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WO2024257790A1 - Procédé de production d'une composition de dispersion - Google Patents

Procédé de production d'une composition de dispersion Download PDF

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Publication number
WO2024257790A1
WO2024257790A1 PCT/JP2024/021314 JP2024021314W WO2024257790A1 WO 2024257790 A1 WO2024257790 A1 WO 2024257790A1 JP 2024021314 W JP2024021314 W JP 2024021314W WO 2024257790 A1 WO2024257790 A1 WO 2024257790A1
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WO
WIPO (PCT)
Prior art keywords
dispersion
liquid medium
material composition
raw material
sealing liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/JP2024/021314
Other languages
English (en)
Japanese (ja)
Inventor
秀彰 高井
和彦 坪谷
悟 相澤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toyocolor Co Ltd
Artience Co Ltd
Original Assignee
Toyocolor Co Ltd
Artience Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Toyocolor Co Ltd, Artience Co Ltd filed Critical Toyocolor Co Ltd
Publication of WO2024257790A1 publication Critical patent/WO2024257790A1/fr
Anticipated expiration legal-status Critical
Pending legal-status Critical Current

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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
    • B01F23/41—Emulsifying
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/45—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/46—Homogenising or emulsifying nozzles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/71—Feed mechanisms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/06—Jet mills
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/02—Feeding devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B1/00—Multi-cylinder machines or pumps characterised by number or arrangement of cylinders
    • F04B1/04—Multi-cylinder machines or pumps characterised by number or arrangement of cylinders having cylinders in star- or fan-arrangement
    • F04B1/0404—Details or component parts
    • F04B1/0448—Sealing means, e.g. for shafts or housings

Definitions

  • the present invention relates to a method for producing a dispersion composition.
  • Methods for dispersing dispersoids in a dispersion medium include agitators, ball mill dispersers, bead mill dispersers, ultrasonic dispersers, single-axis kneaders, multi-axis kneaders, roll mill dispersers, and high-pressure homogenizers.
  • Bead mill dispersers are widely used from the viewpoint of dispersion efficiency, and while bead mills have the advantage of applying impact to the dispersoid to finely disperse it, the impact can damage the dispersoid and reduce its original properties.
  • High-pressure homogenizers can homogenously disperse the treatment liquid by ejecting the treatment liquid from a nozzle or by passing the treatment liquid through a homogenizing valve. Since the treatment liquid is supplied at high pressure to increase dispersion efficiency, the dispersoids can be finely dispersed by shear forces and collisions between the treatment liquids themselves and collisions with the wall of the homogenizing valve.
  • Valve-type high-pressure homogenizers are suitable for mass production because they can increase the flow rate of the processing liquid and do not require nozzles, which can cause clogging, and are used as homogenizers for aqueous products such as dairy products and beverages.
  • Dairy products and other products are aqueous with a low solid content, so they have a small effect on the components of the dispersion device, and have the advantage that the packing of the high-pressure pump, for example, deteriorates slowly and can be replaced at longer intervals.
  • high-pressure homogenizers have also been used as dispersion devices for a variety of dispersion compositions, such as inks.
  • Inks and other products use a variety of dispersoids and liquid media.
  • Raw material compositions containing solids are prone to attack the packing of high-pressure pumps, and deterioration of the packing can shorten the replacement interval for the packing, reducing work efficiency. Furthermore, deterioration of the packing can also cause the problem of increased leakage of the raw material composition from the high-pressure pump.
  • Patent Document 1 proposes a method in which a crude dispersion containing carbon nanotubes and a solvent is stored in a tank and then sent to a disperser by a high-pressure pump for dispersion processing, in which the high-temperature carbon nanotube dispersion discharged from the disperser is cooled to prevent air bubbles from being generated in the dispersion, and the back pressure of the dispersion is reduced in multiple stages to prevent air bubbles from being generated in the dispersion when atmospheric pressure is released, thereby improving the dispersibility of the carbon nanotubes.
  • a plunger is used in a high-pressure pump to supply the raw material composition to a dispersion mechanism at high pressure. Since the plunger is installed inside a cylinder, a gland packing has been arranged in the gap between the plunger and the cylinder in the conventional technology.
  • the gland packing deteriorates with repeated use and requires replacement, and the possibility of liquid leakage due to deterioration of the gland packing cannot be completely eliminated.
  • the raw material composition contains dispersoids and dispersion medium
  • the gland packing tends to deteriorate due to solids. Therefore, there is an increasing demand for a new technology that solves the problem of deterioration of the gland packing in raw material compositions containing solids.
  • the sealing device disclosed in Patent Document 2 does not use a gland packing, but there was no knowledge of using it in the manufacturing method of a dispersion composition containing solids.
  • One object of the present invention is to improve the life of the sealing mechanism in the dispersion process of a raw material composition containing a dispersion medium and a dispersoid, and to improve the productivity of the dispersion composition.
  • the inventors of the present invention conducted extensive research aimed at solving the above problems and discovered that by using a sealing liquid medium as the sealing mechanism for the plunger, it is possible to seal the plunger without using a gland packing as the sealing mechanism for the plunger.
  • a method for producing a dispersion composition using a dispersion device including a dispersion mechanism for pressurizing and dispersing a raw material composition, a supply mechanism including a plunger portion and for supplying the raw material composition to the dispersion mechanism, and a sealing mechanism for sealing the plunger portion using a sealing liquid medium, wherein the raw material composition includes a dispersoid and a dispersion medium, and the sealing liquid medium includes at least the same dispersoid as the raw material composition and the same dispersion medium as the raw material composition.
  • ⁇ 2> The method for producing a dispersion composition according to ⁇ 1>, wherein the sealing liquid medium is pressurized using an independent pump and supplied to the sealing mechanism.
  • ⁇ 3> The method for producing a dispersion composition according to ⁇ 1> or ⁇ 2>, wherein the sealing liquid medium has a particle diameter D50 at a cumulative 50% volumetric percentage of a particle size distribution measured by a dynamic light scattering method of 5 ⁇ m or less.
  • ⁇ 4> The method for producing a dispersion composition according to any one of ⁇ 1> to ⁇ 3>, wherein the sealing liquid medium has a viscosity of 10,000 mPa ⁇ s or less at 25° C.
  • the life of the sealing mechanism can be improved during the dispersion process of a raw material composition containing a dispersion medium and a dispersoid, and the productivity of the dispersion composition can be improved.
  • FIG. 2 is a schematic diagram illustrating an example of a dispersing device.
  • FIG. 2 is a cross-sectional view illustrating a schematic diagram of a high-pressure pump and a sealing mechanism of an example of a dispersion device.
  • FIG. 2 is a cross-sectional view showing a schematic diagram of a homogenization valve of a dispersing section of an example of a dispersing device.
  • the dispersion composition may further contain a dispersant.
  • the dispersion composition can be produced using a dispersion device that includes a dispersion mechanism for pressurizing and dispersing the raw material composition, a supply mechanism that includes a plunger portion and supplies the raw material composition to the dispersion mechanism, and a sealing mechanism that seals the plunger portion using a sealing liquid medium.
  • the raw material composition is a composition that contains the raw materials of the dispersion composition mixed together.
  • the raw material composition may be a composition in a mixed state, or a composition in a roughly dispersed state after mixing.
  • a dispersion device is a high-pressure homogenizer.
  • the raw material composition is supplied at high pressure from a high-pressure pump to a dispersion section by reciprocating movement of a plunger, and the raw material composition can be dispersed in the dispersion section.
  • the dispersion section the raw material composition is sprayed at high pressure from a minute opening at the tip of a nozzle, and the dispersoids can be dispersed in the dispersion medium by collisions and shear forces between the raw material compositions.
  • the raw material composition is supplied at high pressure to a homogenizing valve, and the raw material composition is collided with the wall surface of the homogenizing valve to apply an impact, thereby dispersing the dispersoids in the dispersion medium.
  • a method of performing dispersion processing using a homogenizing valve can increase the flow rate of the raw material composition, avoid problems such as nozzle clogging, and is suitable for mass production.
  • the pressure of the raw material composition when supplied to the dispersion section is preferably 10 to 150 MPa. If the dispersion section is a nozzle type, the pressure of the raw material composition when supplied to the dispersion section is preferably in the normal range of 60 to 150 MPa. If the dispersing machine is a valve type, the pressure of the raw material composition when supplied to the dispersing machine is preferably in the normal range of 10 to 150 MPa.
  • FIG. 1 shows a schematic diagram of an example of a dispersion device.
  • the dispersion device 100 includes a high-pressure pump 20, which is one form of a supply mechanism, a dispersion section 30, which is one form of a dispersion mechanism, and a sealing mechanism 40.
  • the high-pressure pump 20 includes a plunger 10.
  • the raw material composition tank 50 is a container that contains the raw material composition to be supplied to the high-pressure pump 20.
  • the high-pressure pump 20 has a supply port 22 through which the raw material composition is supplied from the raw material composition tank 50, and a discharge port 23 through which the raw material composition is discharged to the dispersion section 30.
  • the high-pressure pump 20 has a cylinder 21 that supports the plunger 10 so that it can move back and forth in the axial direction.
  • the cylinder 21 is provided with a sealing mechanism 40 to prevent the raw material composition and pressure from leaking out of the high-pressure pump 20.
  • One end of the plunger 10 is inserted into the high-pressure pump 20, and the other end extends outside the high-pressure pump 20 and is supported by the cylinder 21.
  • the sliding surfaces of the plunger 10 and the cylinder 21 are preferably sealed to prevent leakage of the raw material composition from the high-pressure pump 20, and it is also preferable that pressure loss does not occur due to air leaking from the high-pressure pump 20 to the outside.
  • the plunger 10 reciprocates in the axial direction, changing the volume of the pressure chamber of the high-pressure pump 20.
  • the raw material composition When the plunger 10 is pulled out of the high-pressure pump 20 and the volume of the pressure chamber increases, the raw material composition is sucked in from the supply port 22 of the high-pressure pump 20, and when the plunger 10 is pushed out into the high-pressure pump 20 and the volume of the pressure chamber decreases, the raw material composition is discharged from the discharge port 23 of the high-pressure pump 20.
  • the supply port 22 and discharge port 23 of the high-pressure pump 20 are each preferably provided with a valve to prevent backflow of the raw material composition.
  • the raw material composition discharged from the high-pressure pump 20 is supplied to the dispersion section 30 at high pressure.
  • the dispersion section 30 may be of a nozzle type or a valve type. Since it is possible to supply a large amount of raw material composition at high pressure to the dispersion section 30 using a plunger 10, the dispersion section 30 is preferably of a valve type, and more specifically, a homogenization valve is preferable.
  • a dispersion composition in which dispersoids are dispersed in a dispersion medium is obtained.
  • the dispersion composition that has been subjected to the dispersion process can be collected in a dispersion composition tank through piping from the outlet of the dispersion section 30.
  • the sealing mechanism 40 includes a sealing liquid medium supply pipe 41, a sealing liquid medium discharge pipe 42, and a storage section 43 that supplies the sealing liquid medium to the sealing liquid medium supply pipe 41 and collects the sealing liquid medium from the sealing liquid medium discharge pipe 42.
  • the sealing liquid medium supplied from the sealing mechanism 40 into the cylinder 21 fills the gap G between the outer circumferential surface of the plunger 10 and the inner circumferential surface of the cylinder 21, sealing this gap G.
  • this gap G is densely filled with the raw material composition and/or the sealing liquid medium.
  • the gap G is preferably formed around the entire circumference of the outer circumferential surface of the plunger 10.
  • the pressure load can be reduced.
  • the liquid medium in contact with the outer circumferential surface of the plunger 10 may be a sealing liquid medium, or may be a raw material composition indirectly pressurized by the sealing liquid medium.
  • the boundary B between the raw material composition and the sealing liquid medium may form an interface without mixing with each other, or may mix with each other and show a concentration gradient.
  • the boundary B is formed in the gap G between the outer circumferential surface of the plunger 10 and the inner circumferential surface of the cylinder 21. The supply pressures of the sealing liquid medium and the raw material composition are adjusted so that the boundary B is not formed on the pump chamber 24 side of the tip of the plunger 10 within the range of the reciprocating movement of the plunger 10 in the axial direction of the plunger 10.
  • the solids concentration and other properties of the resulting dispersion composition do not fluctuate significantly, but it is advisable to prevent a large amount of the sealing liquid medium from being discharged into the pump chamber 24.
  • the sealing liquid medium is supplied from and collected in the storage section 43.
  • the sealing liquid medium collected in the storage section 43 may be reused and recirculated.
  • the sealing liquid medium discharged from the sealing liquid medium discharge pipe 42 may be discarded.
  • the sealing liquid medium may be pressurized using an independent pump and supplied to the sealing mechanism.
  • a pump may be provided in the path of the sealing liquid medium supply pipe 41, making it possible to supply high-pressure sealing liquid medium into the cylinder 21. Pressurization by this pump applies a shear force to the sealing liquid medium, making it possible to maintain good dispersibility of the dispersoids in the sealing liquid medium.
  • the sealing liquid medium is mixed with the raw material composition, the possibility of causing aggregation of the dispersoids can be further reduced.
  • FIG. 2 A specific example of a dispersion device will be described with reference to Figures 2 and 3. Components common to Figure 1 are given the same reference numerals, and parts not specifically described are as described in Figure 1 above.
  • the supply port 22 and discharge port 23 of the high-pressure pump 20 are provided with check valves 22a and 23a, respectively.
  • the inner circumferential surface of the cylinder 21 is tightly filled with a sealing liquid medium in a chamber 44 by a sealing mechanism 40.
  • a plunger 10 is provided within the cylinder 21.
  • the outer end of the high-pressure pump 20 in the axial direction of the plunger 10 is provided with a mechanism for transmitting reciprocating movement via a rod 81 by a crankshaft 82, and the plunger 10 is capable of reciprocating movement in the axial direction.
  • the sealing mechanism 40 includes a sealing liquid medium supply pipe 41, a sealing liquid medium discharge pipe 42, and a pump 45 capable of supplying the sealing liquid medium at high pressure to the sealing liquid medium supply pipe 41.
  • a tank may be provided in which the sealing liquid medium supplied to the pump 45 is stored.
  • a mechanism may be provided in which the sealing liquid medium discharged from the sealing liquid medium discharge pipe 42 is collected in this tank and recirculated.
  • the sealing mechanism 40 includes a chamber 44 that holds the sealing liquid medium on the inner circumferential surface of the cylinder 21.
  • a gap G is formed between the inner circumferential surface of the cylinder 21 and the outer circumferential surface of the plunger 10.
  • the raw material composition is supplied from the pump chamber 24 and filled into this gap G. Pressure is released between the gap G and the chamber 44 through the through opening 44a.
  • the pressure environment is such that the raw material composition in the gap G is at a positive pressure relative to the sealing liquid medium in the chamber 44. This makes it possible to prevent the sealing liquid medium from flowing from the gap G into the dispersion section.
  • the raw material composition in the gap G is tightly filled into the outer circumferential surface of the plunger 10 by the pressure from the sealing liquid medium in the chamber 44, thereby improving the sealing performance.
  • the external pressure in the chamber 44 can be adjusted by adjusting the output of the pump 45.
  • the internal pressure of the raw material composition can be adjusted by adjusting the output of the plunger 10.
  • the external pressure is 50 to 5000 bar
  • the internal pressure is 80 to 8000 bar
  • the internal pressure is 400 to 1500 bar.
  • the chamber 44 is preferably formed around the entire circumference of the cylinder 21.
  • the chamber 44 may be provided at one or more locations in the axial direction of the cylinder 21.
  • two chambers 44 are arranged at two locations in the axial direction of the cylinder 21 via a partition wall. This allows for more uniform sealing in the gap G within the axial movement range of the plunger 10.
  • the contact area between the raw material composition and the sealing liquid medium can be reduced, so that mixing of the two liquid media can be further suppressed, and fluctuations in the solid content in the resulting dispersion composition can be further reduced.
  • the through openings 44a may be provided in a number separated from one another in the circumferential direction of the chamber 44. In another example, the through openings 44a may be provided in communication around the entire circumferential direction of the chamber 44.
  • FIG 3 is a cross-sectional view showing a schematic diagram of the homogenization valve of the dispersion section 30.
  • the homogenization valve of the dispersion section 30 includes a valve seat 31, an impact ring 32, and a homogenizing valve 33.
  • the raw material composition supplied from the high-pressure pump 20 is supplied to the homogenization valve at high pressure in the direction of the arrow in the figure and subjected to a fine dispersion process, and is then discharged from an outlet section (not shown).
  • a valve-type high-pressure homogenizer may be used, such as the "HC3 Series” manufactured by Sanmaru Machinery Co., Ltd., the "HV-H Series” manufactured by Izumi Food Machinery Co., Ltd., or the "R-Model” manufactured by SPX Flow Co., Ltd.
  • a nozzle-type high-pressure homogenizer may be used.
  • a nozzle-type high-pressure homogenizer As a nozzle-type high-pressure homogenizer, the "Genus PY” manufactured by Genus Co., Ltd., the “Starburst” manufactured by Sugino Machine Co., Ltd., the “Nanomizer” manufactured by Nanomizer Co., Ltd., or the like may be used, but is not limited to these.
  • a nozzle-type high-pressure homogenizer includes a pump and one or more nozzles, and there are various nozzle shapes for dispersion processing. For example, there are types that collide raw materials with each other under high pressure, types that collide high-pressure raw materials with ceramic balls or pass them through slits and process them with the shear force, and types that utilize cavitation caused by a jet of high-pressure raw materials, but are not limited to these.
  • the seal mechanism between the plunger and the cylinder may be changed to the seal mechanism described above.
  • the raw material composition supplied to the dispersion device is not particularly limited as long as it contains a dispersoid and a dispersion medium.
  • the raw material composition may further contain a dispersant to obtain dispersion stability of the dispersoid.
  • the raw material composition may contain optional components such as a resin emulsion, a surfactant, a binder resin, a wetting agent, a wetting penetrating agent, and a leveling agent, as necessary.
  • Ceramics include metal oxides, carbonates, nitrides, phosphates, and carbides, such as calcium oxide, calcium carbonate, magnesium oxide, magnesium carbonate, magnesium phosphate, aluminum oxide, aluminum nitride, aluminum phosphate, boron nitride, silicon oxide, silicon nitride, silicon carbide, zirconium oxide, titanium oxide, and kaolin clay.
  • Metals include zinc, lead, titanium, cadmium, iron, copper, cobalt, etc., or alloys thereof.
  • resin particles are preferred, and examples thereof include polystyrene, polyurethane, polyester, polyamide, vinyl polymers, acrylic polymers, and composite polymers thereof; cellulose, pulp fibers, and the like.
  • organic or inorganic pigments may be used.
  • organic pigments include azo, phthalocyanine, anthraquinone, perylene, perinone, quinacridone, thioindigo, dioxazine, isoindolinone, quinophthalone, azomethine azo, dictopyrrolopyrrole, and isoindoline pigments.
  • carmine 6B lake red C, permanent red 2B, disazo yellow, pyrazolone orange, carmine FB, chromophthalic yellow, chromophthalic red, phthalocyanine blue, phthalocyanine green, dioxazine violet, quinacridone magenta, quinacridone red, indanthrone blue, pyrimidine yellow, thioindigo bordeaux, thioindigo magenta, perylene red, perinone orange, isoindolinone yellow, diketopyrrolopyrrole red, aniline black, and daylight fluorescent pigments.
  • organic pigments include the colorants listed in the Color Index International (C.I.), which are organic compounds or organometallic complexes, such as C.I. Pigment Black, C.I. Pigment Blue, C.I. Pigment Green, C.I. Pigment Red, C.I. Pigment Violet, C.I. Pigment Yellow, C.I. Pigment Orange, and C.I. Pigment Brown.
  • C.I. Color Index International
  • Inorganic pigments include white pigments such as titanium oxide, zinc oxide, zinc sulfide, barium sulfate, calcium carbonate, chromium oxide, and silica; and non-white pigments such as aluminum powder, mica, bronze powder, chrome vermilion, yellow lead, cadmium yellow, cadmium red, aluminum hydroxide, ultramarine, Prussian blue, red iron oxide, yellow iron oxide, iron black, titanium oxide, and zinc oxide.
  • white pigments such as titanium oxide, zinc oxide, zinc sulfide, barium sulfate, calcium carbonate, chromium oxide, and silica
  • non-white pigments such as aluminum powder, mica, bronze powder, chrome vermilion, yellow lead, cadmium yellow, cadmium red, aluminum hydroxide, ultramarine, Prussian blue, red iron oxide, yellow iron oxide, iron black, titanium oxide, and zinc oxide.
  • the above-mentioned dispersoids may be surface-treated.
  • the above-mentioned dispersoids may be used alone or in combination of two or more.
  • the content of the dispersoid in the raw material composition is not particularly limited and may be appropriately adjusted depending on the materials of the dispersoid and the dispersion medium within a range in which the dispersoid can be dispersed in the dispersion medium after dispersion treatment.
  • a dispersion medium capable of dispersing the dispersoid may be used depending on the type of dispersoid.
  • the dispersion medium may be a non-aqueous dispersion medium or an aqueous dispersion medium.
  • the dispersion medium may contain either an organic solvent or water.
  • the dispersion medium may contain at least one of a water-insoluble organic solvent and a water-soluble organic solvent.
  • the dispersion medium is preferably a combination of a water-soluble organic solvent and water.
  • the dispersion medium may also consist of only water.
  • the organic solvent may be either a non-polar solvent or a polar solvent, and may be used in combination within the range of miscibility.
  • Non-polar solvents include aliphatic hydrocarbon solvents such as hexane, cyclohexane, and paraffin, aromatic hydrocarbon solvents such as benzene, toluene, and xylene, and other petroleum-based hydrocarbon solvents.
  • Polar solvents include ester-based solvents, ether-based solvents, alcohol-based solvents, ketone-based solvents, amide-based solvents, heterocyclic solvents, sulfoxide-based solvents, sulfone-based solvents, and carbonate-based solvents.
  • organic solvents include amides (N-methyl-2-pyrrolidone (NMP), N-ethyl-2-pyrrolidone (NEP), N,N-dimethylformamide, N,N-dimethylacetamide, N,N-diethylacetamide, N-methylcaprolactam, etc.), heterocyclics (cyclohexylpyrrolidone, 2-oxazolidone, 1,3-dimethyl-2-imidazolidinone, ⁇ -butyrolactone, etc.), sulfoxides (dimethyl sulfoxide, etc.), sulfones (hexamethylphosphorotriamide, sulfolane, etc.), lower ketones (acetone, methyl ethyl ketone, etc.), carbonates (diethyl carbonate, dimethyl carbonate, ethyl methyl carbonate, fluoroethylene carbonate, propylene carbonate, ethylene carbonate), tetrahydrofuran
  • NMP
  • organic solvents include formic acid, acetic acid, methanol, ethanol, propanol, methyl acetate, ethyl acetate, diethyl ether, etc.
  • examples of the organic solvent include ethyl lactate, benzyl alcohol, 1,2,3-trichloropropane, 1,3-butanediol, 1,3-butylene glycol, 1,3-butylene glycol diacetate, 1,4-dioxane, 2-heptanone, 2-methyl-1,3-propanediol, 3,5,5-trimethyl-2-cyclohexen-1-one, 3,3,5-trimethylcyclohexanone, 3-ethoxyethylpropionate, 3-methyl-1,3-butanediol, 3-methoxy-3-methyl-1-butanol, 3-methoxy-3-methylbutyl acetate, 3-methoxybutanol, 3-methoxybutyl acetate, 4-heptan
  • the raw material composition may further contain a dispersant.
  • the dispersant may be either a resin-type dispersant or a surfactant, but a suitable type of dispersant may be used in a suitable amount depending on the characteristics required for dispersing the dispersoid.
  • Resin-type dispersants that can be used include (meth)acrylic polymers, polymers derived from ethylenically unsaturated hydrocarbons, cellulose derivatives, and copolymers thereof.
  • polymers derived from ethylenically unsaturated hydrocarbons include polyvinyl alcohol resins, polyvinylpyrrolidone resins, polyacrylonitrile resins, and nitrile rubbers.
  • polyvinyl alcohol resins include polyvinyl alcohol, modified polyvinyl alcohols having functional groups other than hydroxyl groups (e.g., acetyl groups, sulfo groups, carboxy groups, carbonyl groups, and amino groups), polyvinyl alcohols modified with various salts, other anion- or cation-modified polyvinyl alcohols, and polyvinyl acetals (polyvinyl acetoacetal, polyvinyl butyral, etc.) modified with aldehydes (acetoacetal-modified or butyral-modified, etc.).
  • functional groups other than hydroxyl groups e.g., acetyl groups, sulfo groups, carboxy groups, carbonyl groups, and amino groups
  • polyvinyl alcohols modified with various salts other anion- or cation-modified polyvinyl alcohols
  • polyvinyl acetals polyvinyl acetoacetal, polyvinyl butyral, etc.
  • the polyacrylonitrile resin may be a homopolymer of polyacrylonitrile, a copolymer of polyacrylonitrile, or a modified product thereof.
  • the acrylonitrile copolymer described in JP-A-2020-163362 can be used.
  • nitrile rubbers include acrylonitrile butadiene rubber and hydrogenated acrylonitrile butadiene rubber.
  • cellulose derivatives include cellulose acetate, cellulose acetate butyrate, cellulose butyrate, cyanoethyl cellulose, ethyl hydroxyethyl cellulose, nitrocellulose, methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl cellulose, and the like, or copolymers thereof.
  • dispersants described in International Publication No. 2008/108360, JP 2018-192379 A, JP 2019-087304 A, Japanese Patent No. 6524479 A, and JP 2009-026744 A may be used, but are not limited thereto.
  • methyl cellulose, ethyl cellulose, polyvinyl alcohol, polyvinyl butyral, polyvinyl pyrrolidone, homopolymer of polyacrylonitrile, copolymer of polyacrylonitrile, and hydrogenated acrylonitrile butadiene rubber are preferred.
  • Polymers in which other substituents have been introduced into a portion of these polymers, modified polymers, and the like may also be used.
  • the surfactant may be any of anionic surfactants, cationic surfactants, zwitterionic surfactants, and nonionic surfactants.
  • the dispersant is preferably 5 to 300 parts by mass, more preferably 10 to 200 parts by mass, and even more preferably 15 to 100 parts by mass, relative to 100 parts by mass of the dispersoid.
  • the content of the dispersoids in the total amount of the raw material composition varies depending on the specific gravity of the dispersoids, but is preferably 0.1 to 80 mass%, more preferably 0.5 to 60 mass%, and even more preferably 0.7 to 50 mass%.
  • the solid content of the raw material composition is preferably 0.5 to 80 mass%, more preferably 0.7 to 60 mass%, and even more preferably 1 to 50 mass%.
  • the sealing liquid medium contains at least the same dispersoid as the raw material composition and the same dispersion medium as the raw material composition.
  • the sealing liquid medium may contain at least the same dispersoid of a simple substance or compound as the raw material composition and the same dispersion medium as the raw material composition.
  • the sealing liquid medium contains at least the same dispersoid as the raw material composition. That is, it is sufficient that at least one dispersoid is the same between the sealing liquid medium and the raw material composition.
  • two or more dispersoids are contained in either the sealing liquid medium or the raw material composition, it is sufficient that any one dispersoid is the same between the sealing liquid medium and the raw material composition.
  • the sealing liquid medium and the raw material composition each contain one dispersoid, and these dispersoids are the same as each other.
  • the sealing liquid medium and the raw material composition each contain two or more dispersoids, it is preferable that these two or more dispersoids are the same as each other.
  • the sealing liquid medium contains at least the same dispersion medium as the raw material composition. That is, it is sufficient that at least one type of dispersion medium is the same between the sealing liquid medium and the raw material composition.
  • at least one type of dispersion medium is the same between the sealing liquid medium and the raw material composition.
  • any one type of dispersion medium is the same between the sealing liquid medium and the raw material composition.
  • the sealing liquid medium and the raw material composition each contain one type of dispersion medium, and these dispersion media are the same as each other.
  • the sealing liquid medium and the raw material composition each contain two or more types of dispersion media, it is preferable that these two or more dispersion media are the same as each other.
  • At least one dispersoid and at least one dispersion medium may be the same between the sealing liquid medium and the raw material composition.
  • the sealing liquid medium and the raw material composition each contain one dispersoid and one dispersion medium, which are the same between the sealing liquid medium and the raw material composition.
  • the sealing liquid medium and the raw material composition each contain two or more dispersoids and two or more dispersion media, which are the same between the sealing liquid medium and the raw material composition.
  • the sealing liquid medium may contain a single component dispersoid, or may contain two or more types of dispersoid.
  • the type of dispersoid is not particularly limited, and one or more types may be selected and used from those described in the raw material composition.
  • the dispersoid of the sealing liquid medium is selected so that at least one type is the same as the dispersoid of the raw material composition.
  • the raw material composition and the sealing liquid medium may each contain dispersoids having the same chemical composition, or may each contain dispersoids that are the same simple substance or compound.
  • the raw material composition and the sealing liquid medium may each contain the same simple substance or compound selected from inorganic particles, organic particles, inorganic-organic composite particles, etc.
  • inorganic particles include carbon materials and titanium oxide
  • organic particles include phthalocyanine blue and isoindolinone pigments.
  • the dispersoids of each of them are the same, so that the variation in dispersibility of the dispersoids in the mixed liquid of the raw material composition and the sealing liquid medium can be reduced.
  • the raw material composition and the sealing liquid medium may each contain dispersoids having the same particle shape.
  • the particle shape being the same may mean that at least one of the physical property values such as particle appearance observation, average particle size, particle size distribution, and specific surface area is within a predetermined range.
  • the particle diameter D50 at the cumulative 50% volume of the particle size distribution of the raw material composition measured by the dynamic light scattering method of the sealing liquid medium is within ⁇ 20% of the particle diameter D50 at the cumulative 50% volume of the particle size distribution of the raw material composition measured by the dynamic light scattering method.
  • the raw material composition and the sealing liquid medium may each contain a dispersoid that is the same allotrope.
  • allotropes of carbon materials include graphite, fullerene, carbon nanotubes, graphene, etc. These examples of carbon materials can be treated as the same material as a dispersoid, but it is preferable that the raw material composition and the sealing liquid medium each contain the same allotrope, for example, carbon nanotubes, as a dispersoid. This can further reduce the fluctuation in solid concentration in the dispersion composition after the dispersion treatment, and can further reduce the fluctuation in the uniformity of the solid components.
  • the dispersoid either single-walled carbon nanotubes or multi-walled carbon nanotubes may be used.
  • carbon nanotubes regardless of the type of single-walled carbon nanotubes or multi-walled carbon nanotubes, at least one of them may be included as a dispersoid in the raw material composition and the sealing liquid medium, respectively.
  • the raw material composition and the sealing liquid medium each include single-walled carbon nanotubes or multi-walled carbon nanotubes as a dispersoid.
  • the sealing liquid medium may contain a single component dispersion medium, or may contain two or more types of dispersion medium.
  • the type of dispersion medium is not particularly limited, and one or more types may be selected from those described in the raw material composition.
  • the dispersion medium of the sealing liquid medium is selected so that at least one type is the same as the dispersion medium of the raw material composition.
  • the raw material composition and the sealing liquid medium may each contain a dispersion medium having the same chemical composition, or may each contain a dispersion medium that is the same compound.
  • the raw material composition and the sealing liquid medium may each contain the same compound from N-methyl-2-pyrrolidone, water, propylene glycol monomethyl acetate, etc.
  • the content of the dispersoid in the total amount of the sealing liquid medium varies depending on the specific gravity of the dispersoid, but is preferably 0.1 to 80 mass%, more preferably 0.5 to 60 mass%, and even more preferably 0.7 to 50 mass%.
  • the solid content of the sealing liquid medium is preferably 0.5 to 80 mass%, more preferably 0.7 to 60 mass%, and even more preferably 1 to 50 mass%.
  • the content of the dispersoid in the total amount of the sealing liquid medium varies within a range of 80 to 120% by mass relative to that of the raw material composition, so that the solid content can be more appropriately maintained in the resulting dispersion composition.
  • the content of the dispersoid in the sealing liquid medium varies within a range of 80 to 120% by mass relative to that of the raw material composition, so that the solid content can be more appropriately maintained in the resulting dispersion composition.
  • the sealing liquid medium may further contain a dispersant to obtain dispersion stability of the dispersoid.
  • the dispersant may be either a resin-type dispersant or a surfactant, but a suitable type of dispersant may be used in a suitable amount depending on the characteristics required for dispersing the dispersoid.
  • At least one dispersant may be selected from the dispersants listed in the raw material composition above.
  • the raw material composition and the sealing liquid medium preferably contain the same dispersant. This makes it possible to further suppress the decrease in dispersibility of the dispersoid when the raw material composition and the sealing liquid medium come into contact with or mix with each other in the sealing mechanism.
  • the mass ratio of the dispersant to the dispersoid in the sealing liquid medium from 80 to 120% by mass with respect to that of the raw material composition, the mass ratio of the dispersant to the dispersoid in the resulting dispersion composition can be maintained, and the decrease in dispersibility can be further suppressed.
  • the sealing liquid medium may contain optional components such as a resin emulsion, a surfactant, a binder resin, a wetting agent, a wetting penetrant, and a leveling agent, as necessary. It is preferable that the raw material composition and the sealing liquid medium each contain the same optional components. This makes it possible to further suppress the decrease in dispersibility of the dispersoid when the raw material composition and the sealing liquid medium come into contact with or are mixed in the sealing mechanism.
  • optional components such as a resin emulsion, a surfactant, a binder resin, a wetting agent, a wetting penetrant, and a leveling agent, as necessary. It is preferable that the raw material composition and the sealing liquid medium each contain the same optional components. This makes it possible to further suppress the decrease in dispersibility of the dispersoid when the raw material composition and the sealing liquid medium come into contact with or are mixed in the sealing mechanism.
  • the sealing liquid medium has a particle diameter D50 of 5 ⁇ m or less at a cumulative 50% of the volume of the particle size distribution measured by dynamic light scattering.
  • this particle diameter D50 is also referred to simply as D50. If the D50 of the sealing liquid medium is excessively large, it may rub against the inner surface of the cylinder 21 or the outer surface of the plunger 10 in the sealing mechanism, which may promote deterioration of these components. In addition, if coarse particles are contained in the sealing liquid medium held in the chamber 44 in the sealing mechanism, the possibility of clogging in the gaps between the components cannot be eliminated, which may promote deterioration of the components.
  • the D50 of the sealing liquid medium may be 5 ⁇ m or less, 3 ⁇ m or less, 1 ⁇ m or less, or 0.5 ⁇ m or less.
  • the D50 of the sealing liquid medium may be 0.1 ⁇ m or more, 0.2 ⁇ m or more, or 0.3 ⁇ m or more.
  • the D50 of the sealing liquid medium may be 0.1 to 5 ⁇ m, 0.1 to 3 ⁇ m, 0.1 to 1 ⁇ m, or 0.1 to 0.5 ⁇ m.
  • the D50 of the sealing liquid medium is more preferably 0 to 5 ⁇ m, 0.1 to 3 ⁇ m, or 0.1 to 2 ⁇ m.
  • the sealing liquid medium contains carbon nanotubes
  • the D50 of the sealing liquid medium satisfies the above-mentioned numerical range.
  • Carbon nanotubes are a relatively hard dispersoid, but when the above-mentioned numerical range is satisfied, deterioration of the sealing mechanism components can be more reliably suppressed.
  • the particle size distribution of the dispersoid in the dispersion medium is measured using a dynamic light scattering method. More specifically, it can be measured according to the method described in the Examples.
  • the viscosity of the sealing liquid medium at 25°C is 20,000 mPa ⁇ s or less. If the viscosity of the sealing liquid medium is excessive, the frictional force between the cylinder 21 and the plunger 10 in the sealing mechanism increases, which may increase the driving load and promote deterioration of the components. Furthermore, in a state in which a high-viscosity sealing liquid medium is held in the chamber 44 in the sealing mechanism, the possibility of clogging in the gaps between the components cannot be eliminated, which may promote deterioration of the components.
  • the viscosity of the sealing liquid medium may be 20,000 mPa ⁇ s or less, 15,000 mPa ⁇ s or less, 10,000 mPa ⁇ s or less, 8,000 mPa ⁇ s or less, or 5,000 mPa ⁇ s or less.
  • the lower limit of the viscosity is not particularly limited, but from the viewpoint of ensuring the fluidity of the sealing liquid medium, the viscosity of the sealing liquid medium may be 1 mPa ⁇ s or more, 10 mPa ⁇ s or more, 30 mPa ⁇ s or more, or 100 mPa ⁇ s or more.
  • the viscosity of the sealing liquid medium may be 10 to 20,000 mPa ⁇ s, 10 to 15,000 mPa ⁇ s, 30 to 10,000 mPa ⁇ s, 30 to 8,000 mPa ⁇ s, or 100 to 5,000 mPa ⁇ s.
  • the viscosity of the sealing liquid medium is more preferably 10 to 10,000 mPa ⁇ s, 10 to 8,000 mPa ⁇ s, or 10 to 5,000 mPa ⁇ s.
  • the sealing liquid medium contains carbon nanotubes
  • Carbon nanotubes are a dispersoid that has a relatively high viscosity, but when the above-mentioned numerical range is satisfied, deterioration of the components of the sealing mechanism can be more reliably suppressed.
  • the viscosity of a composition containing a dispersoid and a dispersion medium is the viscosity measured at 25°C using a Brookfield viscometer at 60 rpm. More specifically, it can be measured according to the method described in the Examples.
  • the sealing mechanism life can be determined by operating a dispersion device for 100 hours using a combination of a raw material composition and a sealing liquid medium described in the Examples below, and the leakage rate (%) can be calculated by measuring the amount of raw material composition leaked from the sealing mechanism and the supply amount of the raw material composition, which are expressed by the following formula.
  • Leakage rate (%) (leakage amount (L)/supplied amount of raw material composition (L)) ⁇ 100
  • the amount of raw material composition leaking from the sealing mechanism is the amount of raw material composition leaking out of the sealing mechanism during 100 hours of operation
  • the amount of raw material composition supplied is the total amount discharged from the dispersion device during 100 hours of operation.
  • the sealing mechanism of the dispersion device be replaced infrequently.
  • the mechanism uses a sealing liquid medium to seal the dispersion device, there is no need to replace the gland packing periodically, and the leakage rate can be controlled by pressure, improving production efficiency.
  • the leakage rate represented by the above formula is preferably 0.2% or less, and more preferably 0.1% or less. If the leakage rate is 0.21% or more, the amount of raw material composition leaking from the sealing mechanism increases as the operating time increases, and the yield of the dispersion composition tends to decrease. If the sealing performance of the dispersion device can be better ensured by controlling the sealing pressure of the sealing liquid medium, the particle diameter D50 at 50% cumulative volume of the particle size distribution measured by dynamic light scattering, the viscosity, etc., it is expected that the leakage rate represented by the above formula will approach 0%.
  • the dispersing device can disperse particles by high pressure treatment without applying mechanical shock to the particles, and is therefore suitable for use in maintaining the shape of the particles while dispersing them. Furthermore, it is suitable for use in use in defibrating aggregates such as fibrous particles to increase dispersibility. For example, it can be suitably used in a method for producing a carbon nanotube dispersion.
  • carbon nanotubes are also referred to as CNT.
  • the dispersion medium can be the above-mentioned dispersion medium.
  • the dispersion medium may be either a non-aqueous dispersion medium or an aqueous dispersion medium, but it is preferable to include an aprotic solvent, a non-polar solvent, or a combination thereof, more preferably to include an aprotic solvent, and even more preferably to include an aprotic polar solvent.
  • the aprotic polar solvent can better prevent the aggregation of carbon nanotubes, and is also excellent in solubility of a resin-type dispersant suitable for dispersing carbon nanotubes.
  • the solvent contains an amide solvent, and specifically, it is more preferable that the solvent contains at least one selected from the group consisting of N-methyl-2-pyrrolidone, N-ethyl-2-pyrrolidone, and 1-n-octyl-2-pyrrolidone.
  • the carbon nanotubes preferably have the following characteristics before being dispersed and used in the raw material composition.
  • CNTs are flat graphite rolled into a cylindrical shape, and include single-walled CNTs and multi-walled CNTs, which may be mixed together.
  • Single-walled CNTs have a structure in which a single layer of graphite is rolled.
  • Multi-walled CNTs have a structure in which two or more layers of graphite are rolled.
  • the sidewalls of the CNTs do not have to have a graphite structure.
  • CNTs with sidewalls having an amorphous structure are also considered CNTs in this disclosure.
  • the shape of the CNT is not limited. Examples of such shapes include needle-like, cylindrical tube-like, fishbone-like (fishbone or cup stack type), trump-like (platelet) and coil-like. Of these, the shape of the CNT is preferably needle-like or cylindrical tube-like.
  • the CNT may be a single shape or a combination of two or more shapes.
  • CNTs may have the following forms: graphite whiskers, filamentous carbon, graphite fibers, ultrafine carbon tubes, carbon tubes, carbon fibrils, carbon microtubes, and carbon nanofibers. Carbon nanotubes may have any of these forms alone or in combination of two or more of them.
  • the average outer diameter of the CNTs is preferably 1 nm or more, and more preferably 4 nm or more. It is also preferably 30 nm or less, more preferably 20 nm or less, and even more preferably 15 nm or less.
  • the average outer diameter of the CNTs can be calculated by first observing and photographing the CNTs using a transmission electron microscope, randomly selecting 300 CNTs from the photograph, measuring the outer diameter of each, and averaging the results.
  • the average fiber length of the CNTs is preferably 0.5 ⁇ m or more, more preferably 0.8 ⁇ m or more, and even more preferably 1.0 ⁇ m or more. It is also preferably 1000 ⁇ m or less, more preferably 100 ⁇ m or less, and even more preferably 10 ⁇ m or less.
  • the average fiber length of the CNTs can be calculated by first observing and photographing the CNTs with a scanning electron microscope, randomly selecting 300 CNTs from the photograph, measuring the fiber length of each, and averaging the measured fiber length.
  • the aspect ratio is the fiber length of CNT divided by the outer diameter.
  • a representative aspect ratio can be calculated using the average fiber length and average outer diameter.
  • the aspect ratio of CNT is preferably 30 or more, more preferably 50 or more, and even more preferably 80 or more. It is also preferably 1,000,000 or less, more preferably 100,000 or less, and even more preferably 10,000 or less.
  • the specific surface area of the CNT is preferably 100 m 2 /g or more, more preferably 150 m 2 /g or more, and even more preferably 200 m 2 /g or more. Also, it is preferably 1200 m 2 /g or less, and more preferably 1000 m 2 /g or less.
  • the specific surface area of the CNT is calculated by the BET method using nitrogen adsorption measurement.
  • the carbon nanotubes may be surface-treated carbon nanotubes.
  • the carbon nanotubes may be carbon nanotube derivatives to which a functional group, such as a carboxyl group, has been added.
  • Carbon nanotubes that encapsulate organic compounds, metal atoms, or substances, such as fullerenes, may also be used.
  • the raw material composition containing carbon nanotubes may contain a dispersant, and the above-mentioned dispersants can be used as the dispersant.
  • a resin-type dispersant In order to further increase the dispersion stability of carbon nanotubes in the dispersion medium, it is preferable to use a resin-type dispersant.
  • methyl cellulose, ethyl cellulose, polyvinyl alcohol, polyvinyl butyral, polyvinylpyrrolidone, polyacrylonitrile homopolymer, polyacrylonitrile copolymer, and hydrogenated acrylonitrile butadiene rubber are preferable.
  • the raw material composition containing carbon nanotubes may further contain optional components such as the above-mentioned binder resin.
  • the carbon nanotube content is preferably 0.1 to 20 mass% relative to the total amount of the raw material composition, more preferably 0.5 to 15 mass%, and even more preferably 0.7 to 10 mass%.
  • the dispersant is preferably 5.0 to 300 parts by mass relative to 100 parts by mass of the carbon nanotubes.
  • the raw material composition containing carbon nanotubes has a solid content of preferably 0.5 to 50 mass%, more preferably 0.7 to 30 mass%, and even more preferably 1 to 20 mass%.
  • the sealing liquid medium preferably contains carbon nanotubes as a dispersoid. Details of CNTs are as described above.
  • the sealing liquid medium preferably contains carbon nanotubes as a dispersoid and contains an aprotic solvent, a nonpolar solvent, or a combination thereof as a dispersion medium.
  • the content of carbon nanotubes in the total amount of the sealing liquid medium is preferably 0.1 to 80 mass%, more preferably 0.5 to 60 mass%, and even more preferably 0.7 to 50 mass%.
  • the dispersant is preferably 5.0 to 300 mass parts per 100 mass parts of carbon nanotubes.
  • the solid content of the sealing liquid medium is preferably 0.5 to 80 mass%, more preferably 0.7 to 60 mass%, and even more preferably 1 to 50 mass%.
  • the formulation of the raw material composition is as shown in Table 1.
  • the components were mixed according to the formulation shown in the table to obtain a raw material composition. Details of the components shown in the table are as follows.
  • Multilayer CNT "K-Nanos 100P" (trade name), manufactured by Kumho Petrochemical.
  • Single-walled CNT “TNSR” (product name), manufactured by Timesnano.
  • Copper phthalocyanine "FASTOGEN EP-210" (product name) manufactured by DIC.
  • Zetpol 2000L (product name): manufactured by Zeon Corporation.
  • APP-84 (trade name): Carboxymethyl cellulose, manufactured by Nippon Paper Industries Co., Ltd., "Sunrose A APP-84" (trade name), weight average molecular weight 17,600.
  • BYK-P104 (product name): manufactured by BYK.
  • PGMAc in the table is propylene glycol monomethyl acetate.
  • the binder resin solutions shown in the table are the same as those prepared from the CuPc dispersion liquid of the sealing liquid medium described below.
  • sealing fluid The formulation of the sealing liquid medium is described below. In the following formulation, the same components as those in the above-mentioned sealing liquid medium are used.
  • CNT dispersion (2) Multilayer CNT: 3% by mass N-methyl-2-pyrrolidone: 96% by mass Dispersant "Zetpol 2000L" (product name): 1% by mass Dispersion time: 5 hours
  • the method for producing the CNT dispersion liquid among the sealing liquid mediums is as follows.
  • the components were mixed according to the above recipe, and a CNT dispersion was obtained using the following dispersing device.
  • the dispersion device used was a valve-type high-pressure homogenizer "HC3-5" (product name) manufactured by Sanmaru Machinery Co., Ltd.
  • the dispersion conditions were as follows: ⁇ Dispersion conditions> Processing pressure: 100 MPa Type of homogenizing part: flat valve Flow rate of raw material composition: 2000 L/H
  • the method for producing the CuPc dispersion liquid among the sealing liquid media is as follows. The components were mixed according to the above recipe, and a CuPc dispersion was obtained using a dispersing device in the same procedure as for the CNT dispersion of the above sealing liquid medium.
  • the method for producing the resin-type dispersant solution in the CuPc dispersion formulation is as follows. PGMAc was added to BYK-P104 (manufactured by BYK Japan: non-volatile content 50%) to adjust the non-volatile content to 40%, to obtain a resin-type dispersant solution.
  • Binder resin solution The method for producing the binder resin solution in the CuPc dispersion formulation is as follows. A separable 4-neck flask was fitted with a thermometer, a cooling tube, a nitrogen gas inlet tube, and a stirrer. 70.0 parts of cyclohexanone was charged in the reaction vessel, which was then heated to 80°C and substituted with nitrogen in the reaction vessel.
  • a mixture of 13.3 parts of n-butyl methacrylate, 4.6 parts of 2-hydroxyethyl methacrylate, 4.3 parts of methacrylic acid, 7.4 parts of paracumylphenol ethylene oxide modified acrylate ("Aronix M110" manufactured by Toa Gosei Co., Ltd.), and 0.4 parts of 2,2'-azobisisobutyronyl methyl acrylate was added dropwise over 2 hours. After completion of the dropwise addition, the reaction was continued for another 3 hours to obtain a solution of an acrylic resin having a weight average molecular weight (Mw) of 26,000. After cooling to room temperature, about 2 g of the resin solution was sampled and dried by heating at 180° C. for 20 minutes to measure the non-volatile content. Propylene glycol monoethyl ether acetate (PGMAc) was added to the previously synthesized resin solution so that the non-volatile content was 20 mass % to obtain a binder resin solution.
  • PGMAc Propylene
  • a dispersion device equipped with a supply mechanism equivalent to the high pressure pump 20 shown in FIG. 2 and a dispersion mechanism using a homogenizing valve was used.
  • the raw material composition is supplied from the supply mechanism to a plunger, and the raw material composition is supplied from the plunger to the dispersion mechanism.
  • the outer peripheral surface of the plunger is sealed with a sealing liquid medium.
  • Dispersion treatment was performed using the raw material composition and the sealing liquid medium in the combination shown in Table 1.
  • the dispersion conditions were as follows. ⁇ Dispersion conditions> Processing pressure: 100 MPa Type of homogenizing part: flat valve Flow rate of raw material composition: 2000 L/H
  • Comparative Example 2 a gland packing was used for the sealing mechanism. Specifically, a valve-type high-pressure homogenizer "HC3-5" (product name) manufactured by Sanmaru Machinery Co., Ltd. was used for the dispersion device. The dispersion conditions were as follows. The other conditions were the same as those in Example 1. ⁇ Dispersion conditions> Processing pressure: 100 MPa Type of homogenizing part: flat valve Flow rate of raw material composition: 2000 L/H
  • the D50 of the sealing liquid medium was measured using the same procedure as the particle size distribution of the dispersion composition after the dispersion treatment described below.
  • the viscosity of the sealing liquid medium was measured by leaving the carbon nanotube dispersion liquid in a thermostatic chamber at 25°C for at least one hour, and then using a B-type viscometer ("BL" manufactured by Toki Sangyo Co., Ltd.) at a rotor rotation speed of 60 rpm.
  • the types of rotors used in the measurements were No. 1 when the viscosity value was less than 100 mPa ⁇ s, No. 2 when it was 100 to less than 500 mPa ⁇ s, No. 3 when it was 500 to less than 2,000 mPa ⁇ s, and No. 4 when it was 2,000 to less than 10,000 mPa ⁇ s.
  • the leakage amount is a value calculated by the following formula.
  • the sealing mechanism is a sealing liquid medium; (1) The amount of liquid in the sealing liquid medium tank before the start of operation is A liters. (2) When the total operating time reaches 100 hours, the amount of liquid in the sealing liquid medium tank is B liters.
  • Leakage volume (L) B(L) - A(L)
  • Leakage rate is 0.1% or less
  • Leakage rate is greater than 0.1% and 0.2% or less
  • Leakage rate is 0.21% or more
  • Refractive index of water 1.333, refractive index of N-methyl-2-pyrrolidone: 1.47, refractive index of PGMAc: 1.402, density of multi-walled CNT and single-walled CNT: 1.80, density of copper phthalocyanine: 1.84
  • the life of the sealing mechanism tends to be improved by reducing the D50 of the sealing liquid medium.
  • the D50 can be controlled in the resulting dispersion composition.
  • the life of the sealing mechanism tends to be improved by reducing the viscosity of the sealing liquid medium.

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Abstract

La présente invention améliore la durée de vie d'un mécanisme d'étanchéité dans un traitement de dispersion d'une composition de matériau d'alimentation comprenant un milieu de dispersion et une phase dispersée, ce qui permet d'améliorer l'efficacité de la production d'une composition de dispersion. La présente invention concerne un procédé de production d'une composition de dispersion au moyen d'un dispositif de dispersion comprenant : un mécanisme de dispersion qui met sous pression et disperse une composition de matériau d'alimentation; un mécanisme d'alimentation qui est équipé d'une partie piston et fournit la composition de matériau d'alimentation au mécanisme de dispersion; et un mécanisme d'étanchéité qui ferme de manière étanche la partie piston avec un milieu liquide pour l'étanchéité. La composition de matériau d'alimentation comprend une phase dispersée et un milieu de dispersion, et le milieu liquide pour l'étanchéité comprend au moins la même phase dispersée que celle de la composition de matériau d'alimentation et le même milieu de dispersion que celui de la composition de matériau d'alimentation.
PCT/JP2024/021314 2023-06-14 2024-06-12 Procédé de production d'une composition de dispersion Pending WO2024257790A1 (fr)

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JP2009026744A (ja) 2007-06-18 2009-02-05 Toyo Ink Mfg Co Ltd 電池用組成物
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JP2018511018A (ja) 2015-03-18 2018-04-19 ハンメルマン ゲゼルシャフト ミット ベシュレンクテル ハフツング シールデバイス
JP2018192379A (ja) 2017-05-12 2018-12-06 東洋インキＳｃホールディングス株式会社 分散剤、分散組成物、電池用分散組成物、電極、電池
JP2019087304A (ja) 2017-11-01 2019-06-06 東洋インキＳｃホールディングス株式会社 分散剤、分散組成物、電池用分散組成物、電極、電池
JP6524479B1 (ja) 2018-07-20 2019-06-05 東洋インキＳｃホールディングス株式会社 化合物、分散剤、電池用分散組成物、電極、電池
JP2020163362A (ja) 2019-03-29 2020-10-08 東洋インキＳｃホールディングス株式会社 分散剤、分散体、電極、および樹脂組成物
DE102020003401A1 (de) * 2020-06-05 2021-12-09 Netzsch-Feinmahltechnik Gmbh Hochdruckhomogenisator
JP2023097975A (ja) 2021-12-28 2023-07-10 トヨタ自動車株式会社 セパレータのリーク検査装置

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