WO2018186295A1 - 無機粒子分散体 - Google Patents
無機粒子分散体 Download PDFInfo
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- WO2018186295A1 WO2018186295A1 PCT/JP2018/013660 JP2018013660W WO2018186295A1 WO 2018186295 A1 WO2018186295 A1 WO 2018186295A1 JP 2018013660 W JP2018013660 W JP 2018013660W WO 2018186295 A1 WO2018186295 A1 WO 2018186295A1
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
- C08L101/02—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C08L101/06—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing oxygen atoms
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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
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/40—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/062—Copolymers with monomers not covered by C08L33/06
- C08L33/066—Copolymers with monomers not covered by C08L33/06 containing -OH groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/002—Pigment pastes, e.g. for mixing in paints in organic medium
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/006—Metal
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D201/00—Coating compositions based on unspecified macromolecular compounds
- C09D201/02—Coating compositions based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C09D201/06—Coating compositions based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0831—Gold
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
Definitions
- the present invention relates to a dispersion containing inorganic particles having excellent spinnability.
- the coating solution when coating is performed by the above coating method, the coating solution is required to have high elasticity and stringiness so that the coating solution does not break during coating.
- the coating amount is increased to increase the coating thickness (the coating thickness is the same as the clearance) and the coating speed is reduced. There are restrictions.
- the present invention has been proposed in view of the above points, and an object thereof is to provide an inorganic particle dispersion having high spinnability in one aspect.
- the inorganic particle dispersion according to an embodiment of the present invention includes an inorganic powder, hydrophilic fumed silica, and a resin having a hydroxyl group.
- an inorganic particle dispersion having high spinnability can be provided.
- FIG. 1 is a view for explaining the spinnability of the inorganic particle dispersion according to this embodiment.
- FIG. 2 is an example of a coating film applied using the inorganic particle dispersion according to the present embodiment.
- FIG. 3 is an example of a coating film applied using the inorganic particle dispersion according to the present embodiment.
- FIG. 4 is a diagram for explaining the printability of a coating film applied using the inorganic particle dispersion according to the present embodiment.
- FIG. 5 is a diagram for explaining the effect of the glass component modifier in the inorganic particle dispersion according to the present embodiment.
- the inorganic particle dispersion includes an inorganic component as a main component, but may include an organic component as another component.
- the other components include, for example, various additives for improving the spinnability, a dispersant for improving the dispersibility of the inorganic particles, a leveling agent for improving the leveling property, and adjusting the viscosity of the coating liquid. Including organic solvents, and the like.
- the inorganic particle dispersion according to the present embodiment is applied onto a substrate and dried. And after giving desired printing (including drawing) on the obtained dry film
- the inorganic particle dispersion according to the present embodiment includes at least an inorganic powder, hydrophilic fumed silica, and a resin having a hydroxyl group.
- the inorganic particle dispersion according to the present embodiment may contain other organic components for improving the characteristics.
- the inorganic powder contained in the inorganic particle dispersion according to the present embodiment is not particularly limited.
- glass powder, gold powder, silver powder, copper powder, iron powder, stainless steel powder, titanium powder, nickel powder, chromium powder, tungsten examples thereof include metal powders such as powder and molybdenum powder.
- the above-mentioned powders are sintered by firing at a high temperature (for example, when glass powder is used, the temperature is equal to or higher than the softening point of glass). By utilizing this, a dense inorganic film can be formed on the substrate.
- a component adjusting agent for suppressing foaming from the glass and for preventing breakage of characters after printing.
- the component modifier dissolves in the glass film formed when the glass is baked, and plays a role of controlling the fluidity and clarification action when the glass is softened.
- Preferred component modifiers include kaolin containing an alumina component as a main component, calcined kaolin, bentonite containing an alkali metal as a main component, and the like.
- kaolin containing an alumina component as a main component
- calcined kaolin bentonite containing an alkali metal as a main component
- the foaming and character collapse can be suppressed without reducing the Vickers strength of the resulting inorganic film. it can.
- the content of the inorganic powder in the inorganic particle dispersion according to the present embodiment is not particularly limited, but is usually 10% by mass to 85% by mass, and preferably 40% by mass to 70% by mass.
- the content of the inorganic powder is less than 10% by mass, sufficient performance of the sintered product may not be ensured because sufficient filler cannot be present in the inorganic film obtained after sintering.
- content of inorganic powder exceeds 85 mass%, it may become impossible to adjust to the viscosity suitable for application
- Hydrophilic fumed silica is a kind of dry silica obtained by using silicon tetrachloride as a starting material and undergoing processes such as oxidation, desalting and purification in a flame.
- Hydrophilic fumed silica improves the spinnability of the resulting inorganic particle dispersion by interacting with a hydroxyl group resin described later. Therefore, even when a relatively strong shear stress is applied during the application of the inorganic particle dispersion as the coating liquid, the coating liquid is difficult to break. Therefore, even if it is a case where the inorganic particle dispersion which concerns on this embodiment is applied to the coating method which requires a shear stress, it can apply
- fumed silica examples include hydrophilic fumed silica and hydrophobic fumed silica obtained by surface-treating this hydrophilic fumed silica with a silane-based additive (silane coupling agent). From the viewpoint of the spinnability of the particle dispersion, it is preferable to use hydrophilic fumed silica.
- the content of hydrophilic fumed silica in the inorganic particle dispersion according to this embodiment is not particularly limited, but is usually 0.01% by mass to 5% by mass, preferably 0.05% by mass to 2% by mass. %.
- content of fumed silica is less than 0.01% by mass, the spinnability of the obtained inorganic particle dispersion may not be exhibited.
- content of fumed silica exceeds 5 mass%, the silica which remains in a sintered film after sintering may change the characteristic of a sintered film.
- ⁇ Resin having a hydroxyl group Although it does not specifically limit as resin which has a hydroxyl group, In order to improve the spinnability of the inorganic particle dispersion obtained, it is preferable to use resin which has high elasticity. Specifically, a modified acrylic resin having a hydroxyl group, an epoxy resin, a urethane resin, a phenol resin, ethyl cellulose, a butyral resin (butyral resin has a hydroxyl group remaining in the production process), a gelatin resin, or the like is preferably used. it can. In addition, you may use these resin modified so that it may have a hydroxyl group.
- the spinnability of the resulting inorganic particle dispersion is improved by the interaction between the hydroxyl group-containing resin and the hydrophilic fumed silica. Therefore, even when a relatively strong shear stress is applied during coating, the coating solution containing the inorganic particle dispersion is difficult to break. Therefore, even if it is a case where the inorganic particle dispersion which concerns on this embodiment is applied to the coating method which requires a shear stress, it can apply
- the content of the resin having a hydroxyl group in the inorganic particle dispersion according to the present embodiment is not particularly limited, but is usually 1% by mass to 50% by mass, and preferably 5% by mass to 35% by mass.
- content of the resin having a hydroxyl group is less than 1% by mass, the spinnability of the obtained inorganic particle dispersion may not be exhibited.
- content of resin which has a hydroxyl group exceeds 50 mass%, it may become impossible to adjust to the viscosity suitable for application
- the inorganic particle dispersion according to this embodiment may contain other components for improving the properties of the coating liquid.
- Other components include a dispersant for improving the dispersibility of the inorganic particles, a leveling agent for improving the leveling property, an organic solvent for adjusting the viscosity of the coating liquid, and various types for improving the spinnability. And additives.
- the inorganic particle dispersion according to this embodiment may contain a dispersant having a functional group or the like at the end in order to stably disperse the particles in the dispersion.
- the content of the dispersant is preferably 0.1 to 5% by mass.
- the dispersant is not particularly limited, and for example, a cationic dispersant, an anionic dispersant, a nonionic dispersant, an amphoteric dispersant, a silicone dispersant, a fluorine-based dispersant, and the like can be used.
- the inorganic particle dispersion according to this embodiment may contain a wetting dispersant (anti-settling agent) in order to prevent the filler from settling.
- the content of the wetting and dispersing agent is preferably 0.1 to 5% by mass.
- wetting and dispersing agent examples include “TIXOGEL series” (for example, trade name “TIXOGEL-EZ 100”) of bentonite additives manufactured by Big Chemie Japan, Inc.
- TIXOGEL series for example, trade name “TIXOGEL-EZ 100”
- bentonite-based additives “CLAYTONE series”, “GARAMITE series”, “CLOISITE series”, “OPTIGEL series” manufactured by Big Chemie Japan Co., Ltd. and the like can be mentioned.
- the inorganic particle dispersion according to this embodiment may contain a leveling agent for defoaming and improving leveling properties.
- the content of the leveling agent is preferably 0.1 to 5% by mass.
- the leveling agent improves wettability by reducing the contact angle and surface tension of the inorganic particle dispersion against obstacles that occur on the coating surface, such as coating streaks, craters, and pinholes, and the leveling agent is applied to the coating surface.
- the orientation serves to expand the inorganic particle dispersion.
- the leveling agent is not particularly limited, and conventionally known leveling agents can be used.
- Specific examples of the leveling agent include trade names “BYK (trade name) -361N”, “BYK (trade name) -360P”, “BYK (trade name) -364P”, “BYK (trade name)” manufactured by BYK Chemie. -368P "," BYK (product name) -3900P ",” BYK (product name) -3931P “,” BYK (product name) -3933P “,” BYK (product name) -3950P ",” BYK (product name) " -3951P “,” BYK (trade name) -3955P ", and the like.
- the inorganic particle dispersion according to this embodiment may contain other resin components in order to improve the spinnability.
- the content of other resin components is preferably 1 to 10% by mass.
- the other resin component is preferably a resin having a high modulus of elasticity, for example, the above-described resin having a hydroxyl group, acrylic resin having no hydroxyl group, polybutadiene rubber, polyisoprene rubber, butyl rubber, urethane rubber and the like. Can be mentioned.
- These resins may be hydrogenated resins.
- the spinnability of the inorganic particle dispersion can be improved. Specifically, although depending on the type and content of other components, the normal force value is about 0.2 Pa. Yarn property can be improved.
- the inorganic particle dispersion according to this embodiment may contain an organic solvent for adjusting the viscosity of the coating solution.
- the content of the organic solvent is preferably 10 to 50% by mass.
- Preferable organic solvents include hydrocarbon solvents such as toluene, xylene, cyclohexane, octane, butane, dodecane, and tetradecane.
- a ketone organic solvent may be used. Examples of the ketone organic solvent include acetone, methyl ethyl ketone, methyl isobutyl ketone, diisobutyl ketone, isophorone, and cyclohexanone.
- the inorganic particle dispersion according to the present embodiment may contain other additives depending on required characteristics.
- the content of other additives is preferably 0.1 to 5% by mass.
- additives having high solvent absorbability which are added for the purpose of enabling high-quality printing on the obtained inorganic film.
- the additive having high solvent absorbability exhibits high printability by sucking and holding the ink in the small holes.
- the additive having high solvent absorbability include porous fine particles such as porous silica and porous alumina (fumed alumina), resin components that swell and absorb the solvent, and hydrated alumina.
- hydrophilic fumed silica and the hydroxyl group-containing resin are mixed in a predetermined amount and stirred using a high-speed disperser such as a disper until uniform.
- a high-speed disperser such as a disper until uniform.
- other components such as a dispersant, a leveling agent, an additive having high solvent absorbability, and a glass component modifier are added, they are added at the same timing as the timing at which the above materials are added.
- the above-described inorganic powder is added to the obtained stirring liquid and stirred using a high-speed disperser such as a disper until it is uniformly dispersed.
- a high-speed disperser such as a disper until it is uniformly dispersed.
- resin which has a high elasticity modulus it adds at the same timing as the timing which adds inorganic powder.
- the obtained coating solution is filtered through a 400 mesh stainless steel net or the like, and the coating solution is adjusted to a predetermined viscosity using the solvent described above.
- the inorganic particle dispersion according to this embodiment has high spinnability. Therefore, even when shear stress is applied, it is difficult to cut, and even when applied to various coating methods in which shear stress is applied, high-speed and high-precision coating can be realized.
- the inorganic particle dispersion according to the present embodiment is a method in which a coating liquid is applied to be stretched on a base material using a flat nozzle type dispenser, and the discharge liquid is spirally formed by a needle nozzle or a multi-nozzle. Even when it is applied to a method of coating while being wound around, a coating method using a slit coater, etc., it can be applied at high speed and with high accuracy.
- Example 1 In a high-speed disperser, 157 g of a modified acrylic resin (DHM-63-20HC: manufactured by Harima Chemical Co., Ltd.) as a resin having a hydroxyl group, and hydrophilic fumed silica (AEROSIL 380: average particle diameter of 50 nm: manufactured by Nippon Aerosil Co., Ltd.) 0.5 g, 7 g of fumed alumina (SpectrAl 100: product code FA-100) as an ink absorption component, 5 g of Neugen (ET-89) as a dispersant, and calcined kaolin (PoleStar 400) as a glass component modifier 19.5 g, 10 g filler anti-settling agent (TIXOGEL-EZ 100), and 5 g leveling agent (BYK-392) were added. And it stirred at 1500 rpm for 30 minutes using the high-speed disperser, and dispersed each component.
- DDM-63-20HC manufactured by Harima Chemical Co., Ltd.
- the obtained dispersion was charged with 300 g of glass powder and 5 g of hydrogenated polybutadiene (GI-3000), and further stirred at 1500 rpm for 15 minutes.
- GI-3000 hydrogenated polybutadiene
- Tetradecane was added as a diluting solvent to the kneaded product so that the viscosity was adjusted to a specified viscosity (10 to 11 Pa ⁇ s).
- the maximum normal force value was 2.6 Pa.
- the measurement of the normal force value first, using a rheometer MCR301 (manufactured by Anton Pearl Japan Co., Ltd.), the behavior of normal force (normal stress) when a flat cone plate with a diameter of 25 mm is pulled up at a speed of 10 mm / s. was measured. The normal force behavior reached its maximum value just before the coating solution stretched and started to break, and this maximum value was used to evaluate the stringiness.
- the inorganic particle dispersion obtained in this example has a high spinnability because the hydroxyl group of the modified acrylic resin and the hydrophilic fumed silica are in an interaction state. That is, even when shear stress is applied to the inorganic particle dispersion obtained in this example, it is difficult to cut.
- the inorganic particle dispersion obtained in this example was applied on the substrate so as to stretch the coating solution using a flat nozzle type dispenser, but high-speed and high-precision coating could be realized. It was. A high-speed and high-precision application evaluation method will be described later.
- the inorganic particle dispersion according to the present embodiment can contain a leveling agent, the coating film can be smoothed after application. Furthermore, since the inorganic particle dispersion according to the present embodiment can contain an ink absorbing component, even when ink-jet printing is applied to the coating film, characters and designs do not blur. Furthermore, since the inorganic particle dispersion according to the present embodiment can be blended with a glass component modifier, even when printed characters and patterns are baked, the characters and patterns are not easily broken.
- Example 2 In a high-speed disperser, 157 g of a modified acrylic resin (DHM-63-20HC: manufactured by Harima Chemical Co., Ltd.) as a resin having a hydroxyl group, and hydrophilic fumed silica (AEROSIL 380: average particle diameter of 50 nm: manufactured by Nippon Aerosil Co., Ltd.) 0.5 g and 5 g of Neugen (ET-89) as a dispersant were added. And it stirred at 1500 rpm for 30 minutes using the high-speed disperser, and dispersed each component.
- AEROSIL 380 average particle diameter of 50 nm: manufactured by Nippon Aerosil Co., Ltd.
- Tetradecane was added as a diluting solvent to the kneaded product so that the viscosity was adjusted to a specified viscosity (10 to 11 Pa ⁇ s).
- the maximum normal force value of the obtained inorganic particle dispersion was 2.6 Pa.
- the inorganic particle dispersion had high spinnability even when other components such as a leveling agent were not blended.
- the inorganic particle dispersion obtained in this example was applied on the substrate so as to stretch the coating solution using a flat nozzle type dispenser, but high-speed and high-precision coating could be realized. It was.
- Example 3 The hydrophilic fumed silica (AEROSIL 380: average particle size 50 nm: manufactured by Nippon Aerosil Co., Ltd.) used in Example 1 was changed to hydrophilic fumed silica (AEROSIL 50: average particle size 30 nm: manufactured by Nippon Aerosil Co., Ltd.). Except that, an inorganic particle dispersion was obtained in the same manner as in Example 1.
- AEROSIL 380 average particle size 50 nm: manufactured by Nippon Aerosil Co., Ltd.
- the maximum normal force value was 2.5 Pa, which was about the same as the inorganic particle dispersion obtained in Example 1.
- Example 4 An inorganic particle dispersion of Example 4 was obtained in the same manner as in Example 1 except that the hydrogenated polybutadiene (GI-3000) used in Example 1 was not blended.
- GI-3000 hydrogenated polybutadiene
- the maximum normal force value was 2.2 Pa, which was a little smaller than the inorganic particle dispersion obtained in Example 1, but was a sufficient value. .
- Comparative Example 1 Inorganic particle dispersion of Comparative Example 1 by the same method as in Example 1 except that the hydrophilic fumed silica (AEROSIL 380: average particle size 50 nm: manufactured by Nippon Aerosil Co., Ltd.) in Example 1 was not blended. Got.
- AEROSIL 380 average particle size 50 nm: manufactured by Nippon Aerosil Co., Ltd.
- the normal force value of the obtained inorganic particle dispersion was measured, the normal force value was 1.6 Pa, and it was found that the spinnability was small as compared with the inorganic particle dispersions obtained in Examples 1 to 4. It was.
- the inorganic particle dispersion obtained in Comparative Example 1 was applied on the substrate so as to stretch the coating solution using a flat nozzle type dispenser, but could not be applied to the thin film at high speed. It was.
- Comparative Example 2 As another comparative example, hydrophilic fumed silica (AEROSIL 380: average particle size 50 nm: manufactured by Nippon Aerosil Co., Ltd.) in Example 1 was used as hydrophobic fumed silica (R805: average particle size 60 nm: manufactured by Nippon Aerosil Co., Ltd.). The inorganic particle dispersion of Comparative Example 2 was obtained in the same manner as in Example 1, except that the change was changed to).
- AEROSIL 380 average particle size 50 nm: manufactured by Nippon Aerosil Co., Ltd.
- R805 average particle size 60 nm: manufactured by Nippon Aerosil Co., Ltd.
- the inorganic particle dispersion obtained in Comparative Example 2 was applied on the substrate so as to stretch the coating solution using a flat nozzle type dispenser, but could not be applied to the thin film at high speed. It was.
- Comparative Example 3 As another comparative example, the modified acrylic resin (DHM-63-20HC: manufactured by Harima Chemicals Co., Ltd.) in Example 1 was used as a resin not containing a hydroxyl group, polyisoprene LIR-50 (manufactured by Kuraray), polybutadiene LBR-305 ( An inorganic particle dispersion of Comparative Example 3 was obtained in the same manner as in Example 1, except that the product was changed to Kuraray Co., Ltd. or polymethyl methacrylate, Epester MA1002 (manufactured by Nippon Shokubai Co., Ltd.).
- the normal force value of the obtained inorganic particle dispersion was measured, the normal force value was 1.0 Pa or less, and the spinnability was remarkably small as compared with the inorganic particle dispersions obtained in Examples 1 to 4. I understood.
- the inorganic particle dispersion obtained in Comparative Example 3 was applied on the substrate so as to stretch the coating solution using a flat nozzle type dispenser, but could not be applied to the thin film at high speed. It was.
- FIG. 1 is a diagram for explaining the spinnability of the inorganic particle dispersion according to this embodiment.
- the left inorganic particle dispersion in FIG. 1 is the inorganic particle dispersion according to Example 1, and the right inorganic particle dispersion is the inorganic particle dispersion according to Comparative Example 1.
- Example 1 the inorganic particle dispersion according to Example 1 is superior in the spinnability as compared with the inorganic particle dispersion according to Comparative Example 1.
- the inorganic particle dispersion obtained in each Example could be uniformly applied to the entire circumference without being uncoated with a thin film having a coating thickness of 240 ⁇ m on the base material.
- the inorganic particle dispersions obtained in the respective comparative examples were interrupted during application and applied in spots. It was confirmed that the inorganic particle dispersion obtained in the comparative example can be uniformly applied by increasing the discharge speed to 40 mm / s. However, in this case, the coating amount is 0.36 g and the coating film thickness is 0.6 mm, and the amount of the coating solution applied is greatly increased, so that thin film coating on the substrate is impossible.
- a flat nozzle having a slit width of 0.6 mm and a width of 25 mm is used on the outer surface of a cylindrical base material having an outer diameter of ⁇ 1 cm and a length of 30 mm having a plurality of groove-shaped irregularities on the outer peripheral portion in the circumferential direction.
- the inorganic particle dispersion 0.14 g obtained in the above was applied in 0.4 seconds.
- variety into the shape which follows the shape of a base-material outer peripheral side surface.
- the flat nozzle is kept 0.6 mm above the side surface of the substrate (clearance 0.6 mm), the substrate is rotated in the circumferential direction at a rotation speed of 150 rpm (application speed 79 mm / s), and discharged from the flat nozzle. It apply
- the inorganic particle dispersion obtained in each Example could be uniformly applied to the entire circumference without being uncoated with a thin film having a coating thickness of 240 ⁇ m on the base material.
- FIG. 2 and 3 show an example of a coating film applied using the inorganic particle dispersion according to this embodiment.
- 2 is a coating film using the inorganic particle dispersion according to Example 1
- FIG. 3 is a coating film using the inorganic particle dispersion according to Example 2.
- the coating film shown in FIG. 2 shows that the surface of the coating film shown in FIG. 2 is uniform as compared with the coating film shown in FIG. Further, the coating film shown in FIG. 3 has coating film defects such as pinholes on the surface. Since the inorganic particle dispersion according to Example 1 includes a leveling agent, the leveling property is high. For this reason, coating defects such as coating marks and pinholes that occur during coating can be compensated for by the leveling of the inorganic particle dispersion. As a result, it is considered that a uniform coating film was obtained.
- the inorganic particle dispersion according to this embodiment preferably contains a leveling agent.
- FIG. 4 the figure for demonstrating the printability of the coating film apply
- the left figure in FIG. 4 printed predetermined characters (letters E, N, and S) on the dried film of the coating film obtained using the inorganic particle dispersion according to Example 1 (overpainted).
- the right figure in FIG. 4 shows a predetermined character printed on the dried film of the coating film obtained using the inorganic particle dispersion according to Example 2.
- the inorganic particle dispersion according to this embodiment preferably contains an additive having high solvent absorbability.
- FIG. 5 the figure for demonstrating the effect of the glass component regulator in the inorganic particle dispersion which concerns on this embodiment is shown.
- the left figure and the middle figure in FIG. 5 print a predetermined character (letters E, N, and S) on the dried film of the coating film obtained using the inorganic particle dispersion according to Example 2 (upper picture).
- the right figure in FIG. 5 shows the result of firing after printing predetermined characters on the dried film of the coating film obtained using the inorganic particle dispersion according to Example 1. It is.
- the inorganic particle dispersion according to this embodiment preferably includes a component modifier such as kaolin when glass powder is used as the inorganic particles.
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Abstract
Description
本実施形態に係る無機粒子分散体は、少なくとも無機粉末、親水性フュームドシリカ及び水酸基を有する樹脂を有する。また、本実施形態に係る無機粒子分散体は、特性を向上させるための、その他の有機成分を含んでいてもよい。
本実施形態に係る無機粒子分散体に含まれる無機粉末としては、特に限定されないが、例えばガラス粉や、金粉、銀粉、銅粉、鉄粉、ステンレス粉、チタン粉、ニッケル粉、クロム粉、タングステン粉、モリブデン粉等の金属粉が挙げられる。
親水性フュームドシリカは、四塩化珪素を出発原料として、火炎中酸化・脱塩・精製などの工程を経て得られる乾式シリカの一種である。
水酸基を有する樹脂としては、特に限定されないが、得られる無機粒子分散体の曳糸性を向上させるために、高い弾性を有する樹脂を使用することが好ましい。具体的には、水酸基を有する変性アクリル樹脂、エポキシ樹脂、ウレタン樹脂、フェノール樹脂、エチルセルロース、ブチラール樹脂(ブチラール樹脂は、生産工程上、水酸基が残存する)、ゼラチン樹脂、等を好ましく使用することができる。なお、これらの樹脂は、水酸基を有するように変性させた樹脂を使用してもよい。
本実施形態に係る無機粒子分散体は、塗布液の特性を向上させるための、その他の成分を含んでいてもよい。その他の成分としては、無機粒子の分散性を向上させるための分散剤、レベリング性を向上させるためのレベリング剤、塗布液の粘度を調整するための有機溶媒、曳糸性を向上させるための各種添加剤、等が挙げられる。
本実施形態に係る無機粒子分散体は、分散体中に粒子を安定的に分散させるために、末端に官能基などを有する分散剤を含んでいてもよい。分散剤の含有量は、0.1~5質量%とすると好ましい。分散剤を含むことにより、分散剤の官能基を粒子の表面に配位させて粒子同士の接近を阻害することで粒子の再凝集を抑制し、粒子の分散性を向上させることができる。
本実施形態に係る無機粒子分散体は、消泡やレベリング性改良のために、レベリング剤を含んでいてもよい。レベリング剤の含有量は、0.1~5質量%とすると好ましい。レベリング剤は、塗布筋、クレーター、ピンホールなど、塗膜表面に生じる障害に対し、無機粒子分散体の接触角や表面張力を下げることにより濡れ性を向上させると共に、レベリング剤が塗膜表面に配向することで、無機粒子分散体を拡張する役割を果たす。
本実施形態に係る無機粒子分散体は、曳糸性の向上のために、その他の樹脂成分を含んでいてもよい。その他の樹脂成分の含有量は、1~10質量%とすると好ましい。その他の樹脂成分としては、高い弾性率を有する樹脂であることが好ましく、例えば、上記説明した水酸基を有する樹脂、水酸基を有さないアクリル樹脂、ポリブタジエンゴム、ポリイソプレンゴム、ブチルゴム、ウレタンゴム等が挙げられる。また、これらの樹脂は、水素添加した樹脂を使用してもよい。
本実施形態に係る無機粒子分散体は、塗布液の粘度を調整するための有機溶媒を含んでいてもよい。有機溶媒の含有量は、10~50質量%とすると好ましい。好ましい有機溶媒としては、トルエン、キシレン、シクロヘキサン、オクタン、ブタン、ドデカン、テトラデカンなどの炭化水素系溶媒が挙げられる。また、使用した樹脂の種類によっては、ケトン系有機溶媒を使用してもよい。ケトン系有機溶媒として、アセトン、メチルエチルケトン、メチルイソブチルケトン、ジイソブチルケトン、イソホロン、シクロヘキサノンなどが挙げられる。
本実施形態に係る無機粒子分散体は、求められる特性に応じて、その他の添加剤を含んでいてもよい。その他の添加剤の含有量は、0.1~5質量%とすると好ましい。
上記説明した材料を用いて、本実施形態に係る無機粒子分散体を製造する方法について、説明する。
本実施形態に係る無機粒子分散体は、高い曳糸性を有する。そのため、せん断応力を加えた場合であっても切れにくく、せん断応力がかかる種々の塗布方法に適用した場合であっても、高速で高精度の塗布を実現できる。
高速分散機に、水酸基を有する樹脂として変性アクリル樹脂(DHM-63-20HC:ハリマ化成株式会社製)を157g、親水性フュームドシリカ(AEROSIL 380:平均粒子径50nm:日本アエロジル株式会社製)を0.5g、インクの吸収成分としてフュームドアルミナ(SpectrAl 100:商品コードFA-100)を7g、分散剤としてノイゲン(ET-89)を5g、ガラスの成分調整剤として仮焼カオリン(PoleStar 400)を19.5g、フィラーの沈降防止剤(TIXOGEL-EZ 100)を10g、レベリング剤(BYK-392)を5g入れた。そして、高速分散機を用いて1500rpmで30分攪拌して、各成分を分散させた。
高速分散機に、水酸基を有する樹脂として変性アクリル樹脂(DHM-63-20HC:ハリマ化成株式会社製)を157g、親水性フュームドシリカ(AEROSIL 380:平均粒子径50nm:日本アエロジル株式会社製)を0.5g、分散剤としてノイゲン(ET-89)を5g入れた。そして、高速分散機を用いて1500rpmで30分攪拌して、各成分を分散させた。
実施例1で使用した親水性フュームドシリカ(AEROSIL 380:平均粒子径50nm:日本アエロジル株式会社製)を、親水性フュームドシリカ(AEROSIL 50:平均粒子径30nm:日本アエロジル株式会社製)に変更した以外には実施例1と同様の方法により、無機粒子分散体を得た。
実施例1で使用した水素添加ポリブタジエン(GI-3000)を配合しなかった以外は、実施例1と同様の方法により、実施例4の無機粒子分散体を得た。
実施例1における、親水性フュームドシリカ(AEROSIL 380:平均粒子径50nm:日本アエロジル株式会社製)を配合しなかった以外は、実施例1と同様の方法により、比較例1の無機粒子分散体を得た。
別の比較例として、実施例1における、親水性フュームドシリカ(AEROSIL 380:平均粒子径50nm:日本アエロジル株式会社製)を疎水性フュームドシリカ(R805:平均粒子径60nm:日本アエロジル株式会社製)に変更した以外は、実施例1と同様の方法により、比較例2の無機粒子分散体を得た。
別の比較例として、実施例1における、変性アクリル樹脂(DHM-63-20HC:ハリマ化成株式会社製)を、水酸基を含まない樹脂としてポリイソプレンLIR-50(クラレ製)、ポリブタジエンLBR-305(クラレ製)又はポリメタクリル酸メチル エポスターMA1002(日本触媒社製)に変更した以外は、実施例1と同様の方法により、比較例3の無機粒子分散体を得た。
実施例1の無機粒子分散体と比較例1の無機粒子分散体との間の曳糸性の差を明確にするために、各々の無機粒子分散体を同じ力で引き上げた際の曳糸性について図1を参照して説明する。
外径φ1cm長さ30mmの円筒形基材の外側面に対して、スリット幅0.6mmで幅25mmの平ノズルを用い、各実施例及び各比較例で得られた無機粒子分散体0.14gを0.4秒で塗布した。より具体的には、平ノズルを基材側面上方0.6~1.2mm(クリアランス0.6~1.2mm)に保ち、基材を周方向に回転速度150rpm(塗布速度79mm/s)で回転させ、平ノズルからの吐出速度15.6mm/sで0.4秒吐出することで基材上に塗布した。
外周部に周方向に向かう複数の溝状凹凸を持つ外径φ1cm長さ30mmの円筒形基材の外側面に対して、スリット幅0.6mmで幅25mmの平ノズルを用いて、各実施例で得られた無機粒子分散体0.14gを0.4秒で塗布した。なお、平ノズルは、基材外周側面の形状に沿う形状にノズル口およびスリット幅を加工したものを用いた。より具体的には、平ノズルを基材側面上方0.6mm(クリアランス0.6mm)に保ち、基材を周方向に回転速度150rpm(塗布速度79mm/s)で回転させ、平ノズルからの吐出速度15.6mm/sで0.4秒吐出することで基材上に塗布した。
図2及び図3に、本実施形態に係る無機粒子分散体を用いて塗布した塗膜の一例を示す。図2は、実施例1に係る無機粒子分散体を用いた塗膜であり、図3は、実施例2に係る無機粒子分散体を用いた塗膜である。
図4に、本実施形態に係る無機粒子分散体を用いて塗布した塗膜の印字性を説明するための図を示す。図4における左図は、実施例1に係る無機粒子分散体を用いて得られた塗膜の乾燥膜上に、所定の文字(E、N及びSの文字)を印字(上絵付け)したものであり、図4における右図は、実施例2に係る無機粒子分散体を用いて得られた塗膜の乾燥膜上に、所定の文字を印字したものである。
図5に、本実施形態に係る無機粒子分散体における、ガラスの成分調整剤の効果を説明するための図を示す。図5における左図及び中図は、実施例2に係る無機粒子分散体を用いて得られた塗膜の乾燥膜上に、所定の文字(E、N及びSの文字)を印字(上絵付け)した後に焼成したものであり、図5における右図は、実施例1に係る無機粒子分散体を用いて得られた塗膜の乾燥膜上に、所定の文字を印字した後に焼成したものである。
Claims (9)
- 無機粉末、
親水性フュームドシリカ、及び
水酸基を有する樹脂、
を有する、無機粒子分散体。 - 前記水酸基を有する樹脂は、水酸基を有する変性アクリル樹脂、エポキシ樹脂、ウレタン樹脂、フェノール樹脂、エチルセルロース、ブチラール樹脂又はゼラチン樹脂を含む、
請求項1に記載の無機粒子分散体。 - 前記無機粉末は、ガラス粉、金粉、銀粉、銅粉、鉄粉、ステンレス粉、チタン粉、ニッケル粉、クロム粉、タングステン粉又はモリブデン粉を含む、
請求項1に記載の無機粒子分散体。 - 前記無機粒子分散体は更に、分散剤を含む、
請求項1に記載の無機粒子分散体。 - 前記無機粒子分散体は更に、レベリング剤を含む、
請求項1に記載の無機粒子分散体。 - 前記無機粒子分散体は更に、アクリル樹脂、ポリブタジエンゴム、ポリイソプレンゴム、ブチルゴム又はウレタンゴムを含む、
請求項1に記載の無機粒子分散体。 - 前記無機粉末はガラス粉であり、
前記無機粒子分散体は更に、前記ガラス粉の成分調整剤を含む、
請求項1に記載の無機粒子分散体。 - 前記無機粒子分散体は更に、前記無機粒子分散体の粘度を調整するための有機溶媒を含む、
請求項1に記載の無機粒子分散体。 - 少なくとも親水性フュームドシリカ及び水酸基を有する樹脂を、所定の量で混合して攪拌する第1工程と、
前記第1工程で得られた混練物に所定の量の無機粉末を加え、攪拌する第2工程と、
前記第2工程で得られた混練物をろ過する第3工程と、
を含む、無機粒子分散体の製造方法。
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US20200062989A1 (en) | 2020-02-27 |
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CN110461949A (zh) | 2019-11-15 |
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