# US 2020/0399438 A1 · ABSORBING FINE PARTICLE DISPERSION LIQUID AND ABSORBING FINE PARTICLES DISPERSION BODY HAVING EXCELLENt LONG-TERM STABILITY, AND METHOD FOR PRODUCING THEM

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- Number: US 2020/0399438 A1
- Document ID: US20200399438A1
- Status: Published application
- Kind: A1
- Application number: 16/763,750
- Filed: 2018-11-13
- Published: 2020-12-24
- Earliest claimed: 2017-11-13
- Assignees: Sumitomo Metal Mining Co., Ltd.
- Applicants: Sumitomo Metal Mining Co., Ltd.
- Inventors: Hirofumi TSUNEMATSU; Takeshi CHONAN; Takahisa KAWANO
- Web page: https://patentgrep.com/patent/US20200399438A1

## CPC

- C08K 3/22: of metals
- C08K 3/24: Acids; Salts thereof {(C08K3/16 takes precedence)}
- C08J 5/18: Manufacture of films or sheets
- C08K 5/527: Cyclic esters
- C08K 9/02: Ingredients treated with inorganic substances
- C08K 9/04: Ingredients treated with organic substances {(treated with macromolecular compounds C08K9/08)}
- C09C 3/063: {Coating}
- C09C 3/08: Treatment with low-molecular-weight {non-polymer} organic compounds {(C09C3/006, C09C3/048 take precedence)}
- C09D 7/61: inorganic
- G02B 5/208: {for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation}
- C01P 2002/60: Compounds characterised by their crystallite size
- C01P 2002/76: by a space-group or by other symmetry indications
- C08J 2369/00: Characterised by the use of polycarbonates; Derivatives of polycarbonates
- C08K 2003/2258: {of tungsten}
- C09D 5/32: Radiation-absorbing paints {(protection against X-, gamma- or corpuscular radiation G21F)}
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- 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}
- 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)
- G02B: OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A dispersion body having excellent heat ray shielding properties and long-term high temperature stability, and a dispersion liquid for producing the dispersion body, wherein the dispersion liquid contains liquid medium, absorbing fine particles dispersed in the medium, and a phosphite ester compound, the absorbing fine particles are one or more kinds of oxide fine particles selected from tungsten oxide fine particles represented by a general formula WyOz, and the phosphite ester compound is a phosphite ester compound represented by the following predetermined structural formula, and an addition amount of the phosphite ester compound is more than 500 parts by mass and 50000 parts by mass or less with respect to 100 parts by mass of the absorbing fine particles.

## Claims

### Claim 1

An absorbing fine particle dispersion liquid containing liquid medium, absorbing fine particles dispersed in the medium, and a phosphite ester compound,
the absorbing fine particles being one or more kinds of oxide fine particles selected from tungsten oxide fine particles represented by a general formula WyOz (where W is tungsten, O is oxygen, 2.25≤z/y≤2.999), and composite tungsten oxide fine particles represented by a general formula MxWyOz (where, M is one or more elements selected from 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, T, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Be, Hf, Os, Bi, I, and Yb, W is tungsten, O is oxygen, 0.001≤x/y≤1, 2.05≤z/y≤3),
the phosphite ester compound being a phosphite ester compound represented by the following structural formula (1), and an addition amount of the phosphite ester compound being more than 500 parts by mass and 50000 parts by mass or less with respect to 100 parts by mass of the absorbing fine particles,
where, in the structural formula (1), R1, R2, R4 and R5 are each independently a hydrogen atom, an alkyl group having 1 to 8 carbon atoms, an alicyclic group having 5 to 12 carbon atoms, an aralkyl group having 7 to 12 carbon atoms or an aromatic group,
R3 is either a hydrogen atom or an alkyl group having 1 to 8 carbon atoms, and
X is any one of a single bond or a sulfur atom or a divalent residue represented by structural formula (1-1),
A is either an alkylene group having 2 to 8 carbon atoms or a divalent residue represented by structural formula (1-2),
one of Y and Z is a hydroxyl group, an alkyl group having 1 to 8 carbon atoms, an alkoxyl group having 1 to 8 carbon atoms, or an aralkyloxy group having 7 to 12 carbon atoms, and the other one is either a hydrogen atom or an alkyl group having 1 to 8 carbon atoms,
in the structural formula (1-1), R6 is a hydrogen atom or an alkyl group having 1 to 5 carbon atoms, and
in the structural formula (1-2), R7 is either a single bond or an alkylene group having 1 to 8 carbon atoms, and * indicates that the residue is bonded to an oxygen atom side of the phosphite ester compound represented by the structural formula (1).

### Claim 2 (depends on 1)

The absorbing fine particle dispersion liquid according to claim 1, further containing one or more kinds of stabilizers selected from a phosphoric acid-based stabilizer other than the phosphite ester compound, a hindered phenol-based stabilizer, a sulfide-based stabilizer, and a metal deactivator.

### Claim 3 (depends on 1)

The absorbing fine particle dispersion liquid according to claim 1, wherein the absorbing fine particles are composite tungsten oxide fine particles represented by the general formula MxWyOz, and the M is one or more kinds selected from Cs, Rb, K, Tl, In, Ba, Li, Ca, Sr, Fe and Sn.

### Claim 4 (depends on 1)

The absorbing fine particle dispersion liquid according to claim 1, wherein the absorbing fine particles are composite tungsten oxide fine particles having a hexagonal crystal structure.

### Claim 5 (depends on 1)

The absorbing fine particle dispersion liquid according to claim 1, wherein a crystallite size of the absorbing fine particles is 1 nm or more and 200 nm or less.

### Claim 6 (depends on 1)

The absorbing fine particle dispersion liquid according to claim 1, wherein surfaces of the absorbing fine particles are coated with a compound containing at least one element of Si, Ti, Zr, Al and Zn.

### Claim 7 (depends on 1)

The absorbing fine particle dispersion liquid according to claim 1, wherein the medium for dispersing the absorbing fine particles are high molecular.

### Claim 8

An absorbing fine particle dispersion body containing absorbing fine particles dispersed in a medium and a phosphite ester compound,
the absorbing fine particles being one or more kinds of oxide fine particles selected from tungsten oxide fine particles represented by a general formula WyOz (where W is tungsten, O is oxygen, 2.2≤z/y≤2.999), and composite tungsten oxide fine particles represented by a general formula MxWyOz (where, M is one or more elements selected from 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, T, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Be, Hf, Os, Bi, I, and Yb, W is tungsten, O is oxygen, 0.001≤x/y≤1, 2.0≤z/y≤3),
the phosphite ester compound being a phosphite ester compound represented by the following structural formula (1), and an addition amount of the phosphite ester compound being more than 500 parts by mass and 50000 parts by mass or less with respect to 100 parts by mass of the absorbing fine particles,
where in the structural formula (1), R1, R2, R4 and R5 are each independently a hydrogen atom, an alkyl group having 1 to 8 carbon atoms, an alicyclic group having 5 to 12 carbon atoms, an aralkyl group having 7 to 12 carbon atoms or an aromatic group,
R3 is either a hydrogen atom or an alkyl group having 1 to 8 carbon atoms, and
X is any one of a single bond or a sulfur atom or a divalent residue represented by structural formula (1-1),
A is either an alkylene group having 2 to 8 carbon atoms or a divalent residue represented by structural formula (1-2),
one of Y and Z is a hydroxyl group, an alkyl group having 1 to 8 carbon atoms, an alkoxyl group having 1 to 8 carbon atoms, or an aralkyloxy group having 7 to 12 carbon atoms, and the other one is either a hydrogen atom or an alkyl group having 1 to 8 carbon atoms,
in the structural formula (1-1), R6 is a hydrogen atom or an alkyl group having 1 to 5 carbon atoms, and
in the structural formula (1-2), R7 is either a single bond or an alkylene group having 1 to 8 carbon atoms, and * indicates that the residue is bonded to an oxygen atom side of the phosphite ester compound represented by the structural formula (1).

### Claim 9 (depends on 8)

The absorbing fine particle dispersion body according to claim 8,
further containing one or more kinds of stabilizers selected from a phosphoric acid-based stabilizer other than the phosphite ester compound, a hindered phenol-based stabilizer, a sulfide-based stabilizer, and a metal deactivator.

### Claim 10 (depends on 8)

The absorbing fine particle dispersion body according to claim 8, wherein the absorbing fine particles are composite tungsten oxide fine particles represented by the general formula MxWyOz, and the M is one or more kinds selected from Cs, Rb, K, T, In, Ba, Li, Ca, Sr, Fe and Sn.

### Claim 11 (depends on 8)

The absorbing fine particle dispersion body according to claim 8, wherein the absorbing fine particles are composite tungsten oxide fine particles having a hexagonal crystal structure.

### Claim 12 (depends on 8)

The absorbing fine particle dispersion body according to claim 8, wherein a crystallite size of the absorbing fine particles is 1 nm or more and 200 nm or less.

### Claim 13 (depends on 8)

The absorbing fine particle dispersion body according to claim 8, wherein surfaces of the absorbing fine particles are coated with a compound containing at least one element of Si, Ti, Zr, Al and Zn.

### Claim 14 (depends on 8)

The absorbing fine particle dispersion body according to claim 8, wherein a medium for dispersing the absorbing fine particles are high molecular.

### Claim 15 (depends on 8)

The absorbing fine particle dispersion body according to claim 8, wherein the medium for dispersing the absorbing fine particles is polycarbonate resin, acrylic resin, olefin resin, polystyrene resin, polyamide resin, polyethylene terephthalate resin, fluorine resin, vinyl chloride resin, or epoxy resin.

### Claim 16

A method for producing an absorbing fine particle dispersion liquid, comprising:
mixing absorbing fine particles which are one or more kinds of oxide fine particles selected from tungsten oxide fine particles represented by a general formula WyOz (where W is tungsten, O is oxygen, and 2.25≤z/y≤2.999), and composite tungsten oxide fine particles represented by a general formula MxWyOz (where M is one or more elements selected from 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, I, Yb, and W is tungsten, O is oxygen, 0.001≤x/y≤1, 2.0≤z/y≤3), and water, an organic solvent, a liquid resin, an oil and fat, a liquid plasticizer for the resin, a high molecular monomer, or a mixture of two or more selected from these groups, then, performing dispersion treatment, to obtain a dispersion liquid of absorbing fine particles;
adding more than 500 parts by mass and 50.000 parts by mass or less of phosphite ester with respect to 100 parts by mass of the absorbing fine particles while stirring the dispersion liquid; and
continuing the stirring after the addition, to obtain a dispersion liquid of the absorbing fine particles whose surfaces are coated with the phosphite ester compound.