WO2012164999A1 - 強制薄膜式流体処理装置を用いた微粒子の生産量増加方法 - Google Patents
強制薄膜式流体処理装置を用いた微粒子の生産量増加方法 Download PDFInfo
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- WO2012164999A1 WO2012164999A1 PCT/JP2012/056734 JP2012056734W WO2012164999A1 WO 2012164999 A1 WO2012164999 A1 WO 2012164999A1 JP 2012056734 W JP2012056734 W JP 2012056734W WO 2012164999 A1 WO2012164999 A1 WO 2012164999A1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1887—Stationary reactors having moving elements inside forming a thin film
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/53—Mixing liquids with solids using driven stirrers
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/02—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed system contains two hetero rings
- C07D471/04—Ortho-condensed systems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Definitions
- the present invention relates to a method for increasing the production amount of fine particles.
- Fine particles are required in the industrial field as a whole, and it is necessary to make fine particles according to the intended use, from micrometer-size fine particles to nanometer-size fine particles.
- nano particles nano-sized fine particles
- nano-sized fine particles that are fine particles having a particle size of less than 1 ⁇ m exhibit new properties different from those of particles, and therefore, development of a new production method for industrial production of nanoparticles. Is needed.
- micrometer-sized fine particles there are problems with reproducibility and energy costs in the conventional production methods, and therefore, a fine particle production method that can easily control the particle diameter from micrometer to nanometer.
- the demand is growing. At the same time, the demand for the production amount of fine particles is increasing, and a production method of fine particles with a high production amount is demanded in the same manner as particle size control.
- Patent Document 2 a method for producing nanoparticles using the principle of the apparatus shown in Patent Document 1 and using stirring and instantaneous uniform mixing of a plurality of types of fluids under a microchannel.
- Patent Document 2 This device uses the principle of mechanical seal, forms a forced thin film fluid of the fluid to be processed between the relatively displaceable processing surfaces that can be approached and separated, and is processed between the rotating processing surfaces.
- the fluid is supplied, and the distance between the processing surfaces is made minute by the pressure balance between the supply pressure of the fluid and the pressure applied between the rotating processing surfaces.
- the method before the method in the above principle is a method of mechanically adjusting the distance between the processing surfaces, which cannot absorb the heat generated by the rotation and the deformation caused by the rotation, or the runout, etc. It is practically impossible to make the distance between the processing surfaces at least 10 ⁇ m or less. That is, it is possible to realize the production of nanoparticles by an instantaneous chemical / physicochemical reaction or the like in a microchannel using the principle of the apparatus of Patent Document 1 above. As a result of research, it has surprisingly made it possible to instantaneously stir, mix, react and deposit in a microchannel of 0.1 to 10 ⁇ m, as well as below 1 mm.
- the method for producing fine particles proposed in Patent Documents 2 and 3 is an extremely effective method for producing fine particles in that the fine particles can be produced at low cost and low energy, but the second fluid is used to increase the throughput.
- the case where the particle diameter of the resulting fine particles is changed by increasing the concentration or introduction speed of the fine particle raw material contained in the (fluid introduced from the introduction path having an opening on the processing surface) is specifically disclosed.
- a method for further increasing the production amount has been appealed in the implementation of this production method.
- an object of the present invention is to provide a new method for increasing the production amount of fine particles.
- At least two kinds of fluids are used as the fluid to be treated.
- at least one kind of fluid is a raw material fluid containing at least one kind of fine particle raw material.
- the type of fluid is a fluid for treating the fine particle raw material, and the two or more kinds of fluids to be treated are disposed so as to face each other.
- the raw material fluid is disposed so as to be opposed to and can be separated from each other.
- a method for increasing the production of fine particles wherein at least one is introduced from the center of at least two processing surfaces that rotate relative to the other.
- this invention can be implemented as said treatment being at least any one selected from precipitation, emulsification, dispersion, reaction, and aggregation.
- the present invention includes an additional introduction path that is independent of a flow path through which the raw material fluid passes between the processing surfaces while forming the thin film fluid and through which the raw material fluid flows.
- At least one of the processing surfaces includes at least one opening that leads to the separate introduction path, the at least one other type of fluid is introduced between the processing surface through the opening, and The raw material fluid and the at least one other fluid can be mixed in the thin film fluid.
- at least one of the processing surfaces has an annular shape, and the raw material fluid is introduced between the processing surfaces from the center of the annular shape.
- the total opening area (a) of the gap between the two processing surfaces at the point closest to the center of the ring where the fluids of the two fluids merge is 5 of the total opening area (b) of the opening leading to the separate introduction path. It can be implemented as being less than double. Further, at least one of the processing surfaces has an annular shape, and the raw material fluid is introduced between the processing surfaces from the center of the annular shape, and the separate introduction path leading to the processing surface is provided.
- the total opening area of the gap between the processing surfaces (a) at a point closest to the center of the ring where at least two openings are provided and the raw material fluid and the at least one other kind of fluid meet. ) Is not more than five times the opening area of each opening that leads to the separate introduction path.
- the shape of the opening part of the said separate introduction path leading to the said process surface being a ring shape.
- at least one of the processing surfaces has an annular shape, and the raw material fluid is introduced between the processing surfaces from the annular center, and is introduced between the processing surfaces from the annular center.
- the flow rate of the raw material fluid per unit time is 0.1 to 20000 times the flow rate of the at least one other fluid per unit time from the opening.
- the present invention provides a fluid pressure applying mechanism for applying pressure to a fluid to be processed, a first processing portion having a first processing surface among the two processing surfaces, and the two processing surfaces.
- a second processing unit having a second processing surface, a rotation driving mechanism for relatively rotating these processing units, and the first processing unit and the second processing unit.
- at least the second processing portion has a pressure receiving surface, and at least a part of the pressure receiving surface is constituted by the second processing surface, and the pressure receiving surface is covered by the fluid pressure applying mechanism. It is appropriate to use a device that receives a pressure applied to the treatment fluid and generates a force that moves the second treatment surface away from the first treatment surface.
- the inventor introduces a fluid to be processed between at least two processing surfaces disposed opposite to each other and capable of approaching / separating at least one rotating relative to the other.
- the processing surface is more annular than the second introduction part d2 leading to the opening laid on the processing surface. It has been found that it is possible to increase the flow rate of the fluid to be processed or the flow rate per unit time that can be sent between the processing surfaces from the first introduction part d1 at the center (upstream side) of the surface.
- the present invention has been completed by knowing that among the fluids to be treated introduced between the processing surfaces, the amount of the fine particles can be increased by introducing the raw material fluid between the processing surfaces from the center of the processing surface. This is a fine particle We were able to provide a new way to increase production.
- FIG. 1 is a schematic cross-sectional view of a fluid processing apparatus according to an embodiment of the present invention.
- A is a schematic plan view of a first processing surface of the fluid processing apparatus shown in FIG. 1, and
- B) is an enlarged view of a main part of the processing surface of the apparatus.
- A) is sectional drawing of the 2nd introducing
- B) is the principal part enlarged view of the processing surface for demonstrating the 2nd introducing
- 2 is a TEM photograph of titanium oxide nanoparticles produced in Example 11.
- the fluid processing apparatus shown in FIGS. 1 to 3 is the same as the apparatus described in Patent Documents 2 and 3, and the processing surface in the processing section in which at least one of which can be approached and separated rotates relative to the other.
- the first fluid which is the first fluid to be treated, of the fluids to be treated is introduced between the processing surfaces, and the first fluid is introduced into the flow.
- a second fluid which is a second fluid to be treated, is introduced between the processing surfaces from another flow path having an opening that communicates between the processing surfaces independently of the path.
- U indicates the upper side
- S indicates the lower side.
- the upper, lower, front, rear, left and right only indicate a relative positional relationship, and do not specify an absolute position.
- R indicates the direction of rotation.
- C indicates the centrifugal force direction (radial direction).
- This apparatus uses at least two kinds of fluids as a fluid to be treated, and at least one kind of fluid includes at least one kind of an object to be treated and is opposed to each other so as to be able to approach and separate.
- a processing surface at least one of which rotates with respect to the other, and the above-mentioned fluids are merged between these processing surfaces to form a thin film fluid.
- An apparatus for processing an object to be processed As described above, this apparatus can process a plurality of fluids to be processed, but can also process a single fluid to be processed.
- This fluid processing apparatus includes first and second processing units 10 and 20 that face each other, and at least one of the processing units rotates.
- the opposing surfaces of both processing parts 10 and 20 are 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 the 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.
- the interval between the processing surfaces 1 and 2 can be changed as appropriate, but is usually adjusted to a minute interval of 1 ⁇ m to 1 mm, particularly 1 ⁇ m to 10 ⁇ m.
- the fluid to be processed that passes between the processing surfaces 1 and 2 becomes a forced thin film fluid forced by the processing surfaces 1 and 2.
- the apparatus When processing a plurality of fluids to be processed using this apparatus, the apparatus is connected to the flow path of the first fluid to be processed and forms a part of the flow path of the first fluid to be processed. At the same time, a part of the flow path of the second fluid to be treated is formed separately from the first fluid to be treated. And this apparatus performs processing of fluid, such as making both flow paths merge and mixing both the to-be-processed fluids between the processing surfaces 1 and 2, and making it react.
- “treatment” is not limited to a form in which the object to be treated reacts, but also includes a form in which only mixing and dispersion are performed without any reaction.
- the first holder 11 that holds the first processing portion 10 the second holder 21 that holds the second processing portion 20, a contact pressure applying mechanism, a rotation drive mechanism, A first introduction part d1, a second introduction part d2, and a fluid pressure imparting mechanism p are provided.
- the first processing portion 10 is an annular body, more specifically, a ring-shaped disk.
- the second processing unit 20 is also a ring-shaped disk.
- the materials of the first and second processing parts 10 and 20 are metal, carbon, ceramic, sintered metal, wear-resistant steel, sapphire, and other metals that have undergone hardening treatment, Those with coating, plating, etc. can be used.
- at least a part of the first and second processing surfaces 1 and 2 facing each other is mirror-polished in the processing units 10 and 20.
- the surface roughness of this mirror polishing is not particularly limited, but is preferably Ra 0.01 to 1.0 ⁇ m, more preferably Ra 0.03 to 0.3 ⁇ m.
- At least one of the holders can be rotated relative to the other holder by a rotational drive mechanism (not shown) such as an electric motor.
- Reference numeral 50 in FIG. 1 denotes a rotation shaft of the rotation drive mechanism.
- the first holder 11 attached to the rotation shaft 50 rotates and is used for the first processing supported by the first holder 11.
- the unit 10 rotates with respect to the second processing unit 20.
- the second processing unit 20 may be rotated, or both may be rotated.
- the first and second holders 11 and 21 are fixed, and the first and second processing parts 10 and 20 are rotated with respect to the first and second holders 11 and 21. May be.
- 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, and the second processing unit 20 is disposed in the storage unit 41 provided in the second holder 21. It is housed in a hauntable manner.
- the first processing unit 10 may approach or separate from the second processing unit 20, and both the processing units 10 and 20 may approach or separate from each other. It may be a thing.
- the accommodating portion 41 is a concave portion that mainly accommodates a portion of the second processing portion 20 on the side opposite to the processing surface 2 side, and is a groove that has a circular shape, that is, is formed in an annular shape in plan view. .
- the accommodating portion 41 accommodates the second processing portion 20 with a sufficient clearance that allows the second processing portion 20 to rotate.
- the second processing unit 20 may be arranged so that only the parallel movement in the axial direction is possible, but by increasing the clearance, the second processing unit 20
- the center line of the processing part 20 may be inclined and displaced so as to break the relationship parallel to the axial direction of the storage part 41. Further, the center line of the second processing part 20 and the storage part 41 may be displaced. The center line may be displaced so as to deviate in the radial direction. As described above, it is desirable to hold the second processing unit 20 by the floating mechanism that holds the three-dimensionally displaceably.
- the above-described fluid to be treated is subjected to both treatment surfaces from the first introduction part d1 and the second introduction part d2 in a state where pressure is applied by a fluid pressure application mechanism p configured by various pumps, potential energy, and the like. It is introduced between 1 and 2.
- the first introduction part d1 is a passage provided in the center of the annular second holder 21, and one end of the first introduction part d1 is formed on both processing surfaces from the inside of the annular processing parts 10 and 20. It is introduced between 1 and 2.
- the second introduction part d2 supplies the second processing fluid to be reacted with the first processing fluid to the processing surfaces 1 and 2.
- the second introduction part d ⁇ b> 2 is a passage provided inside the second processing part 20, and one end thereof opens at the second processing surface 2.
- the first fluid to be processed that has been pressurized by the fluid pressure imparting mechanism p is introduced from the first introduction part d1 into the space inside the processing parts 10 and 20, and the first processing surface 1 and the second processing surface 2 are supplied. It passes between the processing surfaces 2 and tries to pass outside the processing portions 10 and 20. Between these processing surfaces 1 and 2, the second fluid to be treated pressurized by the fluid pressure applying mechanism p is supplied from the second introduction part d 2, merged with the first fluid to be treated, and mixed.
- the above-mentioned contact surface pressure applying mechanism applies a force that acts in a direction in which the first processing surface 1 and the second processing surface 2 approach each other to the processing portion.
- the contact pressure applying mechanism is provided in the second holder 21 and biases the second processing portion 20 toward the first processing portion 10.
- the contact surface pressure applying mechanism is a force that pushes the first processing surface 1 of the first processing portion 10 and the second processing surface 2 of the second processing portion 20 in the approaching direction (hereinafter referred to as a contact surface).
- This is a mechanism for generating pressure.
- a thin film fluid having a minute film thickness in the unit of nm to ⁇ m is generated by the balance between the contact surface pressure and the force separating the processing surfaces 1 and 2 such as fluid pressure. 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 is arranged between the accommodating portion 41 and the second processing portion 20.
- a spring 43 that biases the second processing portion 20 in a direction approaching the first processing portion 10 and a biasing fluid introduction portion 44 that introduces a biasing fluid such as air or oil.
- the contact surface pressure is applied by the spring 43 and the fluid pressure of the biasing fluid. Any one of the spring 43 and the fluid pressure of the urging fluid may be applied, and other force such as magnetic force or gravity may be used.
- the second processing unit 20 causes the first treatment by the separation force generated by the pressure or viscosity of the fluid to be treated which is pressurized by the fluid pressure imparting mechanism p against the bias of the contact surface pressure imparting mechanism.
- the first processing surface 1 and the second processing surface 2 are set with an accuracy of ⁇ m by the balance between the contact surface pressure and the separation force, and a minute amount between the processing surfaces 1 and 2 is set. An interval is set.
- the separation force the fluid pressure and viscosity of the fluid to be processed, the centrifugal force due to the rotation of the processing portion, the negative pressure when the urging fluid introduction portion 44 is negatively applied, and the spring 43 are pulled.
- the force of the spring when it is used as a spring can be mentioned.
- This contact surface pressure imparting mechanism may be provided not in the second processing unit 20 but in the first processing unit 10 or in both.
- the second processing unit 20 has the second processing surface 2 and the inside of the second processing surface 2 (that is, the first processing surface 1 and the second processing surface 2).
- a separation adjusting surface 23 is provided adjacent to the second processing surface 2 and located on the entrance side of the fluid to be processed between the processing surface 2 and the processing surface 2.
- the separation adjusting surface 23 is implemented as an inclined surface, but may be a horizontal surface.
- the pressure of the fluid to be processed acts on the separation adjusting surface 23 to generate a force in a direction in which the second processing unit 20 is separated from the first processing unit 10. Accordingly, the pressure receiving surfaces for generating the separation force are the second processing surface 2 and the separation adjusting surface 23.
- the proximity adjustment surface 24 is formed on the second processing portion 20.
- the proximity adjustment surface 24 is a surface opposite to the separation adjustment surface 23 in the axial direction (upper surface in FIG. 1), and the pressure of the fluid to be processed acts on the second processing portion 20. A force is generated in a direction that causes the first processing unit 10 to approach the first processing unit 10.
- the pressure of the fluid to be processed that acts on the second processing surface 2 and the separation adjusting surface 23, that is, the fluid pressure, is understood as a force constituting an opening force in the mechanical seal.
- the projected area A1 of the proximity adjustment surface 24 projected on a virtual plane orthogonal to the approaching / separating direction of the processing surfaces 1 and 2, that is, the protruding and protruding direction (axial direction in FIG. 1) of the second processing unit 20 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 of the second processing unit 20 projected onto the virtual plane is called a balance ratio K. This is important for the adjustment of the opening force.
- the opening force can be adjusted by the pressure of the fluid to be processed, that is, the fluid pressure, by changing the balance line, that is, the area A1 of the adjustment surface 24 for proximity.
- 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 proximity adjustment surface 24 may be implemented with a larger area than the separation adjustment surface 23.
- the fluid to be processed becomes a thin film fluid forced by the two processing surfaces 1 and 2 holding the minute gaps, and tends to move to the outside of the annular processing surfaces 1 and 2.
- the mixed fluid to be processed does not move linearly from the inside to the outside of the two processing surfaces 1 and 2, but instead has an annular radius.
- a combined vector of the movement vector in the direction and the movement vector in the circumferential direction acts on the fluid to be processed and moves in a substantially spiral shape from the inside to the outside.
- the rotating shaft 50 is not limited to what was arrange
- At least one of the first and second processing parts 10 and 20 may be cooled or heated to adjust the temperature.
- the first and second processing parts 10 and 20 are adjusted.
- 20 are provided with temperature control mechanisms (temperature control mechanisms) J1, J2.
- the temperature of the introduced fluid to be treated may be adjusted by cooling or heating. These temperatures can also be used for the deposition of the treated material, and also to generate Benard convection or Marangoni convection in the fluid to be treated between the first and second processing surfaces 1 and 2. May be set.
- a groove-like recess 13 extending from the center side of the first processing portion 10 to the outside, that is, in the radial direction is formed on the first processing surface 1 of the first processing portion 10. May be implemented.
- the planar shape of the recess 13 is curved or spirally extending on the first processing surface 1, or is not shown, but extends straight outward, L It may be bent or curved into a letter shape or the like, continuous, intermittent, or branched.
- the recess 13 can be implemented as one formed on the second processing surface 2, and can also be implemented as one formed on both the first and second processing surfaces 1, 2.
- the base end of the recess 13 reaches the inner periphery of the first processing unit 10.
- the tip of the recess 13 extends toward the outer peripheral surface of the first processing surface 1, and the depth (cross-sectional area) gradually decreases from the base end toward the tip.
- a flat surface 16 without the recess 13 is provided between the tip of the recess 13 and the outer peripheral surface of the first processing surface 1.
- the opening d20 of the second introduction part d2 is provided in the second processing surface 2, it is preferably provided at a position facing the flat surface 16 of the facing first processing surface 1.
- the opening d20 is desirably provided on the downstream side (outside in this example) from the concave portion 13 of the first processing surface 1.
- it is installed at a position facing the flat surface 16 on the outer diameter side from the point where the flow direction when introduced by the micropump effect is converted into a laminar flow direction in a spiral shape formed between the processing surfaces. It is desirable to do.
- the distance n in the radial direction from the outermost position of the recess 13 provided in the first processing surface 1 is preferably about 0.5 mm or more.
- the shape of the opening d20 may be circular as shown by a solid line in FIG. 2B or FIG. 3B, and the center of the processing surface 2 as shown by a dotted line in FIG. It may be a concentric ring shape surrounding the opening.
- the second fluid can be introduced under the same conditions in the circumferential direction when introduced between the processing surfaces 1 and 2. it can.
- the annular opening d20 may not be provided concentrically with the central opening of the processing surface 2. Further, the annular opening d20 may be continuous or discontinuous.
- the second introduction part d2 can have directionality.
- the introduction direction from the opening d20 of the second processing surface 2 is inclined with respect to the second processing surface 2 at a predetermined 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 d ⁇ b> 20 of the second processing surface 2 has directionality in the 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 preferably set to more than 0 degree and less than 90 degrees.
- This angle ( ⁇ 2) can be changed and implemented in accordance with various conditions such as the type of fluid, reaction speed, viscosity, and rotational speed of the processing surface.
- the second introduction part d2 may not have any directionality.
- the number of fluids to be processed and the number of flow paths are two, but may be one, or may be three or more.
- the second fluid is introduced between the processing surfaces 1 and 2 from the second introduction part d2, but this introduction part may be provided in the first processing part 10 or provided in both. Good.
- the shape, size, and number of the opening for introduction provided in each processing portion are not particularly limited, and can be appropriately changed. Further, an introduction opening may be provided immediately before or between the first and second processing surfaces 1 and 2 and further upstream.
- the second fluid is introduced from the first introduction part d1 and the first fluid is introduced from the second introduction part d2, contrary to the above. May be introduced.
- the expressions “first” and “second” in each fluid have only an implication for identification that they are the nth of a plurality of fluids, and a third or higher fluid may exist.
- the third introduction part d3 can be provided in the processing apparatus.
- the first fluid it is possible to introduce the second fluid and the third fluid separately into the processing apparatus. If it does so, the density
- the combination of fluids to be processed (first fluid to third fluid) to be introduced into each introduction portion can be arbitrarily set.
- the temperature of the fluid to be treated such as the first and second fluids is controlled, or the temperature difference between the first fluid and the second fluid (ie, the temperature difference between the fluids to be treated to be supplied) is determined. It can also be controlled.
- the temperature of each processed fluid (processing device, more specifically, the temperature immediately before being introduced between the processing surfaces 1 and 2) is measured. It is also possible to add a mechanism for heating or cooling each fluid to be processed introduced between the processing surfaces 1 and 2.
- the present invention can be carried out by introducing a raw material fluid that is a fluid containing at least one kind of fine particle raw material described later from the first introduction part d1.
- the fluid fed from the first introduction part d1 which is the center (most upstream side) of the processing surface rather than the second introduction path d2 leading to the opening laid on the processing surface, is provided. Since the flow rate that is the flow rate or the flow rate per unit time can be increased, it is also possible to increase the flow rate or flow rate of the raw material fluid that substantially passes between the processing surfaces.
- the first and second processing surfaces 1 and 2 both have an annular shape having an opening in the center, but one of the processing surfaces 1 and 2 has an opening in the center. It can also be carried out without providing an opening in the center on the other side.
- the total opening area (a) of the gap between the first and second processing surfaces 1 and 2 in the central first introduction part d1 is not more than 5 times the total opening area (b) of the opening d20. Is desirable.
- the total opening area (a) is the total between the processing surfaces at a point f (hereinafter referred to as the nearest point f) closest to the center of the ring where the first fluid and the second fluid merge. It means an opening area (see FIG. 3A).
- the distance between the first and second processing surfaces 1 and 2 is a circle having a radius ⁇ from the center of the first and second processing surfaces 1 and 2 to the nearest point f.
- the product of ⁇ is the total opening area (a).
- the closest point f means the innermost side (a point close to the center in the radial direction) in the opening d20, and in the case where two or more openings d20 are provided, it is the innermost position. As shown in FIG.
- the total opening area (a) at the closest point f is not more than five times the opening area of each opening d20a and d20b. It is desirable.
- the total opening area (a) at the nearest point f is preferably 5 times or less of the total opening area (b) of the opening d20, more preferably 3 times or less, and even more preferably 2 times or less. Furthermore, although it does not specifically limit as a minimum, It is desirable that it is 0.001 times or more, and more realistically 0.01 times or more.
- the flow rate of the raw material fluid per unit time from the central first introduction part d1 is 0.1 to 20000 times the flow rate of at least one other kind of fluid per unit time from the second introduction part d2. It is desirable that If it is less than 0.1 times, the flow rate of introduction from the center cannot be increased so much and the effect becomes small. Even if it exceeds 20000 times, there is no particular problem, but there is a possibility that the total flow rate of the second introduction part d2 becomes extremely small or the overall balance is lost.
- processes such as precipitation / precipitation / emulsification or crystallization are arranged so as to be able to approach and separate from each other, and at least one of them rotates with respect to the other. Occurs with forced uniform mixing between surfaces 1 and 2.
- the particle size and monodispersity of the resulting fine particles can be controlled 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 solvent type, and the like. it can.
- the at least 1 sort (s) of fine particle raw material contained in a raw material fluid is not specifically limited. Any material that is intended to be obtained as fine particles can be a raw material for the fine particles that are the target object. Examples include inorganic substances, organic substances, and organic / inorganic composite substances, such as metals and non-metals, or organic and / or inorganic compounds of metals and non-metals, pigments and biological ingestions (used in pharmaceuticals, etc. Compounds, substances intended to be ingested by living bodies), resins, oil components, etc., and all substances intended to be treated between the treatment surfaces can be mentioned.
- the fine particle raw material can be used as it is by introducing it as a raw material fluid between the processing surfaces from the first introduction part d1, or treating it as a raw material fluid mixed / dissolved in various solvents such as water and organic solvents. Even if it introduces between the use surfaces 1 and 2, it can implement.
- at least one type of fluid other than the raw material fluid that is, a fluid for treating the fine particle raw material is not particularly limited, and can be appropriately selected depending on the target fine particles.
- the treatment is not particularly limited, and examples thereof include precipitation, emulsification, dispersion, reaction, and aggregation.
- the raw material fluid and the fluid for precipitating and / or emulsifying the fine particle raw material contained in the raw material fluid are arranged to face each other.
- a precipitated and / or emulsified fine particle material is obtained as fine particles.
- the raw material fluid and the fluid for reducing the fine particle raw material contained in the raw material fluid are arranged to face each other and can be approached and separated, By mixing in a thin film fluid formed between at least two processing surfaces rotating at least one relative to the other, the reduced fine particle material can be obtained as fine particles.
- the fine particle raw material and the obtained fine particles may be the same substance or different substances before and after the treatment.
- a dispersant such as a surfactant may be included.
- the dispersant may be contained in a third fluid different from a fluid containing the raw material fluid and a fluid containing at least one other type of fluid other than the raw material fluid.
- the method for increasing the production amount of fine particles according to the present invention can be used for the production of the following fine particles.
- the present invention is not limited to the following examples, and can be used for the production of fine particles that have been made by conventional batch methods, continuous methods, or microreactors or micromixers.
- a reaction in which at least one pigment is dissolved in a strong acid such as sulfuric acid, nitric acid, hydrochloric acid, and the like, and an acidic pigment solution is mixed with a solution containing water to obtain pigment particles.
- a pigment solution prepared by dissolving at least one pigment in an organic solvent is a poor solvent for the pigment, and is a poor solvent compatible with the organic solvent used for the preparation of the solution
- a reaction in which the pigment particles are precipitated by being put into the inside.
- the pigment solution in which at least one kind of pigment is dissolved in either an acidic or alkaline pH adjusting solution or a mixed solution of the pH adjusting solution and an organic solvent, and the pigment contained in the pigment solution have solubility. Reaction to obtain pigment particles by mixing with a pigment deposition solution that changes the pH of the pigment solution that is not shown or has a lower solubility in the pigment than the solvent contained in the pigment solution.
- Reaction in which metal fine particles are supported on the surface of carbon or carbon black by liquid phase reduction method (as the metal, platinum, palladium, gold, silver, rhodium, iridium, ruthenium, osmium, cobalt, manganese, nickel, iron, chromium, Examples thereof include at least one metal selected from the group consisting of molybdenum and titanium).
- Reaction of producing a crystal composed of fullerene molecules and fullerene nanowhiskers / nanofiber nanotubes by mixing a solution containing a first solvent dissolving fullerene and a second solvent having a solubility of fullerene smaller than that of the first solvent. .
- the metal may be a noble metal such as gold, silver, ruthenium, rhodium, palladium, osmium, iridium, platinum, copper, or an alloy of the two or more metals).
- the ceramic raw materials include Al, Ba, Mg, Ca, La, Fe, Si, Ti, Zr, Pb, Sn, Zn, Cd, As, Ga, Sr, Bi, Ta, Examples include at least one selected from Se, Te, Hf, Ni, Mn, Co, S, Ge, Li, B, and Ce).
- titanium compound as the titanium compound, tetramethoxy titanium, tetraethoxy titanium, tetra-n-propoxy titanium, tetraisopropoxy titanium, tetra-n-butoxy titanium, tetraiso
- titanium compound tetramethoxy titanium, tetraethoxy titanium, tetra-n-propoxy titanium, tetraisopropoxy titanium, tetra-n-butoxy titanium, tetraiso
- examples include at least one selected from tetraalkoxytitanium such as butoxytitanium and tetra-t-butoxytitanium or derivatives thereof, titanium tetrachloride, titanyl sulfate, titanium citrate, and titanium tetranitrate).
- compound semiconductors include II-VI group compound semiconductors, III-V group compound semiconductors, Examples include group IV compound semiconductors and group I-III-VI compound semiconductors).
- Reaction for reducing semiconductor element to produce semiconductor fine particles is an element selected from the group consisting of silicon (Si), germanium (Ge), carbon (C), and tin (Sn)) .
- Magnetic raw materials include nickel, cobalt, iridium, iron, platinum, gold, silver, manganese, chromium, palladium, yttrium, lanthanides (neodymium, samarium, gadolinium , And terbium).
- a fluid in which at least one biologically ingestible particulate raw material is dissolved in a first solvent with a solvent that can be a second solvent having a lower solubility of the biologically ingestible particulate raw material than the first solvent, Reaction to precipitate.
- a reaction in which a fluid containing at least one kind of an acidic substance or a cationic substance and a fluid containing at least one kind of a basic substance or an anionic substance are mixed and the biologically ingested fine particles are precipitated by a neutralization reaction.
- a water-soluble barium salt solution is used as a raw material fluid, and a water-soluble sulfuric acid compound solution containing sulfuric acid is at least one other than the raw material fluid. Both are mixed as a kind of fluid, and barium sulfate fine particles are precipitated by a neutralization reaction.
- At least one of the dispersed phase and the continuous phase contains one or more phospholipids
- the dispersed phase contains a pharmacologically active substance
- the continuous phase comprises at least an aqueous dispersion solvent, and is continuous with the fluid to be treated of the dispersed phase. Treatment to obtain liposomes by mixing with the fluid to be treated in phase.
- a process in which a fluid obtained by dissolving a resin in a solvent that is soluble and compatible with the resin is mixed with an aqueous solvent to obtain resin fine particles by precipitation or emulsification, an oil phase component such as a resin or oil, and an aqueous phase component.
- Processing to obtain an emulsion by mixing or the process which obtains resin fine particles by mixing the resin melted by heating and solvent (it is not limited about aqueous property and oiliness), and emulsifying and dispersing.
- the resin fine particle dispersion is mixed with a compound solution in which a compound such as a salt is dissolved to aggregate the resin fine particles.
- Friedel-Crafts reaction nitration reaction, addition reaction, elimination reaction, transfer reaction, polymerization reaction, condensation reaction, coupling reaction, acylation, carbonylation, aldehyde synthesis, peptide synthesis, aldol reaction, indole reaction, electrophilic substitution Reaction, nucleophilic substitution reaction, Wittig reaction, Michael addition reaction, enamine synthesis, ester synthesis, enzyme reaction, diazo coupling reaction, oxidation reaction, reduction reaction, multistage reaction, selective addition reaction, Suzuki-Miyaura coupling reaction, Kumada-Corriu reaction, metathesis reaction, isomerization reaction, radical polymerization reaction, anion polymerization reaction, cation polymerization reaction, metal catalyzed polymerization reaction, sequential reaction, polymer synthesis, acetylene coupling reaction, episulfide synthesis, episulfide synthesis, Bamberger rearrangement, Chapman rearrangement, Claisen condensation, quinoline synthesis, Paal-Kn
- “from the center” means “from the first introduction part d1” of the fluid treatment apparatus shown in FIG. 1, and the first fluid is the first fluid to be treated described above.
- the second fluid refers to the second fluid to be treated introduced from the second introduction part d2 of the treatment apparatus shown in FIG.
- the shape of the opening d20 of the fluid processing apparatus of FIG. 1 is a concentric ring shape surrounding the central opening of the processing surface 2 as indicated by a dotted line in FIG.
- Examples 1 to 3 Comparative Examples 1 to 3 Production of Quinacridone Nanoparticles
- at least one of them has an approachable / separable processing surface disposed opposite to the other.
- quinacridone pigment (CIPigment Red 122, hereinafter PR-122) is concentrated sulfuric acid.
- the quinacridone solution dissolved in the solution and methanol are mixed and the precipitation reaction is performed in the thin film fluid.
- a 2.0 wt% PR-122 solution in which PR-122 powder is dissolved in concentrated sulfuric acid as the first fluid, which is the first fluid, is fed from the center at a supply pressure / back pressure 0.350 MPa / 0.02 MPa, and methanol is supplied first.
- Two fluids were introduced between the processing surfaces. (Rotation speed: 1500rpm)
- the first fluid and the second fluid were mixed in the thin film fluid, and the PR-122 fine particle dispersion was discharged from between the processing surfaces 1 and 2.
- the PR-122 fine particles in the discharged PR-122 fine particle dispersion were loosely agglomerated, collected using a filter cloth having a mesh opening of 1.0 ⁇ m, washed with pure water, and a wet cake of PR-122 fine particles was obtained.
- the obtained PR-122 dispersion was diluted, placed on a collodion membrane, and subjected to TEM observation to confirm the primary particle size.
- TEM observation JEM-2100 manufactured by JEOL Ltd. was used, and the primary particle diameter was observed and measured at a magnification of 20,000 times for a plurality of visual fields, and an average value was used.
- Table 1 shows the production volume and primary particle size (indicated as particle size in Table 1) of the first and second fluids and PR-122 fine particles.
- the opening d20 of the separate introduction path d2 has a single concentric annular shape surrounding the central opening of the processing surface 2 as described above.
- the ratio (a / b) between the total opening area (a) of the gap between the processing surfaces and the total opening area (b) of the opening leading to the separate introduction path is 1. 0, 2.0 in Example 2, 5.0 in Example 3, 5.6 in Comparative Example 1, 25.0 in Comparative Example 2, and 100.0 in Comparative Example 3. From Table 1, it was found that the production amount can be easily increased by using a PR-122 solution containing PR-122 as the fine particle raw material as the first fluid as the first fluid.
- Examples 4-6 Comparative Examples 4-6
- Production of Silver Nanoparticles As shown in FIG. 1, at least one has a processing surface that is disposed so as to be able to approach and leave, with respect to the other.
- a reactor that uniformly diffuses, stirs, and mixes in a thin film fluid formed between the rotating processing surfaces 1 and 2, an aqueous solution of silver nitrate dissolved in pure water and an interface with sodium borohydride as a reducing agent
- a reducing agent solution in which thiocalcol 08 manufactured by Kao Corporation
- thiocalcol 08 manufactured by Kao Corporation
- the obtained silver nanoparticle dispersion was placed on a collodion film, and TEM observation was performed to confirm the primary particle diameter.
- TEM observation JEM-2100 manufactured by JEOL Ltd. was used, and the primary particle diameter was observed and measured at a magnification of 20,000 times for a plurality of visual fields, and an average value was used.
- Table 1 shows the first and second fluids, the production amount of silver nanoparticles, and the primary particle size (shown as particle size in Table 2).
- the opening d20 of the separate introduction path d2 has a single concentric annular shape surrounding the central opening of the processing surface 2 as described above.
- the ratio (a / b) between the total opening area (a) of the gap between the processing surfaces and the total opening area (b) of the opening leading to the separate introduction path is 0. 5, 0.8 in Example 5, 3.8 in Example 6, 8.0 in Comparative Example 4, 40.0 in Comparative Example 5, and 80.0 in Comparative Example 6. From Table 2, it was found that the production amount can be easily increased by using a silver nitrate solution containing silver nitrate as a fine particle raw material as a raw material fluid as a first fluid.
- the first fluid and the second fluid were mixed and emulsified in the thin film fluid, and a liquid containing an acrylic resin monomer emulsion was discharged from between the processing surfaces 1 and 2.
- the particle diameter of the obtained acrylic resin monomer emulsion was measured using a SALD-7000 (manufactured by Shimadzu Corporation) which is a particle size distribution measuring device.
- Table 3 shows the volume average particle diameter (indicated as particle diameter in Table 3) in the production amounts and particle size distribution measurement results of the first and second fluids and the acrylic resin monomer emulsion.
- the apparatus used for these Examples and Comparative Examples has a single concentric annular shape in which the opening d20 of the separate introduction path d2 surrounds the central opening of the processing surface 2 as described above.
- the ratio (a / b) between the total opening area (a) of the gap between the processing surfaces and the total opening area (b) of the opening leading to the separate introduction path is 1. 5, 3.5 in Example 8, 4.5 in Example 9, 8.5 in Comparative Example 7, 10.0 in Comparative Example 8, and 60.0 in Comparative Example 9. From Table 3, it was found that the production amount can be easily increased by using the acrylic resin monomer as the fine particle raw material as the raw material fluid as the first fluid.
- Examples 10-12, Comparative Examples 10-12 Manufacture of Titanium Oxide As shown in FIG. 1, at least one of them has a processing surface that can be approached / separated and is rotated relative to the other. Titanium tetraisopropoxide (TiOiPr) and acetylacetone dissolved in isopropyl alcohol (IPA) using a reactor that uniformly diffuses, stirs, and mixes in a thin film fluid between the processing surfaces 1 and 2 A compound solution and an aqueous ammonia solution are mixed to deposit titanium oxide in a thin film fluid.
- TiOiPr Titanium tetraisopropoxide
- IPA isopropyl alcohol
- the first fluid and the second fluid are mixed in a thin film fluid, and the titanium oxide nanoparticle dispersion is discharged from between the processing surfaces 1 and 2.
- the 4.5 wt% nitric acid aqueous solution in the same amount as the discharged titanium oxide nanoparticle dispersion And mixed.
- the titanium oxide nanoparticles in the resulting titanium oxide nanoparticle dispersion are loosely agglomerated, the titanium oxide nanoparticles are settled using a centrifuge and the supernatant is removed, and then washed with pure water to prepare a titanium oxide nanoparticle wet cake. Obtained. A part of the wet cake of titanium oxide nanoparticles was diluted with pure water and dispersed with an ultrasonic cleaner to obtain a titanium oxide nanoparticle dispersion.
- the obtained titanium oxide nanoparticle dispersion was placed on a collodion film and subjected to TEM observation to confirm the primary particle diameter.
- TEM observation JEM-2100 manufactured by JEOL Ltd. was used, and the primary particle diameter was observed and measured at a magnification of 20,000 times for a plurality of visual fields, and an average value was used. *
- Table 4 shows the production amounts and primary particle diameters of the first and second fluids and the titanium oxide nanoparticles (shown as particle diameters in Table 4). Moreover, the TEM photograph of the titanium oxide nanoparticle produced in Example 11 is shown in FIG.
- the opening d20 of the separate introduction path d2 has a single concentric annular shape surrounding the central opening of the processing surface 2 as described above.
- the ratio (a / b) between the total opening area (a) of the gap between the processing surfaces and the total opening area (b) of the opening leading to the separate introduction path is 0.00 in Example 10. 4, 0.8 in Example 11, 2.8 in Example 12, 8.0 in Comparative Example 10, 35.0 in Comparative Example 11, and 75.0 in Comparative Example 12. From Table 4, it was found that the production amount can be easily increased by using a titanium compound solution containing titanium tetraisopropoxide as a fine particle raw material as a raw material fluid as a first fluid.
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Abstract
Description
上記原理における方法より以前の方法では、その処理用面間の距離を機械的に調節するなどの方法であり、回転により発生する熱とそれにより生じる変形、又は芯ぶれなどを吸収できず、微小な処理用面間の距離、少なくともその距離を10μm以下にするのは実質的に不可能であった。つまり、上記特許文献1の装置の原理を利用して、微小流路中において瞬間的な化学的・物理化学的反応等によるナノ粒子の製造を実現する事を可能とし、本発明者らは鋭意研究の成果により、1mm以下は勿論、驚くべきことに0.1~10μmの微小流路中での瞬間的な攪拌・混合・反応・析出を可能とした。
また、本発明は、上記の処理が、析出、乳化、分散、反応、凝集から選択された少なくとも何れか1種であるものとして実施することができる。
また、上記処理用面の少なくとも1つは、環状をなし、この環状の中央から上記原料流体が上記処理用面間に導入されるものであり、上記原料流体と、上記の少なくとも他の1種類の流体とが合流する、最も環状の中央に近い地点における上記両処理用面間の隙間の総開口面積(a)が、上記別途の導入路に通じる開口部の総開口面積(b)の5倍以下であるものとして実施することができる。
また、上記処理用面の少なくとも1つは、環状をなし、この環状の中央から上記原料流体が上記処理用面間に導入されるものであり、上記処理用面に通じる上記別途の導入路の開口部を少なくとも2つ以上備え、上記原料流体と、上記の少なくとも他の1種類の流体とが合流する、最も環状の中央に近い地点における上記両処理用面間の隙間の総開口面積(a)が、上記別途の導入路に通じる開口部のそれぞれの開口面積の5倍以下であるものとして実施することができる。
また、上記処理用面に通じる上記別途の導入路の開口部の形状が円環形状であるものとして実施することができる。
さらにまた、上記処理用面の少なくとも1つは環状をなし、この環状の中央から上記原料流体が上記処理用面間に導入されるものであり、上記環状の中央から上記処理用面間に導入される単位時間当たりの上記原料流体の流量は、上記開口部からの単位時間当たりの上記少なくとも他の1種類の流体の流量の0.1~20000倍であるものとして実施することができる。
この鏡面研磨の面粗度は、特に限定されないが、好ましくはRa0.01~1.0μm、より好ましくはRa0.03~0.3μmとする。
このように、3次元的に変位可能に保持するフローティング機構によって、第2処理用部20を保持することが望ましい。
P=P1×(K-k)+Ps
なお、図示は省略するが、近接用調整面24を離反用調整面23よりも広い面積を持ったものとして実施することも可能である。
この凹部13の先端と第1処理用面1の外周面との間には、凹部13のない平坦面16が設けられている。
また、各処理用部に設けられる導入用の開口部は、その形状や大きさや数は特に制限はなく適宜変更して実施し得る。また、上記第1及び第2の処理用面1,2間の直前或いはさらに上流側に導入用の開口部を設けてもよい。
さらに、上記第1、第2流体等の被処理流動体の温度を制御したり、上記第1流体と第2流体等との温度差(即ち、供給する各被処理流動体の温度差)を制御することもできる。供給する各被処理流動体の温度や温度差を制御するために、各被処理流動体の温度(処理装置、より詳しくは、処理用面1,2間に導入される直前の温度)を測定し、処理用面1,2間に導入される各被処理流動体の加熱又は冷却を行う機構を付加して実施することも可能である。
また、本実施形態では、第1、第2の処理用面1,2は、共に中央に開口を有する環状をなしているが、何れか一方の処理用面1,2を、中央に開口を有する環状とし、他方には中央に開口を設けずに実施することもできる。この中央の第1導入部d1における第1、第2の処理用面1,2間の隙間の総開口面積(a)は、開口部d20の総開口面積(b)の5倍以下であることが望ましい。ここで、上記総開口面積(a)は、上記第1流体と第2流体とが合流する、最も環状の中央に近い地点f(以下、最近点fという)における上記両処理用面間の総開口面積を意味する(図3(A)参照)。具体的には、第1、第2の処理用面1,2の中心から最近点fまでの距離βを半径とする円周に、第1、第2の処理用面1,2間の距離αを乗じたものが、総開口面積(a)となる。
上記の最近点fは、開口部d20における最も内側(半径方向における上記中心に近い地点)を意味し、開口部d20を2つ以上備える場合においては、そのうち最も径内側の位置とする。
なお、図4に示すように、開口部d20a,d20bを2つ以上備える場合においては、最近点fにおける総開口面積(a)は、各開口部d20a,d20bの開口面積の5倍以下であることが望ましい。
最近点fにおける総開口面積(a)は、開口部d20の総開口面積(b)の5倍以下が好ましいが、より好ましくは3倍以下が好ましく、さらにこのましくは2倍以下が好ましい。さらに下限としては、特に限定されないが、0.001倍以上、より現実的には0.01倍以上であることが望ましい。
さらに、この中央の第1導入部d1からの単位時間当たりの原料流体の流量は、第2導入部d2からの単位時間当たりの少なくとも他の1種類の流体の流量の0.1倍~20000倍であることが望ましい。0.1倍を下回ると、中央からの導入の流量をさほど増大させることができず、効果が小さくなる。20000倍を上回っても特には問題は生じないが、第2導入部d2の総流量が極端に小さくなったり、全体のバランスがくずれるなどの弊害が生ずるおそれがある。
また、本発明においては、原料流体以外の少なくとも他の1種類の流体、すなわち微粒子原料を処理するための流体は、特に限定されず、目的とする微粒子によって適宜選択して実施できる。上記の処理は、特に限定されないが、析出、乳化、分散、反応、凝集等が挙げられる。例えば、本発明において、析出及び/又は乳化によって微粒子を得る場合には、原料流体と、原料流体に含まれる微粒子原料を析出及び/又は乳化させるための流体とを、対向して配設された、接近・離反可能な、少なくとも一方が他方に対して相対的に回転する少なくとも2つの処理用面間にできる薄膜流体中で混合することによって、析出及び/又は乳化された微粒子原料を微粒子として得るものとして実施できる。また、本発明において、還元反応によって微粒子を得る場合には、原料流体と、原料流体に含まれる微粒子原料を還元させるための流体とを、対向して配設された、接近・離反可能な、少なくとも一方が他方に対して相対的に回転する少なくとも2つの処理用面間にできる薄膜流体中で混合することによって、還元された微粒子原料を微粒子として得るものとして実施できる。このように、微粒子原料と得られた微粒子とは、処理の前後において、両者が同じ物質であってもよいし、別の物質であってもよい。
または、少なくとも1種類の顔料を有機溶媒に溶解し調整された顔料溶液を、前記顔料に対しては貧溶媒であり、かつ前記溶液の調整に使用された有機溶媒には相溶性である貧溶媒中に投入して顔料粒子を沈殿させる反応(再沈法)。
または、酸性またはアルカリ性であるpH調整溶液或いは前記pH調整溶液と有機溶媒との混合溶液のいずれかに、少なくとも1種類の顔料を溶解した顔料溶液と、前記顔料溶液に含まれる顔料に溶解性を示さない、若しくは、前記顔料溶液に含まれる溶媒よりも前記顔料に対する溶解性が小さい、前記顔料溶液のpHを変化させる顔料析出用溶液とを混合して顔料粒子を得る反応。
または、酸性物質もしくは陽イオン性物質を少なくとも1種類含む流体と、塩基性物質もしくは陰イオン性物質を少なくとも1種類含む流体とを混合し、中和反応により生体摂取物微粒子を析出させる反応。例えば、本発明において、造影剤として生体内に摂取される硫酸バリウム微粒子を析出させる場合、水溶性バリウム塩溶液を原料流体とし、硫酸を含む水溶性硫酸化合物溶液を原料流体以外の少なくとも他の1種類の流体として両者を混合し、中和反応により硫酸バリウム微粒子を析出させる。
または、分散相もしくは連続相の少なくともどちらか一方に一種類以上のリン脂質を含み、分散相は薬理活性物質を含み、連続相は少なくとも水系分散溶媒よりなり、分散相の被処理流動体と連続相の被処理流動体とを混合することによりリポソームを得る処理。
または、加温して溶融させた樹脂と溶媒(水性及び油性については限定されない)とを混合し、乳化・分散により樹脂微粒子を得る処理。または樹脂微粒子分散液と塩などの化合物を溶解した化合物溶液とを混合して樹脂微粒子を凝集させる処理。
図1に示すように、対向して配設された接近・離反可能な処理用面をもつ、少なくとも一方が他方に対して回転する処理用面1,2の間にできる薄膜流体中で、均一に拡散・攪拌・混合する反応装置を用いて、有機顔料であるキナクリドン顔料(C.I.Pigment Red 122、以下PR-122)を濃硫酸に溶解したキナクリドン溶液とメタノールとを混合し、薄膜流体中で析出反応を行う。
第1流体と第2流体は薄膜流体中で混合され、PR-122微粒子分散液を処理用面1,2間より吐出させた。吐出されたPR-122微粒子分散液中のPR-122微粒子を緩く凝集させ、目開き1.0μmのろ布を用いてろ集し、純水にて洗浄後、PR-122微粒子のウェットケーキを得た。PR-122微粒子のウェットケーキを一部、界面活性剤としてネオゲンR-K(第一工業製薬株式会社製)水溶液にて希釈し、回転式分散機であるクレアミックス(商品名CLM-2.2S、エム・テクニック株式会社製)にて再分散処理し、PR-122分散液を作製した。
表1より、微粒子原料であるPR-122を含むPR-122溶液を第1流体である原料流体とすることで容易に生産量を増加することが可能であることがわかった。
図1に示すように、対向して配設された接近・離反可能な処理用面をもつ、少なくとも一方が他方に対して回転する処理用面1,2の間にできる薄膜流体中で、均一に拡散・攪拌・混合する反応装置を用いて、硝酸銀を純水に溶解した硝酸銀水溶液と還元剤として水素化ホウ素ナトリウムと界面活性剤としてチオカルコール08(花王株式会社製)をメタノールとトルエンの混合溶媒に溶解した還元剤溶液とを混合し、薄膜流体中で還元反応を行う。
第1流体と第2流体は薄膜流体中で混合され、銀ナノ粒子分散液を処理用面1,2間より吐出させた。吐出された銀ナノ粒子分散液中の銀ナノ粒子を緩く凝集させ、目開き1.0μmのろ布を用いてろ集し、メタノールとトルエンにて洗浄後、銀ナノ粒子のウェットケーキを得た。銀ナノ粒子のウェットケーキの一部をトルエンにて希釈し、超音波洗浄機にて分散処理し、銀ナノ粒子分散液を得た。
表2より、微粒子原料である硝酸銀を含む硝酸銀溶液を第1流体である原料流体とすることで容易に生産量を増加することが可能であることがわかった。
図1に示すように、対向して配設された接近・離反可能な処理用面をもつ、少なくとも一方が他方に対して回転する処理用面1,2の間にできる薄膜流体中で、均一に拡散・攪拌・混合する反応装置を用いて、アクリル樹脂モノマーとポリビニルピロリドン(PVP)を純水に溶解したPVP水溶液とを混合し、薄膜流体中で乳化を行う。
第1流体と第2流体は薄膜流体中で混合・乳化され、アクリル樹脂モノマーエマルションを含む液を処理用面1,2間より吐出させた。
表3より、微粒子原料であるアクリル樹脂モノマーを第1流体である原料流体とすることで容易に生産量を増加することが可能であることがわかった。
図1に示すように、対向して配設された接近・離反可能な処理用面をもつ、少なくとも一方が他方に対して回転する処理用面1,2の間にできる薄膜流体中で、均一に拡散・攪拌・混合する反応装置を用いて、チタニウムテトライソプロポキシド(TiOiPr)とアセチルアセトンをイソプロピルアルコール(IPA)に溶解したチタン化合物溶液と、アンモニア水溶液とを混合し、薄膜流体中で酸化チタンの析出を行う。
第1流体と第2流体は薄膜流体中で混合され、酸化チタンナノ粒子分散液を処理用面1,2間より吐出させ、吐出された酸化チタンナノ粒子分散液と同量の4.5wt%硝酸水溶液とを混合した。得られた酸化チタンナノ粒子分散液中の酸化チタンナノ粒子を緩く凝集させ、遠心分離機を用いて酸化チタンナノ粒子を沈降させ上澄みを除去した後、純水にて洗浄し、酸化チタンナノ粒子のウェットケーキを得た。酸化チタンナノ粒子のウェットケーキの一部を純水にて希釈し、超音波洗浄機にて分散処理し、酸化チタンナノ粒子分散液を得た。
表4より、微粒子原料であるチタンテトライソプロポキシドを含むチタン化合物溶液を第1流体である原料流体とすることで容易に生産量を増加することが可能であることがわかった。
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
d1 第1導入部
d2 第2導入部
d20 開口部
p 流体圧付与機構
Claims (7)
- 被処理流動体として少なくとも2種類の流体を用いるものであり、
そのうちで少なくとも1種類の流体は、微粒子原料を少なくとも1種類含む原料流体であり、
上記以外の流体で少なくとも他の1種類の流体は、上記微粒子原料を処理するための流体であり、
上記の2種以上の被処理流動体を、対向して配設された、接近・離反可能な、少なくとも一方が他方に対して相対的に回転する少なくとも2つの処理用面の間にできる薄膜流体中で混合し、微粒子を得る微粒子の製造方法において、
上記原料流体を、対向して配設された、接近・離反可能な、少なくとも一方が他方に対して相対的に回転する少なくとも2つの処理用面の中央より導入する事を特徴とする、微粒子の生産量増加方法。 - 上記の処理が、析出、乳化、分散、反応、凝集から選択された少なくとも何れか1種であることを特徴とする、請求項1に記載の微粒子の生産量増加方法。
- 上記原料流体が上記薄膜流体を形成しながら上記両処理用面間を通過し、
上記原料流体が流される流路とは独立した別途の導入路を備えており、
上記少なくとも2つの処理用面の少なくとも何れか一方が、上記別途の導入路に通じる開口部を少なくとも一つ備え、
上記少なくとも他の1種類の流体を、上記開口部から上記処理用面の間に導入し、
上記原料流体と上記少なくとも他の1種類の流体とが、上記薄膜流体中で混合されることを特徴とする、請求項1または2に記載の微粒子の生産量増加方法。 - 上記処理用面の少なくとも1つは、環状をなし、この環状の中央から上記原料流体が上記処理用面間に導入されるものであり、
上記原料流体と、上記の少なくとも他の1種類の流体とが合流する、最も環状の中央に近い地点における上記両処理用面間の隙間の総開口面積(a)が、上記別途の導入路に通じる開口部の総開口面積(b)の5倍以下であることを特徴とする、請求項3に記載の微粒子の生産量増加方法。 - 上記処理用面の少なくとも1つは、環状をなし、この環状の中央から上記原料流体が上記処理用面間に導入されるものであり、
上記処理用面に通じる上記別途の導入路の開口部を少なくとも2つ以上備え、
上記原料流体と、上記の少なくとも他の1種類の流体とが合流する、最も環状の中央に近い地点における上記両処理用面間の隙間の総開口面積(a)が、上記別途の導入路に通じる開口部のそれぞれの開口面積の5倍以下であることを特徴とする、請求項3に記載の微粒子の生産量増加方法。 - 上記処理用面に通じる上記別途の導入路の開口部の形状が円環形状である事を特徴とする、請求項3~5何れかに記載の微粒子の生産量増加方法。
- 上記処理用面の少なくとも1つは環状をなし、この環状の中央から上記原料流体が上記処理用面間に導入されるものであり、
上記環状の中央から上記処理用面間に導入される単位時間当たりの上記原料流体の流量は、上記開口部からの単位時間当たりの上記少なくとも他の1種類の流体の流量の0.1~20000倍であることを特徴とする、請求項3~6何れかに記載の微粒子の生産量増加方法。
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KR20140016344A (ko) | 2014-02-07 |
CN103561857B (zh) | 2016-06-15 |
EP2716355B1 (en) | 2020-05-13 |
EP2716355A1 (en) | 2014-04-09 |
JP5959115B2 (ja) | 2016-08-02 |
JPWO2012164999A1 (ja) | 2015-02-23 |
US9539642B2 (en) | 2017-01-10 |
KR101912136B1 (ko) | 2018-10-26 |
CN103561857A (zh) | 2014-02-05 |
EP2716355A4 (en) | 2015-02-25 |
US20140121336A1 (en) | 2014-05-01 |
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