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WO2025094500A1 - Agent de régulation de taille des particules pour suspension de particules ultrafines inorganiques et suspension de particules ultrafines inorganiques - Google Patents

Agent de régulation de taille des particules pour suspension de particules ultrafines inorganiques et suspension de particules ultrafines inorganiques Download PDF

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Publication number
WO2025094500A1
WO2025094500A1 PCT/JP2024/031180 JP2024031180W WO2025094500A1 WO 2025094500 A1 WO2025094500 A1 WO 2025094500A1 JP 2024031180 W JP2024031180 W JP 2024031180W WO 2025094500 A1 WO2025094500 A1 WO 2025094500A1
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WO
WIPO (PCT)
Prior art keywords
inorganic ultrafine
particle size
particle slurry
slurry
ultrafine particle
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Pending
Application number
PCT/JP2024/031180
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English (en)
Japanese (ja)
Inventor
泰裕 山本
克臣 島林
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San Nopco Ltd
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San Nopco Ltd
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Publication date
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Publication of WO2025094500A1 publication Critical patent/WO2025094500A1/fr
Pending legal-status Critical Current
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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

Definitions

  • the present invention relates to a particle size control agent for inorganic ultrafine particle slurry and inorganic ultrafine particle slurry.
  • Inorganic fine particle slurries are widely used in paints, ceramics, inks, etc., but in recent years, there has been a demand to control the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry to 100 nm or less in order to improve performance (improving surface roughness, etc.).
  • D50 dynamic light scattering method
  • the object of the present invention is to provide a particle size control agent for inorganic ultrafine particle slurry that can control the volume average particle size (D50, dynamic light scattering method) of inorganic ultrafine particles in an inorganic ultrafine particle slurry to 100 nm or less.
  • the particle size control agent for inorganic ultrafine particle slurries of the present invention is characterized in that it is composed of a salt (B) of a hydroxycarboxylic acid having 2 to 7 carbon atoms and ammonia or an organic amine having 1 to 14 carbon atoms.
  • the inorganic ultrafine particle slurry of the present invention is characterized in that it contains the above-mentioned particle size control agent for inorganic ultrafine particle slurry, inorganic ultrafine particles (A) and water (C),
  • the main point is that the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles (A) in the slurry is 100 nm or less.
  • the manufacturing method of the present invention is characterized in that it is a method for manufacturing the above-mentioned inorganic ultrafine particle slurry,
  • the gist is that it is prepared by a rotation process using beads and disks with diameters of 0.01 to 1 mm.
  • the particle size control agent for inorganic ultrafine particle slurry of the present invention can easily control the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry to 100 nm or less.
  • the inorganic ultrafine particle slurry of the present invention contains the above-mentioned particle size control agent for inorganic ultrafine particle slurry, so the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry can be easily adjusted to 100 nm or less, and performance can be easily improved (such as improved surface roughness) in fields such as paints, ceramics, and inks.
  • D50 dynamic light scattering method
  • the manufacturing method of the present invention uses the particle size control agent for inorganic ultrafine particle slurry described above, so that it is possible to easily prepare an inorganic ultrafine particle slurry in which the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry is 100 nm or less.
  • D50 dynamic light scattering method
  • hydroxycarboxylic acids having 2 to 7 carbon atoms include monohydroxymonocarboxylic acids (glycolic acid, lactic acid, 2-hydroxybutyric acid, 3-hydroxybutyric acid, ⁇ -hydroxybutyric acid, L-leucinic acid, etc.), monohydroxydicarboxylic acids (malic acid, tartronic acid, citramalic acid, etc.), monohydroxytricarboxylic acids (citric acid, isocitric acid, etc.), dihydroxymonocarboxylic acids (glyceric acid, mevalonic acid, pantoic acid, etc.), dihydroxydicarboxylic acids (tartaric acid, etc.), pentahydroxymonocarboxylic acids (gluconic acid, etc.), and tetrahydroxymonocarboxylic acids (glucoheptonic acid, etc.).
  • monohydroxymonocarboxylic acids glycolic acid, lactic acid, 2-hydroxybutyric acid, 3-hydroxybutyric acid, ⁇ -hydroxybutyric acid, L
  • monohydroxymonocarboxylic acids monohydroxydicarboxylic acids, monohydroxytricarboxylic acids, and dihydroxydicarboxylic acids and pentahydroxymonocarboxylic acids are preferred from the viewpoint of ease of controlling the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry to 100 nm or less.
  • D50 dynamic light scattering method
  • ammonia means inorganic ammonia (NH 3 ), and examples of organic amines having 1 to 14 carbon atoms include monoamines ⁇ monomethylamine, dimethylamine, trimethylamine, monoethylamine, diethylamine, triethylamine, tert-butylamine, pyrrolidine, pyridine, monohydroxymonoamines (monoethanolamine, N-methylethanolamine, dimethylaminoethanol, 2-amino-2-methyl-1-propanol, 1-amino-2-methyl-2-propanol, DL-isopropanolamine, propanolamine, etc.), dihydroxymonoamines (diethanolamine, methyldiethanolamine, etc.), trihydroxymonoamines (diethanolamine, methyldiethanolamine, etc.), amines (triethanolamine, etc.) and pentahydroxymonoamines (D-glucamine, N-methyl-D
  • ammonia and monoamines are preferred, more preferably ammonia, monohydroxymonoamine, dihydroxymonoamine, and trihydroxymonoamine, and particularly preferably ammonia, monohydroxymonoamine, and dihydroxymonoamine.
  • the salt (B) is preferably composed of 100 molar parts of hydroxycarboxylic acid and 50 to 350 (preferably 100 to 330, more preferably 160 to 300) molar parts of ammonia or organic amine. Within this range, the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry can be more easily controlled to 100 nm or less.
  • the particle size control agent for inorganic ultrafine particle slurry of the present invention can be produced by neutralizing a hydroxycarboxylic acid having 2 to 7 carbon atoms with ammonia or an organic amine having 1 to 14 carbon atoms in a solvent (water, lower alcohol, etc.) that can dissolve the hydroxycarboxylic acid.
  • the salt (B) may be prepared and then the solvent may be removed (by filtration or distillation, etc.), or it may be used as is.
  • the particle size control agent for inorganic ultrafine particle slurry of the present invention may be diluted with water before use. There are no particular restrictions on the concentration, but a concentration of 20 to 60% by weight (water concentration: 40 to 80% by weight) is preferred. As the water, the water described below is preferred.
  • Inorganic ultrafine particles that can be used as the particle size control agent for inorganic ultrafine particle slurries of the present invention include, without limitation, metal oxides, metal hydroxides, and metal carbonates, so long as they are mixed with water in the manufacturing process of paints, dielectrics, inks, ceramics, etc. (including intermediates and final products).
  • Metal oxides include titanium oxide, zinc oxide, alumina, iron oxide, magnesium oxide, silica, zirconia, and boehmite.
  • metal hydroxides examples include aluminum hydroxide, magnesium hydroxide, calcium hydroxide, and iron hydroxide.
  • metal carbonates examples include calcium carbonate, barium carbonate, and magnesium carbonate.
  • metal oxides are preferred from the viewpoint of ease of controlling the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry to 100 nm or less.
  • the inorganic ultrafine particles (A) contained in the inorganic ultrafine particle slurry of the present invention the above-mentioned inorganic ultrafine particles can be used, with the preferred range being as described above.
  • the particle size control agent the above-mentioned particle size control agent can be used, with the preferred range being as described above.
  • water (C) tap water, ion-exchanged water, distilled water, A1 to A3 (pure water) and A4 (ultrapure water) as specified in JIS K0557:1998
  • Water to be used in testing water and wastewater can be mentioned, and among these, ion-exchanged water, distilled water, A1 to A3 (pure water) and A4 (ultrapure water) as specified in JIS K0557:1998 are preferred.
  • the volume average particle size (nm, D50, dynamic light scattering method) of the inorganic ultrafine particles (A) in the slurry is preferably 100 or less, and more preferably 50 or less.
  • the measurement limit of the particle size (nm, dynamic light scattering method) is approximately 0.1 nm.
  • the volume average particle size is measured at 25°C using a nanoparticle analyzer (e.g., nanoPartica SZ-100, Horiba, Ltd.) in accordance with JIS Z8828:2019 "Particle size analysis - Dynamic light scattering" (corresponding international standard: ISO 22412:2017, Particle size analysis - Dynamic light scattering (DLS) (IDT)).
  • the volume average particle size (D50, dynamic light scattering) refers to the median diameter (D50, dynamic light scattering), which is the particle size that indicates the 50% cumulative value of the cumulative distribution curve.
  • the content (parts by weight) of the particle size control agent is preferably 5 to 50, more preferably 8 to 30, and particularly preferably 10 to 20, per 100 parts by weight of the inorganic ultrafine particles (A).
  • the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry can be more easily controlled to 100 nm or less.
  • the inorganic ultrafine particle slurry of the present invention may contain known additives, etc., in addition to the inorganic fine particles (A), particle size control agent, and water (C), to the extent that the effects of the present invention are not impaired.
  • additives include antifoaming agents, dispersants, viscosity reducers, wetting agents, and surface treatment agents.
  • the rotary processing device that can be used in the method for producing an inorganic ultrafine particle slurry of the present invention can be any known rotary processing device that uses beads and disks, such as a tower mill, ball mill, sand mill, pearl mill, and bead mill.
  • the diameter (mm) of the beads is preferably 0.01 to 1, and more preferably 0.1 to 0.2. Within this range, it is easier to control the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry to 100 nm or less.
  • D50 dynamic light scattering method
  • the material of the beads is not particularly limited, and examples include glass and zirconia. Zirconia is preferred.
  • Example 1 10,179 parts (100 molar parts as lactic acid) of lactic acid (special reagent grade, containing 11.5% water, Fujifilm Wako Pure Chemical Industries, Ltd.) (b11), 3,036 parts (50 molar parts as ammonia) of 28% aqueous ammonia solution (Nacalai standard grade 1, Nacalai Tesque, Inc.) and 11,431 parts of water were uniformly mixed to obtain an aqueous solution containing the particle size control agent of the present invention (B1; an aqueous solution of ammonium lactate having a concentration of 40%).
  • B1 an aqueous solution of ammonium lactate having a concentration of 40%
  • Example 2 39,232 parts of an aqueous solution of gluconic acid (b12) (50%, FUJIFILM Wako Pure Chemical Industries, Ltd.) (100 parts by mole as gluconic acid), 8,914 parts (100 parts by mole) of dimethylaminoethanol (b22) (purity >99.0%, Tokyo Chemical Industry Co., Ltd.) and 23,179 parts of water were uniformly mixed to obtain an aqueous solution containing the particle size control agent of the present invention (B2; an aqueous solution of dimethylaminoethanol gluconate having a concentration of 40%).
  • Example 3 13,409 parts (100 parts by mole) of L(-)-malic acid (Wako Grade 1, FUJIFILM Wako Pure Chemical Industries, Ltd.) (b13), 16,822 parts (160 parts by mole) of diethanolamine (purity >99.0%, Tokyo Chemical Industry Co., Ltd.) (b23), and 45,348 parts of water were uniformly mixed to obtain an aqueous solution containing the particle size control agent of the present invention (B3; an aqueous solution of L(-)-malic acid diethanolamine salt having a concentration of 40%).
  • B3 an aqueous solution of L(-)-malic acid diethanolamine salt having a concentration of 40%
  • Example 4 15,009 parts (100 parts by mole) of L(+)-tartaric acid (special grade reagent, FUJIFILM Wako Pure Chemical Industries, Ltd.) (b14), 12,216 parts (200 parts by mole) of monoethanolamine (purity >99.0%, Tokyo Chemical Industry Co., Ltd.) (b24), and 40,837 parts of water were uniformly mixed to obtain an aqueous solution containing the particle size control agent of the present invention (B4; an aqueous solution of L(+)-tartaric acid monoethanolamine salt having a concentration of 40%).
  • B4 an aqueous solution containing the particle size control agent of the present invention
  • Example 5 19,212 parts (100 parts by mole) of citric acid anhydride (Wako special grade, FUJIFILM Wako Pure Chemical Industries, Ltd.) (b15), 28,449 parts (300 parts by mole) of 2-amino-2-methyl-1-propanol (purity >93.0%, Wako first grade, FUJIFILM Wako Pure Chemical Industries, Ltd.) (b25) and 67,224 parts of water were uniformly mixed to obtain an aqueous solution containing the particle size control agent of the present invention (B5; an aqueous solution of 2-amino-2-methyl-1-propanol citrate salt having a concentration of 40%).
  • B5 an aqueous solution of 2-amino-2-methyl-1-propanol citrate salt having a concentration of 40%
  • Example 6 3.5 g of the aqueous solution (B1) containing a particle size control agent, 14 g of inorganic fine particles (a1) ⁇ AEROXIDE P-90, Evonik Japan Co., Ltd., fumed titanium dioxide, "AEROXIDE” is a registered trademark of Evonik Operations GmbH ⁇ , 56 g of water (c), and 210 g of zirconia beads (Toray Ceram, particle size: 0.1 mm, Toray Industries, Inc., "Toray Ceram” is a registered trademark of the same company) were placed in a vessel (type 2) of a bead mill (Easy Nano RMB II type, Imex Co., Ltd.) and rotated for 60 minutes with a disk to obtain an inorganic ultrafine particle slurry (1) of the present invention.
  • aqueous solution (B1) containing a particle size control agent 14 g of inorganic fine particles (a1) ⁇ AEROXIDE P-90, Evonik Japan Co., Ltd., fumed titanium dioxide
  • Example 7 The inorganic ultrafine particle slurry (2) of the present invention was obtained in the same manner as in Example 6, except that the "aqueous solution (B1) containing a particle diameter control agent" was changed to the “aqueous solution (B2) containing a particle diameter control agent.”
  • Example 8 The same procedure as in Example 6 was repeated except that 3.5 g of the aqueous solution (B1) containing a particle diameter control agent was replaced with 7.0 g of the aqueous solution (B3) containing a particle diameter control agent, to obtain an inorganic ultrafine particle slurry (3) of the present invention.
  • Example 9 The inorganic ultrafine particle slurry (4) of the present invention was obtained in the same manner as in Example 6, except that the "aqueous solution (B1) containing a particle size control agent” was changed to the “aqueous solution (B4) containing a particle size control agent” and the “inorganic fine particles (a1)” were changed to "inorganic fine particles (a2) ⁇ AEROXIDE P-25, Evonik Japan Co., Ltd., fumed titanium dioxide ⁇ ".
  • Example 10 The inorganic ultrafine particle slurry (5) of the present invention was obtained in the same manner as in Example 6, except that the "aqueous solution containing a particle size control agent (B1)” was changed to the “aqueous solution containing a particle size control agent (B5)” and the “inorganic fine particles (a1)” were changed to the “inorganic fine particles (a2)”.
  • Comparative Example A comparative inorganic ultrafine particle slurry (H) was obtained in the same manner as in Example 6, except that the "aqueous solution (B1) containing a particle size control agent" was not used.
  • the volume average particle size and surface roughness of the slurries were measured as follows, and are summarized in the table below.
  • the inorganic ultrafine particle slurry (H) obtained in the comparative example had a wide particle size distribution that exceeded the measurement range of the nanoparticle analyzer. In addition, the coarse particles settled in a short time, so the volume average particle size (D50, dynamic scattering method) could not be measured.
  • the volume average particle size (D50, laser diffraction scattering method) was measured for comparison using a particle size distribution measuring device (Partica LA-960V2, Horiba Ltd., JIS Z 8825:2022 Particle size analysis - Laser diffraction scattering method (corresponding international standard: ISO 13320:2020, Particle size analysis - Laser diffraction methods)) (however, due to the measurement principle, this method does not have a measurement accuracy of 100 nm or less.).
  • a particle size distribution measuring device Partica LA-960V2, Horiba Ltd., JIS Z 8825:2022 Particle size analysis - Laser diffraction scattering method (corresponding international standard: ISO 13320:2020, Particle size analysis - Laser diffraction methods)
  • this method does not have a measurement accuracy of 100 nm or less.
  • the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry can be easily controlled to 100 nm or less, and an inorganic ultrafine particle slurry in which the volume average particle size (D50, dynamic light scattering method) of the inorganic ultrafine particles in the inorganic ultrafine particle slurry is 100 nm or less can be easily prepared.
  • the inorganic ultrafine particle slurry of the present invention has better surface roughness than the comparative slurry, and performance can be easily improved.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

Le but de la présente invention est de proposer un agent de régulation de taille de particule pour une suspension de particules ultrafines inorganiques, ledit agent pouvant réguler la taille de particule moyenne en volume (D50, procédé de diffusion dynamique de la lumière) de particules ultrafines inorganiques dans la suspension de particules ultrafines inorganiques pour qu'elle soit inférieure ou égale à 100 nm. La présente invention concerne un agent de régulation de taille de particule pour une suspension de particules ultrafines inorganiques, ledit agent étant caractérisé en ce qu'il est composé d'un sel (B), qui est un sel d'un acide hydroxycarboxylique en C2-7 et d'ammoniac ou d'une amine organique en C1-14. Le sel (B) est de préférence composé de 100 parties en moles de l'acide hydroxycarboxylique et de 50 à 350 parties en moles de l'ammoniac ou de l'amine organique.
PCT/JP2024/031180 2023-11-01 2024-08-30 Agent de régulation de taille des particules pour suspension de particules ultrafines inorganiques et suspension de particules ultrafines inorganiques Pending WO2025094500A1 (fr)

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JP2023-187400 2023-11-01
JP2023187400 2023-11-01

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007318152A (ja) * 1998-06-26 2007-12-06 Cabot Microelectronics Corp 銅／タンタル基体に有用な化学的機械研磨スラリー
JP2008508373A (ja) * 2004-07-30 2008-03-21 エボニック デグサ ゲーエムベーハー 二酸化チタンを含有する分散液
JP2008069046A (ja) * 2006-09-14 2008-03-27 Tokyo Univ Of Agriculture & Technology 酸化チタン微粒子含有非水性分散液の製造方法、並びに酸化チタン微粒子及び有機ポリマーを含むポリマー系ナノコンポジットの製造方法
JP2009256131A (ja) * 2008-04-15 2009-11-05 Tokyo Univ Of Agriculture & Technology 無機酸化物粒子、無機酸化物粒子分散体、及びこれらの製造方法
JP2017002393A (ja) * 2015-06-12 2017-01-05 株式会社キャタラー 金属含有粒子の分散液及びその製造方法、並びにその分散液を用いて調製した触媒
JP2017119598A (ja) * 2015-12-28 2017-07-06 多木化学株式会社 ニッケルゾル
JP2017177014A (ja) * 2016-03-30 2017-10-05 株式会社キャタラー 分散液及び排ガス浄化用触媒並びにそれらの製造方法
JP2020172415A (ja) * 2019-04-12 2020-10-22 多木化学株式会社 大粒径アルミナ分散液

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007318152A (ja) * 1998-06-26 2007-12-06 Cabot Microelectronics Corp 銅／タンタル基体に有用な化学的機械研磨スラリー
JP2008508373A (ja) * 2004-07-30 2008-03-21 エボニック デグサ ゲーエムベーハー 二酸化チタンを含有する分散液
JP2008069046A (ja) * 2006-09-14 2008-03-27 Tokyo Univ Of Agriculture & Technology 酸化チタン微粒子含有非水性分散液の製造方法、並びに酸化チタン微粒子及び有機ポリマーを含むポリマー系ナノコンポジットの製造方法
JP2009256131A (ja) * 2008-04-15 2009-11-05 Tokyo Univ Of Agriculture & Technology 無機酸化物粒子、無機酸化物粒子分散体、及びこれらの製造方法
JP2017002393A (ja) * 2015-06-12 2017-01-05 株式会社キャタラー 金属含有粒子の分散液及びその製造方法、並びにその分散液を用いて調製した触媒
JP2017119598A (ja) * 2015-12-28 2017-07-06 多木化学株式会社 ニッケルゾル
JP2017177014A (ja) * 2016-03-30 2017-10-05 株式会社キャタラー 分散液及び排ガス浄化用触媒並びにそれらの製造方法
JP2020172415A (ja) * 2019-04-12 2020-10-22 多木化学株式会社 大粒径アルミナ分散液

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