(D)、図8(B)(C)に示す装置は、処理用面1、2間に達する前に、第1の被処理流動体に対して、他の被処理流動体が合流するものであり、晶出や析出の反応の速いものには適さない。しかし、反応速度の遅いものについては、このような装置を採用することもできる。
前述の通り、この流体処理装置は、被処理流動体に所定の圧力を付与する流体圧付与機構と、この所定圧力の被処理流動体が流される密封された流体流路に設けられた第1処理用部10と第1処理用部10に対して相対的に接近離反可能な第2処理用部20の少なくとも2つの処理用部と、これらの処理用部10、20において互いに対向する位置に設けられた第1処理用面1及び第2処理用面2の少なくとも2つの処理用面と、第1処理用部10と第2処理用部20とを相対的に回転させる回転駆動機構とを備え、両処理用面1、2間にて、少なくとも2種の被処理流動体の混合の処理を行う(反応を伴う場合にあっては反応の処理も行う)ものである。第1処理用部10と第2処理用部20のうち少なくとも第2処理用部20は、受圧面を備えるものであり、且つ、この受圧面の少なくとも一部が第2処理用面2により構成され、受圧面は、流体圧付与機構が被処理流動体の少なくとも一方に付与する圧力を受けて第1処理用面1から第2処理用面2を離反させる方向に移動させる力を発生させる。そして、この装置にあって、接近離反可能且つ相対的に回転する第1処理用面1と第2処理用面2との間に上記の圧力を受けた被処理流動体が通されることにより、各被処理流動体が所定厚みの薄膜流体を形成しながら両処理用面1、2間を通過することで、当該被処理流動体間において、所望の混合状態(反応)が生じる。
尚、上記の加圧装置は、送り込み圧の増減の調整を行えるものを採用する。この加圧装置は、設定した圧力を一定に保つことができる必要があるが、処理用面間の間隔を調整するパラメータとして、調整を行える必要があるからである。
この接面圧付与機構が、前述の装置における、微振動やアライメントを調整する緩衝機構や、変位調整機構を構成するものとして実施することができる。
上記のように、一方の被処理流動体の装置内への供給口となる第1導入部の開口部を第2ホルダに設けるものに限定されるものではなく、第1導入部の当該開口部を第1ホルダに設けるものとしてもよい。また、第1導入部の当該開口部を、両処理用面の少なくとも一方に形成して実施することもできる。但し、反応によって、先に処理用面1、2間に導入しておく必要のある被処理流動体を、第1導入部から供給する必要がある場合において、他方の被処理流動体の装置内への供給口となる第2導入部の開口部は、何れかの処理用面において、上記第1導入部の開口部よりも、下流側に配置する必要がある。
この流体処理装置は、混合(反応)させる2種以上の被処理流動体を別々に導入する複数の導入部と、当該2種以上の被処理流動体の少なくとも一つに圧力を付与する流体圧付与機構pと、この被処理流動体が流される密封された流体流路に設けられた第1処理用部10と第1処理用部10に対して相対的に接近離反可能な第2処理用部20の少なくとも2つの処理用部と、これらの処理用部10、20において互いに対向する位置に設けられた第1処理用面1及び第2処理用面2の少なくとも2つの処理用面1、2と、第1処理用部10と第2処理用部20とを相対的に回転させる回転駆動機構とを備え、両処理用面1、2間にて、被処理流動体間の混合(反応)処理を行うものであって、第1処理用部10と第2処理用部20のうち少なくとも第2処理用部20は、受圧面を備えるものであり、且つ、この受圧面の少なくとも一部が第2処理用面2により構成され、受圧面は、流体圧付与機構が被処理流動体に付与する圧力を受けて第1処理用面1から第2処理用面2を離反させる方向に移動させる力を発生させ、更に、第2処理用部20は、第2処理用面2と反対側を向く接近用調整面24を備えるものであり、接近用調整面24は、被処理流動体に掛けた所定の圧力を受けて第1処理用面1に第2処理用面2を接近させる方向に移動させる力を発生させ、上記接近用調整面24の接近離反方向の投影面積と、上記受圧面の接近離反方向の投影面積との面積比により、被処理流動体から受ける全圧力の合力として、第1処理用面1に対する第2処理用面2の離反方向へ移動する力が決まるものであり、接近離反可能且つ相対的に回転する第1処理用面1と第2処理用面2との間に圧力が付与された被処理流動体が通され、当該被処理流動体に混合(反応)させる他の被処理流動体が両処理用面間において混合され、混合された被処理流動体が所定厚みの薄膜流体を形成しながら両処理用面1、2間を通過することで、処理用面間の通過中に所望の生成物を得るものである。
図25においてUは上方を、Sは下方をそれぞれ示している。図26(A)、図27(B)においてRは回転方向を示している。図27(B)においてCは遠心力方向(半径方向)を示している。
第1ホルダ11には第1処理用部10と回転軸50が設けられている。第1処理用部10はメインティングリングと呼ばれる環状体であり鏡面加工された第1処理用面1を備える。回転軸50は第1ホルダ11の中心にボルトなどの固定具81にて固定されたものであり、その後端が電動機などの回転駆動装置82(回転駆動機構)と接続され、回転駆動装置82の駆動力を第1ホルダ11に伝えて当該第1ホルダ11を回転させる。第1処理用部10は上記第1ホルダ11と一体となって回転する。
上記の第1処理用面1は、第1ホルダ11から露出して、第2ホルダ21を臨む。第1処理用面の材質は、セラミックや焼結金属、対磨耗鋼、その他金属に硬化処理を施したものや、硬質材をライニングやコーティング、鍍金などを施工したものを採用する。
この第2ホルダ21が備えるリング収容部41は、第2リング20の、主として処理用面2側と反対側の部位を収容する凹部であり、平面視において、環状に形成された溝である。
リング収容部41は、第2リング20の寸法より大きく形成され、第2リング20との間に十分なクリアランスを持って、第2リング20を収容する。
少なくとも第2ホルダ21のリング収容部41には、処理用部付勢部としてスプリング43が設けられている。スプリング43は第2処理用部20を第1処理用部10に向けて付勢する。さらに他の付勢方法として、空気導入部44などの空気圧またはその他の流体圧を供給する加圧手段を用いて第2ホルダ21が保持する第2処理用部20を第1処理用部10へ近づける方向に付勢する方法でもよい。
スプリング43及び空気導入部44などの接面圧付与機構は第2処理用部20の周方向の各位置(処理用面の各位置)を均等に、第1処理用部10へ向けて付勢する。
この第2ホルダ21の中央に上記の第1導入部d1が設けられ、第1導入部d1から処理用部外周側へ圧送されてくる流体は、まず当該第2ホルダ21が保持する第2処理用部20と第1処理用部10と当該第1処理用部10を保持する第1ホルダ11とに囲まれた空間内に導かれる。そして第1処理用部10から第2処理用部20を付勢部の付勢に抗して離反させる方向に、第2処理用部20に設けられた受圧面23に流体圧付与機構Pによる上記流体の送圧(供給圧)を受ける。
なお、他の箇所においては説明を簡略にするため、受圧面23についてのみ説明をしているが、正確に言えば、図29(A)(B)に示すように、上記の受圧面23と共に、後述する溝状の凹部13の第2処理用部20に対する軸方向投影面のうちで、上記受圧面23が設けられていない部分23Xも受圧面として、流体圧付与機構Pによる上記流体の送圧(供給圧)を受ける。
処理用面に設けられた凹部13については、被処理物及び生成物を含む流体の物性に対応してその深さ、処理用面に対して水平方向への総面積、本数、及び形状を実施できる。
なお、上記受圧面23と上記凹部13とを一装置内に共に設けても実施できる。
尚、凹部13とは異なる溝については、形状、面積、本数、深さに関しては特に限定されない。目的に応じて当該溝を施す事ができる。
具体的には、第2導入部d2は、図27(A)に示すように、上記の第2処理用面2の開口部d20からの導入方向が、第2処理用面2に対して所定の仰角(θ1)で傾斜している。この仰角(θ1)は、0度を超えて90度未満に設定されており、さらに反応速度が速い反応の場合には1度以上45度以下で設置されるのが好ましい。
また、図27(B)に示すように、上記の第2処理用面2の開口部d20からの導入方向が、上記の第2処理用面2に沿う平面において、方向性を有するものである。この第2流体の導入方向は、処理用面の半径方向の成分にあっては中心から遠ざかる外方向であって、且つ、回転する処理用面間における流体の回転方向に対しての成分にあっては順方向である。言い換えると、開口部d20を通る半径方向であって外方向の線分を基準線gとして、この基準線gから回転方向Rへの所定の角度(θ2)を有するものである。
この角度(θ2)についても、0度を超えて90度未満に設定されており、図27(B)の網かけ部分に向けて開口部d20から吐出される。さらに反応速度が速い反応の場合には、当該角度(θ2)は小さいものであってもよく、反応速度が遅い場合には、当該角度(θ2)も大きく設定することが好ましい。また、この角度は、流体の種類、反応速度、粘度、処理用面の回転速度などの種々の条件に応じて、変更して実施することができる。
また上記処理用部を流体中に浸し、上記処理用面間にて混合(反応)させて得られた流体を直接処理用部の外部にある液体、もしくは空気以外の気体に投入して実施できる。
さらに処理用面間もしくは処理用面から吐出された直後の被処理物に超音波エネルギーを付加する事もできる。
この温調機構は特に限定されないが、冷却が目的の場合には処理用部10、20に冷却部を設ける。具体的には、温調用媒体としての氷水や各種の冷媒を通す配管、あるいはペルチェ素子などの、電気的もしくは化学的に冷却作用をなすことのできる冷却素子を処理用部10、20に取り付ける。
加熱が目的の場合には処理用部10、20に加熱部を設ける。具体的には、温調用媒体としてのスチームや各種の温媒を通す配管、あるいは電気ヒーターなどの、電気的もしくは化学的に発熱作用をなすことのできる発熱素子を処理用部10、20に取り付ける。
また、リング収容部に処理用部と直接接する事の出来る新たな温調用媒体用の収容部を設けても良い。それらにより、処理用部の熱伝導を用いて処理用面を温調する事ができる。また、処理用部10、20の中に冷却素子や発熱素子を埋め込んで通電させたり、冷温媒通過用通路を埋め込んでその通路に温調用媒体(冷温媒)を通す事で、内側より処理用面を温調する事もできる。なお、図25に示した温調機構J1、J2は、その一例であって、各処理用部10、20の内部に設けられた温調用媒体を通す配管(ジャケット)である。
Ra=L3・g・β・ΔT/(α・ν)
で定義される無次元数であるレイリー数Raによって支配される。ベナール対流が生じ始める臨界レイリー数は処理用面と被処理物流体との境界面の性質によって異なるが約1700とされている。それより大きな値ではベナール対流が発生する。さらに、そのレイリー数Raが1010付近より大きな値の条件となると流体は乱流状態となる。つまり、その処理用面間の温度差ΔTもしくは処理用面の距離Lを、レイリー数Raが1700以上になるようにして本装置を調節する事で、処理用面間に処理用面に対して垂直方向の流れを発生する事ができ、上記混合(反応)操作を実施できる。
Ma=σ・ΔT・L/(ρ・ν・α)
で定義される無次元数であるマランゴニ数によって支配される。マランゴニ対流が発生し始める臨界マランゴニ数は80付近であり、その値よりも大きな値となる条件ではマランゴニ対流が発生する。つまり、その処理用面間の温度差ΔTもしくは処理用面の距離Lを、マランゴニ数Ma が80以上になるようにして本装置を調節する事で、10μm以下の微小流路であっても処理用面間に処理用面に対して垂直方向の流れを発生させる事ができ、上記混合(反応)操作を実施できる。
ν:動粘性率[m2/s]、 α:温度伝導率[(m2/s)]、 ΔT:処理用面間の温度差[K]
ρ:密度[kg/m3]、 Cp:定圧比熱[J/kg・K]、 k:熱伝導率[W/m・K]
T1:処理用面における高温側の温度[K]、 T0:処理用面における低温側の温度[K]
ΔT:処理用面間の温度差[K]、 ρ:密度[kg/m3]、 Cp:定圧比熱[J/kg・K]
k:熱伝導率[W/m・K]、 σt:表面張力温度係数[N/m・K]
T1:処理用面における高温側の温度[K]、 T0:処理用面における低温側の温度[K]
図1(A)に示す、接近・離反可能に互いに対向して配設され、少なくとも一方が他方に対して回転する処理用面1、2の間にできる、薄膜流体中で均一に攪拌・混合する装置を用いて、銅フタロシアニンを溶解し、銅フタロシアニン溶液としたものを薄膜流体中で水性溶媒と合流させ、薄膜流体中で均一混合させて、銅フタロシアニンを析出させる。
粒度分布は、ナノトラック粒度分布測定装置 UPA-EX150〔日機装(株)製〕を用いて測定し、体積平均粒子径を採用した。
X線回折測定にはPANalytical社製の全自動多目的X線回折装置(X‘Pert PRO MPD)を用いた。回折角2θ=5~60°の範囲での回折強度を測定した。
透過スペクトルは島津製作所製の紫外可視分光光度計(UV-2450)を用いて380nm~780nmの透過スペクトルを測定した。本発明における、銅フタロシアニンの波長400~450nmにおける透過スペクトルの透過率が、前記400~450nmの波長全体に亘って、従来用いられていたε型銅フタロシアニンのそれよりも大きいという特性は、380~780nmにおける透過スペクトルの透過率が最大となる波長(λmax)での透過率(Tmax )に対する波長425nmにおける透過率(T425 )の比(T425 /Tmax )≧0.70であることを評価基準として確認した。
図31に破線で示すように、得られた銅フタロシアニンは、380~780nmにおける透過スペクトルの透過率が最大となる波長(λmax)は469nmであり、また、(T425 /Tmax )=0.89であった。
また、図30に示すように、その銅フタロシアニン分散液を乾燥して得られた銅フタロシアニン粉末の回折スペクトルにおいて回折強度がピークとなる回折角から、結晶型がα型である事を確認した。
BASF社製のε型銅フタロシアニンである、HELIOGEN BLUE L 6700Fを1%ドデシル硫酸ナトリウム水溶液に超音波分散機を用いて分散した。得られたε型銅フタロシアニンの分散液の透過スペクトルを図31に実線にて示す。
実施例2~5については、銅フタロシアニンの処理用面間への導入量または、処理用面の回転数、または吐出流量を変更して実施した。結果を下記表1に示す。
次に、上記とは別の実施例について説明する。
銅フタロシアニンを濃硫酸に溶解し、純水で希釈することによって銅フタロシアニン微粒子を析出させるアシッドペースティング法は粗顔料の精製方法として一般的であり、またα型の銅フタロシアニンを製造する方法として知られている。本実施例では、アシッドペースティング法を、本願出願人による、特開2004-49957号公報に記載されたものと同原理である装置(Forced thin film reactor、エム・テクニック(株)製、商品名ULREA、以下「FTFR」と略記)を用いて行った。作製した銅フタロシアニン微粒子の形状確認と粒子径測定は電子顕微鏡(透過型および走査型)および粒度分布計にて確認した。作製した銅フタロシアニン微粒子の乾燥粉体を作製し、X線回折測定にて結晶型を、赤外吸収スペクトル測定にて分子構造を、示差熱重量同時測定(TG/DTA)にて熱的挙動を確認した。また、水系分散液を作製し、紫外-可視領域における透過・吸収特性を確認した。
原料の銅フタロシアニンは、β型銅フタロシアニン(商品名:PV FAST BLUE BG、クラリアントジャパン(株)製)を用いた。銅フタロシアニンを溶解するための濃硫酸は、キシダ化学(株)製の98%濃硫酸(試薬特級)を用いた。微粒子を分散するための界面活性剤は、関東化学(株)製のドデシル硫酸ナトリウム(試薬一級、 以下「SDS」と略記)を用いた。pH調整に用いた水酸化ナトリウム水溶液は、関東化学(株)製の水酸化ナトリウム(試薬特級)を純水に溶解して作製した。
銅フタロシアニンを濃硫酸に溶解した銅フタロシアニン濃硫酸溶液を作製した。FTFRの処理用部の回転を開始し(回転数1700rpm)、中央から第1流体として純水を送液温度20℃、送液流量400ml/min.で送液しながら、第2流体として銅フタロシアニン濃硫酸溶液を送液流量3ml/min.で処理用面1、2間に直接導入した。処理用面1、2間にて銅フタロシアニン濃硫酸溶液が純水により希釈されて銅フタロシアニン微粒子が析出し、銅フタロシアニン微粒子の希硫酸水分散液として処理用面1、2間より吐出された。吐出された銅フタロシアニン微粒子の希硫酸水分散液のpHは0.81であった。この希硫酸水分散液を、3 mol/L 水酸化ナトリウム水溶液を用いてpHを7.01に調整し、25℃恒温室にて22時間静置した。
上記のように静置した分散液において、銅フタロシアニン微粒子が凝集・沈降していることを確認した。沈降した銅フタロシアニン微粒子は、真空アスピレーターを使用し、濾布(目開き10 μm)を用いて濾集し、純水で洗浄することで銅フタロシアニン微粒子ペーストを得た。
SDSを純水に溶解し、SDS水溶液を作製した。洗浄後に得られた銅フタロシアニン微粒子ペーストの一部をSDS水溶液に投入して銅フタロシアニン水分散液を作製した。銅フタロシアニン水分散液の処方は、銅フタロシアニン固形分濃度1wt%、SDS濃度0.1wt%である。作製した銅フタロシアニン水分散液を回転式乳化分散機(商品名:クレアミックス、エム・テクニック(株)製)にて分散処理した。分散処理は、1Lの 銅フタロシアニン水分散液を回転数20000rpmにて30 min行った。分散液の作製に使用しなかった銅フタロシアニン微粒子ペーストは、60℃、-0.1MPaGの条件で23時間真空乾燥して乾燥粉体を得た。
比較例2として、バッチ法にて銅フタロシアニン微粒子を作製した。この比較例で利用したバッチ法は、ビーカーとマグネティックスターラーを用いて純水を攪拌しながら、銅フタロシアニン濃硫酸溶液を滴下して銅フタロシアニン微粒子を析出させる方法である。銅フタロシアニン微粒子の洗浄および乾燥方法は、上記のFTFRを用いた実験と同条件で行った。
銅フタロシアニン微粒子分散液の粒度分布測定には、日機装(株)製の動的光散乱方式粒度分布測定装置マイクロトラックUPA-150を使用した。粒度分布の測定条件は、粒子屈折率1.51、粒子比重1.0 g/cm3、測定溶媒が純水、測定時間3 minである。分散液のスペクトル測定には、(株)島津製作所製の紫外可視分光光度計UV-2450を使用した。スペクトルの測定条件は、石英セルを使用し、サンプリングレート0.2 nm、測定速度が低速である。粒子の形状観察には、透過型電子顕微鏡HF-2000(TEM、(株)日立製作所製)と走査型電子顕微鏡S-4800(SEM、(株)日立ハイテクノロジーズ製)を使用した。粉体の結晶型の同定には、粉末X線回折測定装置X'Pert PRO MPD(スペクトリス(株) PANalytical事業部製)を使用した。測定条件は、Cu対陰極、管電圧45 kV、管電流40 mA、走査速度1.6 °/minである。示差熱重量同時測定(TG/DTA)には、TG/DTA6300(セイコーインスツル(株)製)を用いた。測定条件は、アルミナ粉末をリファレンスに用いて、昇温速度20℃/minである。赤外吸収スペクトル(FT-IR)の測定は、FT/IR-4100 type A(日本分光(株)製)を用いて測定した。測定条件は、ATR法を用い、分解能4.0 cm-1、積算回数、16回である。以上の測定による結果の評価はすべて、同じ対象物について3回行った測定結果の平均値を用いるものとした。以下、結果の評価および考察を述べる。
FTFRによって作製した銅フタロシアニン微粒子と、バッチ法にて作製した銅フタロシアニン粒子について走査型電子顕微鏡(SEM)写真(図33)と粒度分布(図34)を示す。図33(A)はFTFRのものを示し、図33(B)はバッチ法のものを示す。そして、図35には、FTFRによって作製された銅フタロシアニン微粒子の透過型電子顕微鏡(TEM)写真を示す。バッチ法で作製した粒子は、粒子径として広い分布の棒状粒子であるのに対し、FTFRを用いて作製した微粒子は粒子径10 nm程度の球状粒子であることが分かった。
図36には銅フタロシアニン微粒子のX線回折測定結果を示す。FTFRで作製した銅フタロシアニン微粒子のX線回折パターンは、バッチ法にて作製した銅フタロシアニン粒子と同様の位置に回折ピークを持つ。これよりFTFRで作製した銅フタロシアニン微粒子がα型の結晶型であることが分かった。また、FTFRで作製した銅フタロシアニン微粒子の回折ピークは、バッチ法にて作製した銅フタロシアニン粒子の回折ピークに比べてブロード化していた。これは、粒子径が小さくなることによって、ピークの半価幅が広がったことによるものと考えられる。
図37に銅フタロシアニン微粒子の指紋領域における赤外吸収スペクトルを示す(図37の(A)はFTFRによって作製した銅フタロシアニン微粒子のものであり、(B)はバッチ法にて作製した銅フタロシアニン粒子のものである)。FTFRで作製した銅フタロシアニン微粒子とバッチ法にて作製した銅フタロシアニン粒子について、共にフタロシアニン骨格の振動に起因されるピーク(約1117-1118、 1089、 1066、 941-943、 863-864、 717 cm-1)が確認された。その他のピークもこれまでの報告(B.N. Achar, K.S. Lokesh:J. Solid State Chem., 117, 1987 (2004))と一致するものであり、銅フタロシアニンの分子構造に変化が無いことが分かった。
図38に示すTG/DTAの結果によって、FTFRで作製した銅フタロシアニンとバッチ法で作製した銅フタロシアニンは、ともに510-530 ℃付近で分解が開始したことが分かる。よって、FTFRで作製した銅フタロシアニン微粒子とバッチ法で作製した銅フタロシアニン粒子には、熱分析結果に相違が無いことが分かった。
波長領域350-800 nmにおける、銅フタロシアニン粒子の0.0050%水分散液の透過スペクトルを、図39および表2に示す。バッチ法で作製したα型の銅フタロシアニンの透過スペクトル、市販品であるβ、ε型の銅フタロシアニンの透過スペクトルと比較して、FTFRで作製した銅フタロシアニン微粒子の分散液は、360-550 nmの波長領域における透過スペクトルの最大透過率の波長が短波長側にシフトし、同じα型の銅フタロシアニンの透過率よりも面積比で20-30%向上していた。特に430-480 nmの領域における透過率が向上し、さらに700 nmより長波長領域の透過率も向上していた。透過性と吸収性共に向上されていることが分かった。また、実施例6において(T425 /Tmax )=0.81であった。
波長領域300-800 nmにおける、銅フタロシアニン微粒子の0.0010%水分散液の吸収スペクトルを図40に示す。330、600、690 nm付近にそれぞれピークが観測される。スペクトルとしてはα型の形状であるが、各ピークがシャープになり、また短波長側にシフトしていた。690 nm付近のピークと600 nm付近のピークについては、それぞれ、単量体と二量体の吸収に帰属される(J. H. Sharp, M. Abkowitz:J. Phys. Chem., 77, 477 (1972)、H. Xia, M. Nogami:Opt. Mater., 15, 93 (2000))。
λ=(8mc/h)(L2/[N+1])
ここで、mは電子の質量、cは光の速度、hはプランク定数、Lはポリメチンの結合距離、Nは電子の数である。式中の2項目は、電子の密度の逆数であり、電子の密度が大きくなると極大波長は短波長側へシフトすることとなる。FTFRで作製した銅フタロシアニン微粒子分散液における吸収極大の短波長側へのシフトは、銅フタロシアニン微粒子の粒子径が小さくなることにより粒子表面の電子密度が高まっていたためと考えられる。
次に、上記とは更に別の実施例について説明する。これら実施例7~10で用いた実験装置は上記実施例6と同じである。
原料の銅フタロシアニンは、上記実施例6と同じβ型銅フタロシアニン(商品名:PV FAST BLUE BG、クラリアントジャパン(株)製)を用いた。銅フタロシアニンを溶解するための濃硫酸および発煙硫酸は、98%濃硫酸(試薬特級、キシダ化学(株)製)および発煙硫酸(試薬特級、SO3濃度30%、ヨツハタ化学工業(株)製)を用いた。SO3濃度5%の発煙硫酸は98%濃硫酸およびSO3濃度30%の発煙硫酸を窒素雰囲気下で混合することで調製した。銅フタロシアニン微粒子の水分散液を作製するための界面活性剤は、ドデシル硫酸ナトリウム(試薬一級、関東化学(株)製、以下、上記実施例6と同様に「SDS」と略記)を用いた。銅フタロシアニン微粒子の有機溶剤分散液を作製するための有機溶剤には、プロピレングリコールモノメチルエーテルアセテート(試薬特級、関東化学(株)製、以下「PGMEA」と略記)およびプロピレングルコールモノメチルエーテル(試薬特級、関東化学(株)製、以下「PGME」と略記)を用いた。有機溶剤分散液を作製するための界面活性剤としては、Disperbyk-2000(変性アクリル系共重合物、アミン価4mg KOH/g、有効成分40%、ビックケミー・ジャパン(株)製)を用いた。pH調整に用いた水酸化ナトリウム水溶液は、水酸化ナトリウム(試薬特級、関東化学(株)製)を純水に溶解して調製した。
実験条件を表3に示す。なお、表3及び図41中では、実施例7を「Ex.1」と表記し、実施例8を「Ex.2」と表記し、実施例9を「Ex.3」と表記し、実施例10を「Ex.4」と表記している。
上記のように静置した銅フタロシアニン微粒子水分散液において銅フタロシアニン微粒子が凝集・沈降していることを確認した。沈降した銅フタロシアニン微粒子は真空アスピレーターを使用し、濾布(目開き 10 μm)を用いて濾集し、純水にて数回洗浄した後、銅フタロシアニン微粒子ペーストを得た。銅フタロシアニン微粒子ペーストを、60℃、-0.1MPaGの条件で23時間真空乾燥して乾燥粉体を得た。
SDSを純水に溶解し、0.2wt%SDS水溶液を調製した。前記の銅フタロシアニン微粒子ペーストに純水および0.2wt%SDS水溶液を加え、銅フタロシアニン微粒子水分散液を調製した。(処方条件:銅フタロシアニン微粒子固形分濃度2wt%、SDS濃度0.1wt%)調製した銅フタロシアニン微粒子水分散液1Lを回転式乳化分散機(商品名:クレアミックス、エム・テクニック(株)製)を用い、ローター回転数20000 rpmにて分散処理した。
銅フタロシアニン微粒子粉体の赤外吸収スペクトル(IR)は、日本分光(株)製のFT/IR-4100 type A(測定条件:ATR法、分解能4.0 cm-1、積算回数16回)を用いて測定した。
図41に銅フタロシアニン微粒子の指紋領域における赤外吸収スペクトルを示す。全ての実験条件において、上記実施例6(図37(A)参照)と同様、フタロシアニン骨格の振動に起因されるピーク(約1117-1118、1089-1090、1065-1066、943、864-865、717-719 cm-1)が確認された。さらに実施例10(Ex.4)のスペクトルには、1388cm-1付近に肩のピーク(図中、*を施したピーク)が確認され、第2流体に発煙硫酸を用いて調製した銅フタロシアニン微粒子にスルホ基が存在し、表面処理がなされたことを確認した。
図42に実施例7(Ex.1)の水分散液および実施例10(Ex.4)の有機溶剤分散液について波長領域350-800 nmにおける、0.005wt%-銅フタロシアニン粒子分散液の透過スペクトルを示す。黒色の線が実施例7の透過スペクトルを示し、灰色の線が実施例10の透過スペクトルを示す。実施例7及び実施例10にあっても、上記実施例6(図39参照)と同様の透過スペクトルを示していることが分かる。
2 第2処理用面
10 第1処理用部
11 第1ホルダ
20 第2処理用部
21 第2ホルダ
Claims (8)
- 結晶型がα型であり、
且つ、380~780nmにおける透過スペクトルの透過率が最大となる波長(λmax)が478nm未満である銅フタロシアニンを含有してなる銅フタロシアニン顔料。 - 結晶型がα型であり、
且つ、380~780nmにおける透過スペクトルの透過率が最大となる波長(λmax)が478nm未満であり、
且つ、波長400~450nmにおける透過スペクトルの透過率が、前記400~450nmの波長全体に亘って、結晶型がε型である銅フタロシアニンよりも大きい銅フタロシアニンを含有してなる銅フタロシアニン顔料。 - 接近・離反可能、且つ相対的に変位する処理用面の間に被処理流動体を供給し、
当該流動体の供給圧と回転する処理用面の間にかかる圧力とを含む接近方向への力と離反方向への力との圧のバランスによって処理用面間の距離を微小間隔に維持し、
この微小間隔に維持された2つの処理用面間を被処理流動体の流路とすることによって、被処理流動体が薄膜流体を形成し、
この薄膜流体中において微粒子として生成されたことを特徴とする、請求項1または2に記載の銅フタロシアニンを含有してなる銅フタロシアニン顔料。 - 銅フタロシアニン微粒子の形状が略球状であることを特徴とする、請求項1~3のいずれかに記載の銅フタロシアニンを含有してなる銅フタロシアニン顔料。
- 銅フタロシアニン微粒子の体積平均粒径が1~600nmであることを特徴とする、請求項4に記載の銅フタロシアニンを含有してなる銅フタロシアニン顔料。
- 接近・離反可能、且つ相対的に変位する処理用面の間に被処理流動体を供給し、
当該流動体の供給圧と回転する処理用面の間にかかる圧力とを含む接近方向への力と離反方向への力との圧のバランスによって処理用面間の距離を微小間隔に維持し、
この微小間隔に維持された2つの処理用面間を被処理流動体の流路とすることによって、被処理流動体が薄膜流体を形成し、
この薄膜流体中において微粒子の析出を行うことを特徴とする銅フタロシアニン微粒子の製造方法。 - 被処理流動体に圧力を付与する流体圧付与機構と、
第1処理用部、及び、この第1処理用部に対して相対的に接近・離反可能な第2処理用部の、少なくとも2つの処理用部と、
上記の第1処理用部と第2処理用部とを相対的に回転させる回転駆動機構とを備え、
上記の各処理用部において互いに対向する位置に、第1処理用面及び第2処理用面の少なくとも2つの処理用面が設けられており、
上記の各処理用面は、上記圧力の被処理流動体が流される、密封された流路の一部を構成するものであり、
上記第1処理用部と第2処理用部のうち、少なくとも第2処理用部は受圧面を備えるものであり、且つ、この受圧面の少なくとも一部が上記の第2処理用面により構成され、
この受圧面は、上記の流体圧付与機構が被処理流動体に付与する圧力を受けて第1処理用面から第2処理用面を離反させる方向に移動させる力を発生させ、
接近・離反可能、且つ相対的に回転する第1処理用面と第2処理用面との間に上記圧力の被処理流動体が通されることにより、上記被処理流動体が上記薄膜流体を形成し、
この薄膜流体中において微粒子の析出を行うことを特徴とする、請求項6に記載の銅フタロシアニン微粒子の製造方法。 - 上記の流体圧付与機構から圧力を付与された一種の被処理流動体が上記第1処理用面と第2処理用面との間に通され、
上記の一種の被処理流動体とは異なる他の一種の被処理流動体が通される独立した別途の導入路を備え、この導入路に通じる少なくとも一つの開口部が上記第1処理用面と第2処理用面の少なくとも何れか一方に設けられ、
この導入路から上記の他の一種の被処理流動体を、上記両処理用面間に導入し、
上記一種の被処理流動体と他の一種の被処理流動体とを、上記薄膜流体中で混合することを特徴とする、請求項7に記載の銅フタロシアニン微粒子の製造方法。
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JP2009049962A JP2009242785A (ja) | 2008-03-11 | 2009-03-03 | 顔料微粒子の表面処理方法 |
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WO2011152095A1 (ja) * | 2010-06-03 | 2011-12-08 | エム・テクニック株式会社 | 新規な銅フタロシアニン顔料及び銅フタロシアニン微粒子の製造方法 |
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WO2012070594A1 (ja) * | 2010-11-24 | 2012-05-31 | エム・テクニック株式会社 | 高耐熱性フタロシアニン |
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Also Published As
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JP4461304B1 (ja) | 2010-05-12 |
CN102165020A (zh) | 2011-08-24 |
JPWO2010035861A1 (ja) | 2012-02-23 |
EP2351796A8 (en) | 2011-09-21 |
EP2351796B1 (en) | 2014-10-22 |
KR20110079607A (ko) | 2011-07-07 |
KR101402731B1 (ko) | 2014-06-02 |
CN102165020B (zh) | 2014-10-15 |
US20110177337A1 (en) | 2011-07-21 |
EP2351796A1 (en) | 2011-08-03 |
EP2351796A4 (en) | 2012-05-30 |
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