# US 10,308,823 B2 · Near-infrared absorbing fine particle dispersion liquid and method for producing the same

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- Number: US 10,308,823 B2
- Document ID: US10308823B2
- Status: Granted
- Kind: B2
- Application number: 15/546,934
- Filed: 2016-01-27
- Published: 2018-01-18
- Granted: 2019-06-04
- Earliest claimed: 2015-01-27
- Assignees: Sumitomo Metal Mining Co., Ltd.
- Applicants: Sumitomo Metal Mining Co., Ltd.
- Inventors: Mika Okada; Hideaki Fukuyama
- Web page: https://patentgrep.com/patent/US10308823B2

## CPC

- C09D 11/037: characterised by the pigment
- C09D 17/007: {Metal oxide}
- C09C 1/02: Compounds of alkaline earth metals or magnesium {(C09C1/0003, C09C1/0009, C09C1/0015, C09C1/0078 take precedence; dolomitic solids C09C1/009)}
- C09D 11/033: characterised by the solvent
- C09D 11/06: based on fatty oils
- C09D 17/00: Pigment pastes, e.g. for mixing in paints (artists' paints C09D5/06)
- C09K 3/00: Materials not provided for elsewhere
- C01P 2002/76: by a space-group or by other symmetry indications
- C01P 2002/77: by unit-cell parameters, atom positions or structure diagrams
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2004/80: Particles consisting of a mixture of two or more inorganic phases
- C09D 11/50: Sympathetic, colour changing or similar inks
- 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 (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS}
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A near infrared absorbing fine particle dispersion liquid, which can be applied to offset printing, including: a solvent of one or more kinds selected from vegetable oils and vegetable oil-derived compounds; near infrared ray-absorbing fine particles of one or more kinds selected from composite tungsten oxide expressed by MxWyOz or tungsten oxide having a Magneli phase expressed by a general formula WyOz; a solvent of one or more kinds selected from alcohols, ethers, esters, ketones, aromatic hydrocarbons and glycol ethers and having a boiling point of 180° C. or less, wherein a content of the solvent of one or more kinds selected from alcohols, ethers, esters, ketones, aromatic hydrocarbons and glycol ethers is 5 mass % or less.

## Claims

### Claim 1

A near infrared absorbing fine particle dispersion liquid, comprising:
a first solvent comprising at least one solvent selected from the group consisting of alcohols, ethers, esters, ketones, aromatic hydrocarbons, and glycol ethers, and having a boiling point of 180° C. or less;
a second solvent comprising at least one solvent selected from the group consisting of vegetable oils and vegetable oil-derived compounds;
near infrared absorbing fine particles selected from the group consisting of: fine particles of a composite tungsten oxide expressed by MxWyOz in which M Is at least one element selected from the group consisting of H, He, alkali metal, alkaline earth metal, rare earth element, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Be, Hf, Os, Bi, and I,
W is tungsten,
O is oxygen, and
0.001≤x/y≤1 and 2.2≤z/y≤3.0, and
fine particles of a tungsten oxide having a Magneli phase and expressed by a general formula WyOz in which
W is tungsten,
O is oxygen, and
2.45≤z/y≤2.999;
wherein: a residual content of the first solvent in the near infrared absorbing fine particle dispersion liquid 1.15 mass % or more and 4.20 mass % or less, and a content of the near Infrared absorbing fine particles in the near infrared absorbing fine particle dispersion liquid is 25 mass % or more and 75 mass % or less.

### Claim 2 (depends on 1)

The near infrared absorbing fine particle dispersion liquid according to claim 1, further comprising:
a dispersant which is soluble in the second solvent and has a fatty acid in its structure,
wherein a content of the fine particles of the composite tungsten oxide in the near infrared absorbing fine particle dispersion liquid is 25 mass % or more and 75 mass % or less.

### Claim 3 (depends on 2)

The near infrared absorbing fine particle dispersion liquid according to claim 2, wherein an anchor portion of the dispersant contains at least one selected from the group consisting of a secondary amino group, a tertiary amino group, and a quaternary ammonium group.

### Claim 4 (depends on 2)

The near infrared absorbing fine particle dispersion liquid according to claim 2, wherein the dispersant has an acid value of 1 mg KOH/g or more.

### Claim 5 (depends on 1)

The near infrared absorbing fine particle dispersion liquid according to claim 1, wherein a dispersed particle size of each near infrared absorbing fine particle is 1 nm or more and 200 nm or less.

### Claim 6 (depends on 1)

The near infrared absorbing fine particle dispersion liquid according to claim 1, comprising the fine particles of a composite tungsten oxide, wherein the fine particles of the composite tungsten oxide have a hexagonal crystal structure or are composed of a hexagonal crystal structure.

### Claim 7 (depends on 1)

The near infrared absorbing fine particle dispersion liquid according to claim 1, comprising the fine particles of a composite tungsten oxide, wherein a lattice constant of the fine particles of the composite tungsten oxide is 0.74060 nm or more and 0.74082 nm or less on the a-axis and 0.76106 nm or more and 0.76149 nm or less on the c-axis.

### Claim 8 (depends on 1)

The near infrared absorbing fine particle dispersion liquid according to claim 1, wherein a surface of each near infrared absorbing fine particle is coated with a compound of at least one element selected from the group consisting of Si, Ti, Al and Zr.

### Claim 9 (depends on 1)

The near infrared absorbing fine particle dispersion liquid according to claim 1, wherein the second solvent comprises at least one vegetable oil selected from the group consisting of drying oils and semi-drying oils.

### Claim 10 (depends on 1)

The near infrared absorbing fine particle dispersion liquid according to claim 1, wherein the near infrared absorbing fine particle dispersion liquid is an offset printing ink.

### Claim 11

A method for producing a near infrared absorbing fine particle dispersion liquid, comprising:
mixing near Infrared absorbing fine particles selected from the group consisting of: fine particles of a composite tungsten oxide expressed by MxWyOz in which M is at least one element selected from the group consisting of H, He, alkali metal, alkaline earth metal, rare earth element, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Be, Hf, Os, Bi, and I,
W is tungsten,
O is oxygen, and
0.001≤x/y≤1 and 2.2≤z/y≤3.0, and
fine particles of a tungsten oxide having a Magneli phase and expressed by a general formula WyOz in which
W is tungsten,
O is oxygen, and
2.45≤z/y≤2.999,
into a first solvent comprising at least one solvent selected from the group consisting of alcohols, ethers, esters, ketones, aromatic hydrocarbons, and glycol ethers, and having a boiling point of 180° C. or less, to thereby obtain a mixture;
then dispersing the mixture in a medium mill, to thereby obtain a first dispersion liquid;
adding and mixing a second solvent comprising at least one solvent selected from the group consisting of vegetable oils and vegetable oil-derived compounds into the first dispersion liquid, to thereby obtain a second dispersion liquid;
removing from the second dispersion liquid the first solvent until a residual content of the first solvent in the second dispersion liquid is 1.15 mass % or more and 4.20 mass % or less, to thereby obtain a near infrared absorbing fine particle dispersion liquid, wherein a content of the near infrared absorbing fine particles in the near infrared absorbing fine particle dispersion liquid is 25 mass % or more and 75 mass % or less.

### Claim 12 (depends on 11)

The method for producing a near infrared absorbing fine particle dispersion liquid according to claim 11, wherein a concentration of the near infrared absorbing fine particles in the first dispersion liquid is 5 mass % or more and 50 mass % or less.

### Claim 13 (depends on 11)

The method for producing a near infrared absorbing fine particle dispersion liquid according to claim 11, wherein a dispersant, which is soluble in the second solvent and has a fatty acid in its structure, is added to the second solvent.

### Claim 14

A method for producing a near Infrared absorbing fine particle dispersion liquid, comprising:
mixing a first solvent comprising at least one solvent selected from the group consisting of alcohols, ethers, esters, ketones, aromatic hydrocarbons, and glycol ethers, and having a boiling point of 180° C. or less, and a second solvent comprising at least one solvent selected from the group consisting of vegetable oils and vegetable oil-derived compounds, to thereby obtain a mixed solvent;
mixing infrared absorbing fine particles selected from the group consisting of: fine particles of a composite tungsten oxide expressed by MxWyOz in which M is at least one element selected from the group consisting of H, He, alkali metal, alkaline earth metal, rare earth element, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Be, Hf, Os, Bi, and I,
W is tungsten,
O Is oxygen, and
0.001≤x/y≤1 and 2.2≤z/y≤3.0, and
fine particles of a tungsten oxide having a Magneli phase and expressed by a general formula WyOz in which
W is tungsten,
O is oxygen, and
2.485≤z/y≤2.999,
into the mixed solvent to obtain a mixture, and dispersing the mixture in a wet medium mill, to thereby obtain a dispersion liquid; and
removing from the dispersion liquid the first solvent until a residual concentration of the first solvent in the dispersion liquid is 1.15 mass % or more and 4.20 mass % or less, to thereby obtain a near infrared absorbing fine particle dispersion liquid, wherein a content of the near Infrared absorbing fine particles in the near Infrared absorbing fine particle dispersion liquid is 25 mass % or more and 75 mass % or less.

### Claim 15 (depends on 14)

The method for producing a near infrared absorbing fine particle dispersion liquid according to claim 14, wherein a concentration of the near infrared ray absorbing fine particles in the dispersion liquid is 5 mass % or more and 50 mass % or less.
