Viscosity adjustment method and particle dispersion liquid production method
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Filing Date
- 2024-10-10
- Publication Date
- 2025-05-01
Abstract
Description
Viscosity adjusting method and particle dispersion manufacturing method
[0001] The present disclosure relates to a method for adjusting viscosity, a method for producing a particle dispersion, and the like.
[0002] Particle dispersions containing particles dispersed in a liquid medium are used to produce various industrial components. For example, Patent Document 1 below describes a particle dispersion using silica particles.
[0003] Special Publication No. 2015-519442
[0004] When particles and a liquid medium are mixed to obtain a particle dispersion, it may be necessary to adjust the viscosity of the particle dispersion relative to the viscosity of the liquid medium before mixing with the particles. According to the findings of the present inventors, although the viscosity of the liquid medium before mixing with the particles is low, the viscosity of the particle dispersion obtained by mixing the liquid medium with the particles may be high. In this case, for example, if the viscosity of the particle dispersion obtained by selecting a liquid medium to be used in the production of an industrial component and then mixing the particles with the liquid medium is unexpectedly high, it may be difficult to achieve sufficient workability. Therefore, a method for adjusting the relative viscosity of the particle dispersion and the viscosity of the liquid medium is required.
[0005] An object of one aspect of the present disclosure is to provide a viscosity adjusting method capable of adjusting the relative relationship between the viscosity of a particle dispersion containing particles and a liquid medium and the viscosity of the liquid medium.Another object of the present disclosure is to provide a method for producing a particle dispersion containing particles and a liquid medium, which is capable of obtaining a particle dispersion in which the relative relationship between the viscosity of the particle dispersion and the viscosity of the liquid medium is adjusted.
[0006] The present inventors have found that adjusting the distance between the HSP value of the particles and the HSP value of the liquid medium is effective in adjusting the relative relationship between the viscosity of the particle dispersion and the viscosity of the liquid medium.
[0007] In some aspects, the present disclosure relates to the following [1] to
[10] , etc. [1] A method for adjusting viscosity, which adjusts the relative relationship between the viscosity of a particle dispersion containing particles and a liquid medium and the viscosity of the liquid medium based on the distance between the HSP value of the particles and the HSP value of the liquid medium. [2] The method for adjusting viscosity according to [1], wherein the liquid medium contains methyl isobutyl ketone. [3] The method for adjusting viscosity according to [1] or [2], wherein the liquid medium contains methyl ethyl ketone. [4] The method for adjusting viscosity according to any one of [1] to [3], wherein the liquid medium contains an organic solvent, and the content of the organic solvent is 80 mass% or more based on the total mass of the liquid medium. [5] The method for adjusting viscosity according to any one of [1] to [4], wherein the particles contain silica. [6] A method for producing a particle dispersion, comprising: a step of selecting the particles and the liquid medium based on the distance between the HSP value of the particles and the HSP value of the liquid medium; and a step of mixing the particles and the liquid medium. [7] The method for producing a particle dispersion liquid according to [6], wherein the liquid medium contains methyl isobutyl ketone. [8] The method for producing a particle dispersion liquid according to [6] or [7], wherein the liquid medium contains methyl ethyl ketone. [9] The method for producing a particle dispersion liquid according to any one of [6] to [8], wherein the liquid medium contains an organic solvent, and the content of the organic solvent is 80 mass % or more based on the total mass of the liquid medium.
[10] The method for producing a particle dispersion liquid according to any one of [6] to [9], wherein the particles contain silica.
[0008] According to one aspect of the present disclosure, there is provided a viscosity adjustment method that can adjust the relative relationship between the viscosity of a particle dispersion containing particles and a liquid medium and the viscosity of the liquid medium. According to another aspect of the present disclosure, there is provided a method for producing a particle dispersion containing particles and a liquid medium, which can obtain a particle dispersion in which the relative relationship between the viscosity of the particle dispersion and the viscosity of the liquid medium is adjusted.
[0009] Hereinafter, embodiments of the present disclosure will be described, but the present disclosure is not limited to these embodiments in any way.
[0010] In this specification, numerical ranges indicated using "to" indicate a range that includes the numerical values before and after "to" as the minimum and maximum values, respectively. A numerical range "A or greater" means a range exceeding A and A. A numerical range "A or less" means a range less than A and A. In numerical ranges described in stages in this specification, the upper or lower limit of a numerical range in a certain stage can be arbitrarily combined with the upper or lower limit of a numerical range in another stage. In numerical ranges described in this specification, the upper or lower limit of the numerical range may be replaced with a value shown in an experimental example. "A or B" may include either A or B, or may include both. Unless otherwise specified, the materials exemplified in this specification can be used alone or in combination of two or more. When multiple substances corresponding to each component are present in the composition, the content of each component in the composition refers to the total amount of the multiple substances present in the composition, unless otherwise specified. The term "process" includes not only an independent process but also a process that cannot be clearly distinguished from other processes as long as the intended effect of the process is achieved. "Solid content" refers to non-volatile content excluding volatile components that can volatilize (water, organic solvents, etc.).
[0011] The viscosity adjustment method according to this embodiment includes an adjustment step of adjusting the relative relationship between the viscosity of a particle dispersion containing particles and a liquid medium and the viscosity of the liquid medium based on the distance between the HSP value of the particles and the HSP value of the liquid medium (hereinafter sometimes referred to as the "HSP distance of the particles to the liquid medium"). The viscosity adjustment method according to this embodiment provides a new method for adjusting the relative relationship of viscosities, by adjusting the relative relationship between the viscosity of the particle dispersion and the viscosity of the liquid medium. In the adjustment step, the viscosity ratio of the particle dispersion to the liquid medium (hereinafter sometimes simply referred to as the "viscosity ratio") may be adjusted.
[0012] The method for producing a particle dispersion according to this embodiment includes a selection step of selecting particles and a liquid medium based on the HSP distance of the particles relative to the liquid medium, and a mixing step of mixing the particles and the liquid medium (the particles and liquid medium selected in the selection step). In the method for producing a particle dispersion according to this embodiment, the relative relationship between the viscosity of the particle dispersion and the viscosity of the liquid medium can be adjusted by selecting the particles and the liquid medium based on the HSP distance of the particles relative to the liquid medium. In the selection step, particles may be selected based on the type of material, particle size, particle size distribution (coefficient of variation of particle size), surface treatment details (type of surface treatment agent, amount of surface treatment agent used, surface treatment method, etc.), and the liquid medium may be selected based on the type of material of the dispersion medium constituting the liquid medium, the content of the dispersion medium, etc.
[0013] The particle dispersion according to this embodiment contains particles and a liquid medium. The particle dispersion according to this embodiment can be obtained by mixing the particles and the liquid medium together, and is, for example, a particle dispersion obtained by the method for producing a particle dispersion according to this embodiment.
[0014] The use of the viscosity adjusting method, particle dispersion, and its manufacturing method according to this embodiment is not particularly limited. The viscosity adjusting method, particle dispersion, and its manufacturing method according to this embodiment can be applied to the manufacture or use of laminates (copper-clad laminates, etc.), die bonding films, circuit connecting members, polishing liquids (CMP polishing liquids, etc.), encapsulants, battery electrode active materials, transfer-type transparent conductive films, etc. For example, the viscosity adjusting method, particle dispersion, and its manufacturing method according to this embodiment can be used in the manufacture of semiconductor members, and the particle dispersion according to this embodiment can be used as a slurry for obtaining semiconductor member laminates, insulating films (insulating films of encapsulants, etc.), etc.
[0015] The HSP distance of a particle to a liquid medium is expressed as δ in the Hansen solubility parameter (HSP). d (dispersion term), δ p (polarization term) and δ h (hydrogen bond term), it can be calculated from the following formula: δ d1 , δ p1 and δ h1 is the particle's δ d , δ p and δ hand δ d2 , δ p2 and δ h2 is the δ of the liquid medium d , δ p and δ h HSP distance = {4 × (δ d1 -δ d2 ) 2 + (δ p1 -δ p2 ) 2 + (δ h1 -δ h2 ) 2} 0.5
[0016] δ of commonly used substances d , δ p and δ h Since there are publicly known information sources such as databases, for example, the δ of a desired substance can be obtained by referring to the database. d , δ p and δ h Parameters for substances not registered in the database can be calculated using computer software such as HSPiP (Hansen Solubility Parameter in Practice; written by Prof. Steven Abbott and Dr. Yamamoto Hiroshi).
[0017] δ of the particle d1 , δ p1 and δ h1 can be calculated by the following procedure. First, the particles are recovered by drying the particle dispersion liquid, and the parameter (δ d , δ p and δ h ) are prepared. Next, a dispersibility test of the particles to be evaluated in each of the evaluation solvents is carried out, and it is determined whether each evaluation solvent is a "solvent with excellent dispersibility" or a "solvent with poor dispersibility." The dispersibility test can be carried out by the method shown in the experimental example described later. Next, δ d , δ p and δ hAfter plotting each evaluation solvent in a three-dimensional space (Hansen space) with the coordinate axes, a virtual sphere is created in the three-dimensional space that encompasses all of the "solvents with excellent dispersibility" without encompassing all of the "solvents with poor dispersibility." Then, δ at the center of the sphere is calculated. d , δ p and δ h the particle's δ d1 , δ p1 and δ h1 can be obtained as:
[0018] δ d1 , δ p1 and δ h1 varies depending on the type of material, particle size, particle size distribution (coefficient of variation of particle size), surface treatment details (type of surface treatment agent, amount of surface treatment agent used, surface treatment method, etc.). For example, the larger the particle size, the d1 tends to increase, and δ p1 and δ h1 The larger the coefficient of variation of particle size, the greater the δ p1 tends to increase, and δ h1 The δ of particles after surface treatment tends to decrease. d1 , δ p1 and δ h1 is for the entire particle after surface treatment, taking into account the effect of the surface treatment. d1 , δ p1 and δ h1 The values at 25°C can be used.
[0019] δ of the liquid medium d2 , δ p2 and δ h2 can be calculated based on the composition of the liquid medium in the particle dispersion. When the liquid medium is a mixture of multiple dispersion media, δ d2 , δ p2 and δ h2 is the parameter of each dispersion medium (δ d , δ p or δ h ) and the volume ratio of each dispersion medium to the entire mixture. d , δ p and δ hThe parameters (δ) of components not registered in the database can be calculated using the values in the database of the analytical software HSPiP (Hansen Solubility Parameter in Practice; written by Prof. Steven Abbott and Dr. Yamamoto Hiroshi). d , δ p and δ h ) may be calculated using structural analysis software called SMILES. d2 , δ p2 and δ h2 The values at 25°C can be used.
[0020] The present inventors have found that adjusting the HSP distance of particles relative to a liquid medium is effective in adjusting the viscosity ratio of a particle dispersion relative to the liquid medium, and that reducing the HSP distance of particles relative to a liquid medium is effective in reducing the viscosity ratio of a particle dispersion relative to the liquid medium. It is presumed that the reason for this tendency is that reducing the HSP distance of particles relative to a liquid medium increases the dispersibility of the particles in the liquid medium, thereby increasing the distance between particles, thereby weakening the interaction between particles and allowing the viscosity ratio of a particle dispersion relative to the liquid medium to be reduced. However, the reasons for the aforementioned tendency are not limited to the above.
[0021] The viscosity of the liquid medium to be compared with the viscosity of the particle dispersion is the viscosity (25°C, shear rate 1 min) listed in the Compact Solvent Pocket Book, 1st Edition, edited by the Society of Organic Synthetic Chemistry (1994). -1 ) can be used, and viscosity not listed is measured at 25°C and a shear rate of 1 min using an E-type viscometer. -1 It can be measured.
[0022] In the viscosity adjusting method, particle dispersion, and manufacturing method thereof according to the present embodiment, the viscosity ratio of the particle dispersion to the liquid medium can be adjusted by adjusting the solid content of the particle dispersion based on the relationship between the viscosity and the solid content of the particle dispersion. Specifically, the solid content of the particle dispersion is adjusted to achieve a boundary state between a non-Bingham fluid and a dilatancy fluid, and the viscosity of the particle dispersion having such a solid content (viscosity in the non-Bingham fluid state) can be used. In the case of a non-Bingham fluid, the viscosity does not increase with increasing viscometer rotation speed (shear rate; the same applies hereinafter), whereas in the case of a dilatancy fluid, the viscosity increases rapidly with increasing viscometer rotation speed. To determine the boundary state between a non-Bingham fluid and a dilatancy fluid, the solid content of the particle dispersion is changed by 5% by mass increments, and the viscosity behavior with respect to the viscometer rotation speed is confirmed. The solid content that exhibits non-Bingham fluid behavior (behavior in which the viscosity does not increase with increasing viscometer rotation speed) can be used as the solid content of the particle dispersion for comparing viscosity with that of the liquid medium. By comparing the viscosity in terms of the solid content in this way, it is easy to determine the difference in the viscosity ratio of the particle dispersion to the liquid medium, and the viscosity ratio can be suitably evaluated. The solid content of the particle dispersion may be adjusted by diluting it with a liquid medium having the same composition as the liquid medium of the particle dispersion, or by volatilizing the liquid medium of the particle dispersion.
[0023] When a particle dispersion contains components other than the particles and the liquid medium (excluding the surface treatment agent for the particles), the viscosity ratio of the particle dispersion to the liquid medium in a state in which the components other than the particles and the liquid medium (excluding the surface treatment agent for the particles) have been removed can be adjusted according to the viscosity adjustment method, particle dispersion, and method for producing the same according to this embodiment. When a particle dispersion contains components other than the particles and the liquid medium (excluding the surface treatment agent for the particles), the viscosity of the particle dispersion in a state in which the components have been removed can be measured as the viscosity of the particle dispersion.
[0024] In the adjusting step of the viscosity adjusting method according to this embodiment, the HSP distance (unit: MPa) of the particles relative to the liquid medium 0.5 In the selection step of the method for producing a particle dispersion according to this embodiment, the HSP distance (unit: MPa) of the particles relative to the liquid medium may be adjusted to the following range.0.5 In the particle dispersion according to this embodiment, the particles and the liquid medium may be selected such that the HSP distance (unit: MPa) of the particles relative to the liquid medium is in the following range. 0.5) may be in the following ranges. From the viewpoint of facilitating a reduction in the viscosity ratio, the HSP distance of the particles to the liquid medium may be 20.0 or less, 19.0 or less, 18.0 or less, 17.0 or less, 16.0 or less, 15.0 or less, 14.8 or less, 14.6 or less, 14.5 or less, 14.4 or less, 14.2 or less, 14.0 or less, 13.8 or less, 13.6 or less, 13.5 or less, 13.4 or less, 13.2 or less, 13.0 or less, 12.5 or less, 12.0 or less, 11.0 or less, 12.5 or less, 13.0 or less, 14.8 or less, 14.6 or less, 14.5 or less, 14.4 or less, 14.2 or less, 14.0 or less, 13.8 or less, 13.6 or less, 13.5 or less, 13.4 or less, 13.2 or less, 13.0 or less, 12.5 or less, 12.0 or less, 11.0 or less, 12.5 or less, 12.0 or less, 13 ... .8 or less, 11.6 or less, 11.5 or less, 11.4 or less, 11.2 or less, 11.0 or less, 10.8 or less, 10.6 or less, 10.5 or less, 10.4 or less, 10.2 or less, 10.0 or less, 9.8 or less, 9.5 or less, 9.0 or less, 8.5 or less, 8.2 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, 5.5 or less, 5.0 or less, 4.8 or less, or 4.6 or less. From the viewpoint of adjusting the viscosity ratio, the HSP distance of the particles to the liquid medium is greater than 0.0, 0.5 or more, 1.0 or more, 1.5 or more, 2.0 or more, 2.5 or more, 3.0 or more, 3.5 or more, 4.0 or more, 4.5 or more, 4.6 or more, 4.8 or more, 5.0 or more, 5.5 or more, greater than 5.5, 6.0 or more, 6.5 or more, 7.0 or more, greater than 7.1, 7.5 or more, 8.0 or more, 8.2 or more, 8.5 or more, 9.0 or more, 9.5 or more, 9.8 or more, 10.0 or more, 10.2 or more, 10.4 or more , 10.5 or more, 10.6 or more, 10.8 or more, 11.0 or more, 11.2 or more, 11.4 or more, 11.5 or more, 11.6 or more, 11.8 or more, 12.0 or more, 12.5 or more, 13.0 or more, 13.2 or more, 13.4 or more, 13.5 or more, 13.6 or more, 13.8 or more, 14.0 or more, 14.2 or more, 14.4 or more, 14.5 or more, 14.6 or more, 15.0 or more, more than 15.0, 16.0 or more, 17.0 or more, 18.0 or more, or 19.0 or more. From these viewpoints, the HSP distance of the particle relative to the liquid medium may be greater than 0.0 and less than 20.0, greater than 0.0 and less than 15.0, greater than 0.0 and less than 12.0, greater than 0.0 and less than 10.0, 7.5 to 20.0, 7.5 to 15.0, 7.5 to 12.0, 7.5 to 10.0, 9.0 to 20.0, 9.0 to 15.0, 9.0 to 12.0, or 9.0 to 10.0.
[0025] In the particle dispersion, at least a portion of the particles may be dispersed in a liquid medium. The particles constitute the solid content of the particle dispersion. The particles may include inorganic particles or organic particles.
[0026] Examples of materials constituting inorganic particles include oxides such as silica, ceria, alumina, titania, zirconia, magnesia, yttria, zinc oxide, and iron oxide; nitrides such as silicon nitride, titanium nitride, and boron nitride; hydroxides such as cerium hydroxide; metal materials such as copper, nickel, gold, silver, tin, zinc, platinum, bismuth, indium, and antimony; silicon carbide; calcium carbonate; aluminum sulfate; barium sulfate; potassium titanate; barium titanate; and calcium titanate. Inorganic particles may be prepared by a melting method, a sol-gel method, a liquid-phase method, or the like. Examples of materials constituting organic particles include resin materials, such as acrylic resin, styrene resin, urea resin, phenolic resin, epoxy resin, and benzoguanamine resin. The particle materials may be used alone or in combination of two or more. From the viewpoint of easily reducing the viscosity ratio and easily obtaining excellent dispersibility of the particles, the particles may contain inorganic particles, may contain a non-metallic material, may contain at least one selected from the group consisting of silica, ceria, alumina, titania, boron nitride, and calcium titanate, may contain at least one selected from the group consisting of silica and alumina, or may contain silica.
[0027] The particles may or may not be surface-treated. Surface-treated particles may have a surface treatment agent on the surface of the particles. The surface treatment method may be a dry treatment or a wet treatment.
[0028] Examples of the surface treatment agent include a silane compound (e.g., a silane coupling agent), a titanium compound (e.g., a titanium coupling agent), an aluminate compound (e.g., an aluminate coupling agent), etc. The surface treatment agent may have an alkoxy group, an alkoxysilyl group, a phenyl group, a vinyl group, an epoxy group, an acryloyl group, a methacryloyl group, an amino group, a ureido group, a mercapto group, an isocyanate group, etc. From the viewpoint of easily obtaining excellent dispersibility of the particles, the surface treatment agent may contain a silane compound or a silane compound having an alkoxysilyl group.
[0029] From the viewpoint of easily obtaining excellent particle dispersibility, the silane compound may include a silane compound having an alkoxy group bonded to a silicon atom as a silane compound having an alkoxysilyl group. In the silane compound, from the viewpoint of easily obtaining excellent particle dispersibility, the number of alkoxy groups bonded to a silicon atom may be 1 to 4, 1 to 3, 2 to 3, or 3 to 4.
[0030] The silane compound may contain a silane compound having a nitrogen-containing organic group, from the viewpoint of easily obtaining excellent particle dispersibility. Examples of the nitrogen-containing organic group include an alkylamino group, an alkylaminoalkyl group, an arylamino group, an arylaminoalkyl group, a heteroarylamino group, and a heteroarylaminoalkyl group. From the viewpoint of easily obtaining excellent particle dispersibility, the nitrogen-containing organic group may contain an arylaminoalkyl group, a phenylaminoalkyl group, or a phenylaminopropyl group.
[0031] Examples of the silane compound include N-phenyl-3-aminopropyltrimethoxysilane, phenyltrimethoxysilane, vinyltrimethoxysilane, epoxytrimethoxysilane, methacryltrimethoxysilane, aminotrimethoxysilane, ureidotrimethoxysilane, mercaptopropyltrimethoxysilane, isocyanatepropyltrimethoxysilane, phenylaminotrimethoxysilane, acryltrimethoxysilane, p-styryltrimethoxysilane, 3-acryloxypropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-isocyanatepropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, etc. The silane compound may contain N-phenyl-3-aminopropyltrimethoxysilane, from the viewpoint of easily obtaining excellent dispersibility of particles.
[0032] From the viewpoint of easily obtaining excellent particle dispersibility, the content of the surface treatment agent may be in the following ranges relative to 100 parts by mass of the particles (not including the content of the surface treatment agent). The content of the surface treatment agent may be 0.01 parts by mass or more, 0.05 parts by mass or more, 0.1 parts by mass or more, 0.3 parts by mass or more, or 0.5 parts by mass or more. The content of the surface treatment agent may be 10 parts by mass or less, 8.0 parts by mass or less, 5.0 parts by mass or less, 3.0 parts by mass or less, 2.0 parts by mass or less, 1.5 parts by mass or less, 1.0 parts by mass or less, 0.8 parts by mass or less, or 0.5 parts by mass or less. From these viewpoints, the content of the surface treatment agent may be 0.01 to 10 parts by mass, 0.05 to 5.0 parts by mass, or 0.1 to 2.0 parts by mass.
[0033] Specific gravity of particles (unit: g / cm 3 ) may be in the following ranges from the viewpoint of adjusting the viscosity ratio or the dispersibility of the particles. The specific gravity of the particles may be 0.1 or more, 0.5 or more, 1.0 or more, 1.5 or more, or 2.0 or more. The specific gravity of the particles may be 8.0 or less, 7.0 or less, 6.0 or less, 5.0 or less, 4.0 or less, 3.0 or less, or 2.5 or less. From these viewpoints, the specific gravity of the particles may be 0.1 to 8.0, 1.0 to 8.0, or 1.0 to 5.0.
[0034] δ of the particle d1 (unit: MPa 0.5) may be in the following range from the viewpoint of adjusting the viscosity ratio or the dispersibility of the particles. d1 may be 8.0 or more, 9.0 or more, 10.0 or more, 10.5 or more, 11.0 or more, 11.5 or more, 12.0 or more, 12.5 or more, or 13.0 or more. d1 may be 25.0 or less, 22.0 or less, 20.0 or less, 19.5 or less, 19.0 or less, 18.5 or less, 18.0 or less, 17.5 or less, 17.0 or less, 16.5 or less, 16.0 or less, 15.5 or less, 15.0 or less, 14.5 or less, 14.0 or less, or 13.5 or less. d1 may be 8.0 to 25.0, 8.0 to 20.0, 8.0 to 15.0, 10.0 to 25.0, 10.0 to 20.0, 10.0 to 15.0, 12.0 to 25.0, 12.0 to 20.0, or 12.0 to 15.0.
[0035] δ of the particle p1 (unit: MPa 0.5 ) may be in the following range from the viewpoint of adjusting the viscosity ratio or the dispersibility of the particles. p1 may be 1.0 or more, 2.0 or more, 3.0 or more, 4.0 or more, 5.0 or more, 6.0 or more, 7.0 or more, 7.5 or more, 8.0 or more, 8.5 or more, 9.0 or more, 9.5 or more, 10.0 or more, 10.5 or more, 11.0 or more, or 11.5 or more. p1 may be 20.0 or less, 18.0 or less, 16.0 or less, 15.0 or less, 14.5 or less, 14.0 or less, 13.5 or less, 13.0 or less, 12.5 or less, or 12.0 or less. p1 may be 1.0 to 20.0, 1.0 to 15.0, 1.0 to 12.0, 8.0 to 20.0, 8.0 to 15.0, 8.0 to 12.0, 10.0 to 20.0, 10.0 to 15.0, or 10.0 to 12.0.
[0036] δ of the particle h1 (unit: MPa 0.5 ) may be in the following range from the viewpoint of adjusting the viscosity ratio or the dispersibility of the particles. h1may be 1.0 or more, 2.0 or more, 3.0 or more, 4.0 or more, 5.0 or more, 6.0 or more, 7.0 or more, 8.0 or more, 8.5 or more, 9.0 or more, 9.5 or more, 10.0 or more, 10.5 or more, 11.0 or more, 11.5 or more, 12.0 or more, 12.5 or more, or 13.0 or more. h1 may be 20.0 or less, 19.0 or less, 18.0 or less, 17.0 or less, 16.0 or less, 15.5 or less, 15.0 or less, 14.5 or less, 14.0 or less, or 13.5 or less. h1 may be 1.0 to 20.0, 1.0 to 18.0, 1.0 to 15.0, 8.0 to 20.0, 8.0 to 18.0, 8.0 to 15.0, 10.0 to 20.0, 10.0 to 18.0, or 10.0 to 15.0.
[0037] From the viewpoint of easily reducing the viscosity ratio and easily obtaining excellent dispersibility of the particles, the content of the inorganic particles (when the inorganic particles are surface-treated, the content of the surface treatment agent is not included) may be 50% by mass or more, more than 50% by mass, 70% by mass or more, 80% by mass or more, 90% by mass or more, 92% by mass or more, 95% by mass or more, 97% by mass or more, 98% by mass or more, 99% by mass or more, or substantially 100% by mass based on the total mass of the particles (the total amount of particles contained in the particle dispersion; when the particles are surface-treated, the content of the surface treatment agent is not included).
[0038] The particle content (in the case where the particles are surface-treated: including the content of the surface treatment agent), the particle content (in the case where the particles are surface-treated: excluding the content of the surface treatment agent), the inorganic particle content (in the case where the particles are surface-treated: including the content of the surface treatment agent), or the inorganic particle content (in the case where the particles are surface-treated: excluding the content of the surface treatment agent) may be in the following ranges based on the total mass of the particle dispersion, from the viewpoint of adjusting the viscosity ratio or the dispersibility of the particles: The content A1 may be 0.1% by mass or more, 0.5% by mass or more, 1% by mass or more, 5% by mass or more, 10% by mass or more, 15% by mass or more, 20% by mass or more, 25% by mass or more, 30% by mass or more, 35% by mass or more, 40% by mass or more, 45% by mass or more, 50% by mass or more, 55% by mass or more, 60% by mass or more, 65% by mass or more, or 70% by mass or more. The content A1 may be 99% by mass or less, 95% by mass or less, 90% by mass or less, 85% by mass or less, 80% by mass or less, 75% by mass or less, or 70% by mass or less. From these viewpoints, the content A1 may be 0.1 to 99% by mass, 0.1 to 90% by mass, 0.1 to 80% by mass, 5 to 99% by mass, 5 to 90% by mass, 5 to 80% by mass, 30 to 99% by mass, 30 to 90% by mass, or 30 to 80% by mass.
[0039] Examples of liquid media (dispersion media constituting the liquid medium) include organic solvents, water, and resin materials (for example, resin materials that are liquid at 25°C). Organic solvents are a general term for organic compounds that have the property of dissolving other substances, and are widely used in painting, cleaning, printing, and the like. The organic solvent may be liquid at 25°C. In the particle dispersion, only one of the organic solvent, water, and resin material may be used, or at least two of the organic solvent, water, and resin material may be used in combination. Each of the organic solvents and resin materials may be used alone or in combination of two or more.
[0040] Examples of organic solvents include ketone compounds (excluding compounds corresponding to alcohols) such as methyl isobutyl ketone (MIBK), methyl ethyl ketone (MEK), diisobutyl ketone, acetone, cyclohexanone, acetophenone, and benzophenone; aromatic hydrocarbon compounds such as benzene, toluene, xylene, styrene, and diethylbenzene; aliphatic hydrocarbon compounds such as pentane, hexane, heptane, octane, nonane, and decane; alicyclic hydrocarbon compounds such as cyclohexane, methylcyclohexane, and decahydronaphthalene; chlorinated hydrocarbon compounds such as chlorobenzene, dichlorobenzene, trichlorobenzene, methylene chloride, chloroform, carbon tetrachloride, and tetrachloroethylene; methanol, ethanol, 1-propanol (n-propyl alcohol), 2-propanol (isopropyl alcohol), propylene glycol 1-monomethyl ether, 1-butanol, 2-butanol, t-butanol, 1-pentanol, 2-pentanol, 3-pentanol, diethanolamine, and the like. ether compounds (excluding compounds corresponding to alcohols) such as dibenzyl ether, ethyl ether, ethylene glycol monomethyl ether, diethylene glycol monobutyl ether, anisole, phenyl ether, dioxane, and tetrahydrofuran; ester compounds such as ethyl acetate, butyl acetate, benzyl acetate, ethyl benzoate, benzyl benzoate, and γ-butyrolactone; nitrile compounds such as acetonitrile; sulfoxide compounds such as dimethyl sulfoxide, diethyl sulfoxide, dipropyl sulfoxide, and diphenyl sulfoxide; amide compounds such as formamide, N,N-dimethylacetamide, 1-methyl-2-pyrrolidone, and N-methyl-2-pyrrolidone; carbonate compounds such as ethylene carbonate and propylene carbonate; and acid anhydrides such as acetic anhydride.The liquid medium may contain an organic solvent, may contain at least one selected from the group consisting of methyl isobutyl ketone, methyl ethyl ketone, and toluene, may contain methyl isobutyl ketone, or may contain methyl ethyl ketone, from the viewpoint of easily reducing the viscosity ratio and easily obtaining excellent dispersibility of the particles.
[0041] The liquid medium may contain a hydrophobic organic solvent, or may contain a plurality of hydrophobic organic solvents. As the hydrophobic organic solvent, a solvent having a solubility in water at 25° C. of 1 g / 100 mL or less may be used.
[0042] When the liquid medium contains an organic solvent, the content of the organic solvent may be 20% by mass or more, 30% by mass or more, 50% by mass or more, more than 50% by mass, 70% by mass or more, 80% by mass or more, 90% by mass or more, 92% by mass or more, 95% by mass or more, 97% by mass or more, 98% by mass or more, 99% by mass or more, or substantially 100% by mass, based on the total mass of the liquid medium (the total amount of the liquid medium contained in the particle dispersion), from the viewpoint of easily reducing the viscosity ratio and easily obtaining excellent dispersibility of the particles.
[0043] δ of the liquid medium in the particle dispersion d2 , δ p2 or δ h2 (unit: MPa 0.5 ) may be in the following range from the viewpoint of adjusting the viscosity ratio: d2 , δ p2 or δ h2 When the liquid medium is composed of a single dispersion medium, the δ d2 , δ p2 or δ h2 When the liquid medium contains multiple dispersion media, the δ of the mixture of all dispersion media contained in the particle dispersion is d2 , δ p2 or δ h2 The target is.
[0044] δ of the liquid medium d2may be 10.0 or more, 11.0 or more, 12.0 or more, 13.0 or more, 14.0 or more, 14.5 or more, 15.0 or more, 15.5 or more, 16.0 or more, 16.5 or more, 17.0 or more, 17.5 or more, 18.0 or more, 18.5 or more, 19.0 or more, or 19.5 or more. d2 may be 25.0 or less, 22.0 or less, 20.0 or less, 19.5 or less, 19.0 or less, 18.5 or less, 18.0 or less, 17.5 or less, 17.0 or less, 16.5 or less, 16.0 or less, 15.5 or less, or 15.0 or less. d2 may be 10.0 to 25.0, 10.0 to 20.0, 10.0 to 17.0, 12.0 to 25.0, 12.0 to 20.0, 12.0 to 17.0, 15.0 to 25.0, 15.0 to 20.0, or 15.0 to 17.0.
[0045] δ of the liquid medium p2 may be 0.0 or more, greater than 0.0, 1.0 or more, 2.0 or more, 3.0 or more, 4.0 or more, 5.0 or more, 5.5 or more, 6.0 or more, 6.5 or more, 7.0 or more, 7.5 or more, 8.0 or more, 8.5 or more, 9.0 or more, 10.0 or more, 11.0 or more, 12.0 or more, 13.0 or more, 14.0 or more, 15.0 or more, 16.0 or more, 17.0 or more, or 18.0 or more. p2 may be 20.0 or less, 19.0 or less, 18.0 or less, 17.0 or less, 16.0 or less, 15.0 or less, 14.0 or less, 13.0 or less, 12.0 or less, 11.0 or less, 10.0 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, 5.5 or less, 5.0 or less, 4.5 or less, 4.0 or less, 3.5 or less, 3.0 or less, 2.5 or less, 2.0 or less, or 1.5 or less. p2 may be 0.0 to 20.0, 0.0 to 15.0 or less, 0.0 to 10.0, 1.0 to 20.0, 1.0 to 15.0, 1.0 to 10.0, 3.0 to 20.0, 3.0 to 15.0, 3.0 to 10.0, 6.0 to 20.0, 6.0 to 15.0, or 6.0 to 10.0.
[0046] δ of the liquid medium h2may be 0.0 or more, greater than 0.0, 1.0 or more, 2.0 or more, 3.0 or more, 4.0 or more, 5.0 or more, 5.5 or more, 6.0 or more, 6.5 or more, 7.0 or more, 7.5 or more, 8.0 or more, 8.5 or more, 9.0 or more, 10.0 or more, 11.0 or more, 12.0 or more, 13.0 or more, 14.0 or more, 15.0 or more, 16.0 or more, 17.0 or more, 18.0 or more, 19.0 or more, 20.0 or more, 21.0 or more, or 22.0 or more. h2 may be 23.0 or less, 22.0 or less, 21.0 or less, 20.0 or less, 19.0 or less, 18.0 or less, 17.0 or less, 16.0 or less, 15.0 or less, 14.0 or less, 13.0 or less, 12.0 or less, 11.0 or less, 10.0 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, 5.5 or less, 5.0 or less, 4.5 or less, 4.0 or less, 3.5 or less, 3.0 or less, 2.5 or less, or 2.0 or less. h2 may be 0.0 to 23.0, 0.0 to 15.0, 0.0 to 6.0, 1.0 to 23.0, 1.0 to 15.0, 1.0 to 6.0, 3.0 to 23.0, 3.0 to 15.0, 3.0 to 6.0, 4.0 to 23.0, 4.0 to 15.0, or 4.0 to 6.0.
[0047] The present inventors have found that, when a liquid medium contains a first dispersion medium and a second dispersion medium as multiple dispersion mediums, adjusting the distance between the HSP value of the second dispersion medium and the HSP value of the first dispersion medium (the HSP distance between dispersion mediums: hereinafter sometimes referred to as the "HSP distance of the second dispersion medium to the first dispersion medium") is effective in adjusting the viscosity ratio of the particle dispersion to the liquid medium, and that when the HSP distance of the second dispersion medium to the first dispersion medium is small, the viscosity ratio tends to be easily reduced. The HSP distance of the second dispersion medium to the first dispersion medium can be calculated using the following formula: δ d21 , δ p21 and δ h21 is the δ of the first dispersion medium d , δ p and δ h and δ d22 , δ p22 and δ h22 is the δ of the second dispersion medium d , δp and δ h HSP distance = {4 × (δ d21 -δ d22 ) 2 + (δ p21 -δ p22 ) 2 + (δ h21 -δ h22 ) 2} 0.5
[0048] The HSP distance of the second dispersion medium relative to the first dispersion medium (unit: MPa 0.5 ) may be in the following ranges. From the viewpoint of easily reducing the viscosity ratio, the HSP distance of the second dispersion medium to the first dispersion medium may be 20.0 or less, 19.0 or less, 18.0 or less, 17.5 or less, 17.0 or less, 16.5 or less, 16.0 or less, 15.5 or less, 15.0 or less, 14.5 or less, 14.0 or less, 13.5 or less, 13.0 or less, 12.5 or less, 12.0 or less, 11.5 or less, 11.0 or less, 10.5 or less, 10.0 or less, 9.5 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, or 5.5 or less. From the viewpoint of adjusting the viscosity ratio, the HSP distance of the second dispersion medium relative to the first dispersion medium may be greater than 0.0, 1.0 or more, 2.0 or more, 3.0 or more, 4.0 or more, 5.0 or more, 5.5 or more, 6.0 or more, 6.5 or more, 7.0 or more, 7.5 or more, 8.0 or more, 8.5 or more, 9.0 or more, 9.5 or more, 10.0 or more, 10.5 or more, 11.0 or more, 11.5 or more, 12.0 or more, 12.5 or more, 13.0 or more, 13.5 or more, 14.0 or more, 14.5 or more, 15.0 or more, 15.5 or more, 16.0 or more, 16.5 or more, 17.0 or more, or 17.5 or more. From these viewpoints, the HSP distance of the second dispersion medium relative to the first dispersion medium may be greater than 0.0 and less than 20.0, greater than 0.0 and less than 18.0, greater than 0.0 and less than 15.0, greater than 0.0 and less than 10.0, 5.0 to 20.0, 5.0 to 18.0, 5.0 to 15.0, 5.0 to 10.0, 7.0 to 20.0, 7.0 to 18.0, 7.0 to 15.0, or 7.0 to 10.0. The particle dispersion may contain three or more dispersion media, and may contain, for example, other dispersion media in addition to the first dispersion medium and second dispersion medium having HSP distances in the above-mentioned ranges.
[0049] From the viewpoint of adjusting the viscosity ratio, the content of the liquid medium may be within the following ranges relative to 100 parts by mass of particles (if the particles are surface-treated: including the content of the surface treatment agent) or 100 parts by mass of particles (if the particles are surface-treated: excluding the content of the surface treatment agent). The content of the liquid medium may be 10 parts by mass or more, 15 parts by mass or more, 20 parts by mass or more, 25 parts by mass or more, 30 parts by mass or more, 35 parts by mass or more, 40 parts by mass or more, 45 parts by mass or more, 50 parts by mass or more, 60 parts by mass or more, 80 parts by mass or more, or 100 parts by mass or more. The content of the liquid medium may be 200 parts by mass or less, 150 parts by mass or less, 120 parts by mass or less, 100 parts by mass or less, less than 100 parts by mass, 80 parts by mass or less, 60 parts by mass or less, 50 parts by mass or less, or 45 parts by mass or less. From these viewpoints, the content of the liquid medium may be 10 to 200 parts by mass, 20 to 120 parts by mass, or 30 to 60 parts by mass.
[0050] From the viewpoint of adjusting the viscosity ratio, the content of the liquid medium may be in the following ranges based on the total mass of the particle dispersion. The content of the liquid medium may be 1% by mass or more, 5% by mass or more, 10% by mass or more, 15% by mass or more, 20% by mass or more, 25% by mass or more, 30% by mass or more, 35% by mass or more, 40% by mass or more, or 45% by mass or more. The content of the liquid medium may be 99.9% by mass or less, 99.5% by mass or less, 99% by mass or less, 95% by mass or less, 90% by mass or less, 85% by mass or less, 80% by mass or less, 75% by mass or less, 70% by mass or less, 65% by mass or less, 60% by mass or less, 55% by mass or less, 50% by mass or less, 45% by mass or less, 40% by mass or less, 35% by mass or less, or 30% by mass or less. From these viewpoints, the content of the liquid medium may be 1 to 99.9% by mass, 5 to 80% by mass, or 10 to 70% by mass.
[0051] From the viewpoint of adjusting the viscosity ratio, the total amount of the particles and the liquid medium (including the content of the surface treatment agent when the particles are surface-treated), the total amount of the particles and the liquid medium (excluding the content of the surface treatment agent when the particles are surface-treated), the total amount of the inorganic particles and the liquid medium (including the content of the surface treatment agent when the inorganic particles are surface-treated), or the total amount of the inorganic particles and the liquid medium (excluding the content of the surface treatment agent when the inorganic particles are surface-treated) may be 50% by mass or more, more than 50% by mass, 70% by mass or more, 80% by mass or more, 90% by mass or more, 92% by mass or more, 95% by mass or more, 97% by mass or more, 98% by mass or more, 99% by mass or more, or substantially 100% by mass based on the total mass of the particle dispersion.
[0052] The particle dispersion may contain components other than the particles and the liquid medium (excluding the surface treatment agent for the particles). For example, a component that dissolves in the liquid medium can be used as such a component. Examples of components other than the particles and the liquid medium include resin materials that are not liquid at 25°C.
[0053] 25°C, shear rate 1 min -1 The viscosity V1 (unit: mPa s) of the particle dispersion in may be in the following range: 100 or more, 200 or more, 300 or more, 400 or more, 500 or more, 600 or more, 700 or more, 800 or more, 900 or more, 1000 or more, 2000 or more, 3000 or more, 4000 or more, 5000 or more, 8000 or more, or 10000 or more. The viscosity V1 may be 300,000 or less, 100,000 or less, 50,000 or less, 30,000 or less, 20,000 or less, 15,000 or less, 12,000 or less, 10,000 or less, 8,000 or less, 5,000 or less, 4,000 or less, 3,000 or less, 2,000 or less, 1,000 or less, 900 or less, 800 or less, 700 or less, 600 or less, 500 or less, 400 or less, or 300 or less. From these viewpoints, the viscosity V1 may be 100 to 300,000, 100 to 15,000, 150 to 5,000, or 200 to 800.
[0054] The present disclosure will be described in more detail below with reference to experimental examples, although the present disclosure is not limited to these experimental examples.
[0055] <Preparation of Materials Used> (Particles) Silica particles: manufactured by Admatechs Co., Ltd., product name "SO-32R", particles produced by a fusion method, particle diameters of 1.5 μm (D50) and 4.5 μm (D95), specific gravity 2.2 g / cm 3 Alumina particles: manufactured by Sumitomo Chemical Co., Ltd., trade name "AA04 Alumina", particle size 0.4 μm (D50) and 0.6 μm (D95), specific gravity 3.9 g / cm 3
[0056] (Surface Treatment Agent) Silane Coupling Agent: N-phenyl-3-aminopropyltrimethoxysilane, manufactured by Shin-Etsu Chemical Co., Ltd., trade name "KBM-573"
[0057] (Liquid medium) Various dispersion media listed in Tables 1 to 3
[0058] <Preparation of particle dispersion> (Experimental Examples A1 to A22) 100 parts by mass of silica particles, 0.5 parts by mass of silane coupling agent, 3.5 × 10 -2 A mixture was obtained by mixing 42.8 parts by mass of pure water and 42.8 parts by mass of the liquid medium (single dispersion medium) shown in Table 1 in a beaker. Next, the beaker containing this mixture was placed in a water bath at 60°C, and then stirred at a rotation speed of 150 min using two stirring blades (made of Teflon) driven by a Three-One motor. -1 The mixture was subjected to a wet treatment at 40°C for 1 hour to obtain a mixed solution having a solid content of 70% by mass.
[0059] Thereafter, a dispersion treatment by cavitation (Nanomizer treatment conditions: passing through the nozzle three times; Filmics treatment conditions: 40 m / s, 1 minute) was carried out using a Nanomizer device (manufactured by Yoshida Kikai Kogyo Co., Ltd., product name "NM2-2000AR") and a Filmics device (manufactured by Primix Corporation, product name "FM40-40L") to prepare a particle dispersion liquid with a solid content of 70% by mass.
[0060] The above-mentioned solid content of the particle dispersion was determined in advance as the solid content of the particle dispersion at which a boundary state between a non-Bingham fluid and a dilatancy fluid was achieved by checking the behavior of viscosity with respect to the rotation speed of an E-type viscometer (manufactured by Toki Sangyo Co., Ltd., trade names "TV-22 Model" and "TV-33 Model") while changing the solid content of the particle dispersion in increments of 5% by mass. The following solid content of the particle dispersion was also determined in advance.
[0061] (Experimental Examples B1 to B22) A particle dispersion liquid with a solid content of 70% by mass was prepared in the same manner as in Experimental Example A1, except that 42.8 parts by mass of the liquid medium was used, which was a liquid medium (a mixture of multiple dispersion media) shown in Table 2.
[0062] (Experimental Examples C1 to C12) 100 parts by mass of alumina particles, 0.5 parts by mass of silane coupling agent, 3.5 × 10 -2 A mixture was obtained by mixing 100 parts by mass of pure water and 100 parts by mass of a liquid medium (single dispersion medium) shown in Table 3 in a beaker. Next, the beaker containing this mixture was placed in a water bath at 60°C, and then stirred at a rotation speed of 150 min using two stirring blades (made of Teflon) driven by a Three-One motor. -1 The mixture was subjected to a wet treatment at 40°C for 1 hour to obtain a mixed solution having a solid content of 50% by mass.
[0063] Thereafter, a dispersion treatment by cavitation (Nanomizer treatment conditions: passing through the nozzle three times; Filmics treatment conditions: 40 m / s, 1 minute) was carried out using a Nanomizer device (manufactured by Yoshida Machinery Industry Co., Ltd., product name "NM2-2000AR") and a Filmics device (manufactured by Primix Corporation, product name "FM40-40L") to prepare a particle dispersion liquid with a solid content of 50% by mass.
[0064] <HSP value of particles> Powdery particles were collected by drying the above particle dispersion at 130° C. for 1 hour. The particle diameters D50 (hereinafter referred to as “particle diameter A”) and D100 of the particles were obtained based on observation of real images using a scanning electron microscope (SEM).
[0065] Next, 0.02 g of these particles were placed in each of 16 containers (screw bottles), and 20 mL of 16 different organic solvents were added to each container to prepare test solutions (particle content: approximately 0.1% by mass). The 16 organic solvents used were methyl isobutyl ketone, toluene, methanol, cyclohexanol, acetone, acetonitrile, formamide, benzyl benzoate, dimethyl sulfoxide, ethyl acetate, ethanol, acetic anhydride, γ-butyrolactone, methyl ethyl ketone, 1-butanol, and cyclohexane. The test solutions were subjected to a 5-minute dispersion treatment using an ultrasonic dispersion device (manufactured by AS ONE Corporation, product name "VS-D100"). Next, the particle size distribution (cumulative particle size distribution, volume distribution) of the particles in the test solutions was measured using a particle size distribution analyzer (manufactured by Shimadzu Corporation, product name "SALD-7500"). For each of the 16 organic solvents mentioned above, the particle size D50 (hereinafter referred to as "particle size B") was obtained based on the particle size distribution measurement results. The particle size distribution of standard particles (MBP1-10) with a defined particle size distribution was measured in advance to confirm that the measurement results were appropriate.
[0066] Based on the results of the particle size distribution measurements, the coefficient of variation (CV) of particle size was obtained for each of the 16 types of organic solvents mentioned above. A coefficient of variation of 20 or more was determined to be a polydispersed state, and a coefficient of variation of less than 20 was determined to be a monodispersed state. The 16 types of organic solvents mentioned above were judged to be "solvents with poor dispersibility" or "solvents with excellent dispersibility" according to the following criteria.
[0067] As a criterion for aggregation in a monodispersed state, a particle diameter twice the particle diameter A (assuming the particle diameter when two particles come into contact) was adopted as a threshold value, and an organic solvent in which the particle diameter B was equal to or greater than this threshold was judged to be a "solvent with poor dispersibility," while an organic solvent in which the particle diameter B was less than this threshold was judged to be a "solvent with excellent dispersibility."
[0068] On the other hand, as for the criterion for aggregation in a polydispersed state, since the particle size distribution is wide and it is desirable to set a criterion that is easy to target aggregated particles, the above-mentioned particle size D100 was adopted as a threshold value, and organic solvents in which the above-mentioned particle size B was equal to or greater than this threshold were judged to be "solvents with poor dispersibility," and organic solvents in which the above-mentioned particle size B was less than this threshold were judged to be "solvents with excellent dispersibility."
[0069] Next, using the analytical software HSPiP (Hansen Solubility Parameter in Practice; written by Prof. Steven Abbott and Dr. Yamamoto Hiroshi), δ d , δ p and δ h The 16 organic solvents mentioned above were plotted in a three-dimensional space (Hansen space) with the coordinate axes of δ. d , δ p and δ h The values in the database of the above-mentioned analysis software were used as the values.
[0070] Next, a virtual sphere was created in the three-dimensional space that encompassed all of the "solvents with excellent dispersibility" without encompassing all of the "solvents with poor dispersibility." Then, δ at the center of this sphere was calculated. d , δ p and δ h the particle's δ d1 , δ p1 and δ h1 In silica particles, "δ d1 = 13.4 MPa 0.5 , δ p1 = 11.7 MPa 0.5 , δ h1 = 13.1 MPa 0.5 " In the alumina particles, "δ d1 = 17.1 MPa 0.5 , δ p1 = 10.3 MPa 0.5 , δ h1 = 12.7 MPa 0.5 "
[0071] <HSP value of liquid medium> δ of liquid medium d , δ pand δ h The values in the database of the analytical software HSPiP (Hansen Solubility Parameter in Practice; written by Prof. Steven Abbott and Dr. Yamamoto Hiroshi) were used as the δ of a liquid medium that is a mixture of multiple dispersion media. d2(mix) , δ p2(mix) and δ h2(mix) is the parameter of each dispersion medium (δ d , δ p or δ h The sum of the products of the volume ratio of each dispersion medium and the volume ratio of each dispersion medium was used. d2 , δ p2 and δ h2 The results are shown in Tables 1 to 3. Because the amount of the above-mentioned pure water mixed with the silane coupling agent was small, the influence of the pure water was not taken into consideration.
[0072] <Calculation of HSP distance> δ of particle d1 , δ p1 and δ h1 , and δ of the liquid medium d2 , δ p2 and δ h2 Based on this, the HSP distance of the particles relative to the liquid medium was calculated using the following formula. The HSP distance (particle / liquid medium) is shown in Tables 1 to 3. HSP distance = {4 × (δ d1 -δ d2 ) 2 + (δ p1 -δ p2 ) 2 + (δ h1 -δ h2 ) 2} 0.5
[0073] When a liquid medium that is a mixture of multiple dispersion media is used, the δ of the first dispersion medium d21 , δ p21 and δ h21 , and δ of the second dispersion medium d22 , δ p22 and δ h22 Based on this, the HSP distance between the dispersion media was calculated using the following formula. The HSP distance (dispersion media 1 / dispersion media 2) is shown in Table 2. HSP distance = {4 × (δ d21-δ d22 ) 2 + (δ p21 -δ p22 ) 2 + (δ h21 -δ h22 ) 2} 0.5
[0074] <Measurement of Viscosity> Using an E-type viscometer (manufactured by Toki Sangyo Co., Ltd., trade names "TV-22" and "TV-33"), the viscosity was measured at 25°C and a shear rate of 1 min -1 The viscosity A of the particle dispersion liquid described above was measured. Since the upper limit of viscosity measurable using a TV-22 viscometer is 14,650 mPa·s, viscosities A of 14,650 mPa·s or less were measured using the TV-22 viscometer, and viscosities A exceeding 14,650 mPa·s were measured using a TV-33 viscometer (upper limit of measurable viscosity: 1,000 Pa·s). Due to the design of the TV-33 viscometer, when the viscosity of the same liquid is measured using a TV-22 viscometer and a TV-33 viscometer, the measured value tends to be twice that measured using the TV-22 viscometer. Therefore, from the viewpoint of using the measured value of the TV-22 viscometer as the standard, the measured value measured using the TV-33 viscometer was corrected by half to obtain the viscosity A.
[0075] The viscosity B (25°C, shear rate 1 min) of the liquid medium used in each particle dispersion -1 (When the liquid medium contains multiple dispersion media, the viscosity of the mixture of all dispersion media contained in the particle dispersion liquid) is the viscosity (25°C, shear rate 1 min) listed in the Compact Solvent Pocket Book, 1st Edition, edited by the Society of Organic Synthetic Chemistry (1994). -1 The viscosity of the mixture of dispersion media was calculated as the sum of the products of the viscosity of each dispersion media and the volume ratio of each dispersion media. The viscosity ratio (A / B) of viscosity A to viscosity B is shown in Tables 1 to 3.
[0076]
[0077]
[0078]
Claims
1. A method for adjusting viscosity, which adjusts the relative relationship between the viscosity of a particle dispersion containing particles and a liquid medium and the viscosity of the liquid medium based on the distance between the HSP value of the particles and the HSP value of the liquid medium.
2. The method for adjusting viscosity according to claim 1, wherein the liquid medium comprises methyl isobutyl ketone.
3. The method for adjusting viscosity according to claim 1, wherein the liquid medium comprises methyl ethyl ketone.
4. The method for adjusting viscosity according to claim 1, wherein the liquid medium contains an organic solvent, and the content of the organic solvent is 80 mass % or more based on the total mass of the liquid medium.
5. The method for adjusting viscosity according to any one of claims 1 to 4, wherein the particles comprise silica.
6. A method for producing a particle dispersion comprising the steps of: selecting particles and a liquid medium based on the distance between the HSP value of the particles and the HSP value of the liquid medium; and mixing the particles and the liquid medium with each other.
7. The method of making a particle dispersion according to claim 6, wherein the liquid medium comprises methyl isobutyl ketone.
8. The method of making a particle dispersion according to claim 6, wherein the liquid medium comprises methyl ethyl ketone.
9. The method for producing a particle dispersion liquid according to claim 6, wherein the liquid medium contains an organic solvent, and the content of the organic solvent is 80 mass % or more based on the total mass of the liquid medium.
10. The method for producing a particle dispersion according to any one of claims 6 to 9, wherein the particles comprise silica.