# US 11,078,087 B2 · Plate-shaped hydrotalcite with high aspect ratio, method for manufacturing same and resin composition

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- Number: US 11,078,087 B2
- Document ID: US11078087B2
- Status: Granted
- Kind: B2
- Application number: 16/470,716
- Filed: 2017-12-19
- Published: 2020-03-19
- Granted: 2021-08-03
- Earliest claimed: 2016-12-22
- Assignees: Kyowa Chemical Industry Co., Ltd.
- Applicants: Kyowa Chemical Industry Co., Ltd.
- Inventors: Kenta Kawahito; Shigeo Miyata
- Web page: https://patentgrep.com/patent/US11078087B2

## CPC

- C01F 7/786: containing, besides aluminium, only anions, e.g. Al[OH]xCly[SO4]z (mixed halides C01F7/48)
- C01F 7/785: Hydrotalcite
- C08K 3/22: of metals
- C08L 101/00: Compositions of unspecified macromolecular compounds
- C01P 2004/03: obtained by SEM
- C01P 2004/24: Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
- C01P 2004/30: extending in three dimensions
- C01P 2004/54: Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
- C01P 2006/12: Surface area
- C08K 2003/2227: {of aluminium}
- C08K 2201/003: Additives being defined by their diameter
- C08K 2201/004: Additives being defined by their length
- C08K 2201/011: Nanostructured additives
- C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00})
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

With respect to a plate-shaped hydrotalcite in which the average width of primary particles is increased, (1) the aspect ratio of secondary particles is increased by suppressing aggregation of primary particles by relatively reducing the average thickness thereof, and 2) the formation of a by-product that impairs the transparency of a resin is suppressed. Provided is a plate-shaped hydrotalcite represented by a formula (1) below: (M2+)1−x(M3+)x(OH)2(An−)x/n·mH2O (1) where M2+ indicates at least one divalent metal, M3+ indicates at least one trivalent metal, An− indicates an n-valent anion, n indicates an integer of 1 to 6, and x and m are within respective ranges of 0.1≤x≤0.33 and 0≤m≤10, the formula (1) satisfying (A) to (D) below: (A) the average width of primary particles as measured using an SEM method is 1 μm or greater; (B) the average thickness of primary particles as measured using an SEM method is 80 nm or less; (C) the degree of monodispersity of width is 50% or greater; and (D) the degree of monodispersity of thickness is 50% or greater.

## Claims

### Claim 1

A plate-shaped hydrotalcite represented by a formula (1) below:
(M2+)1−x(M3+)x(OH)2(An−)x/n.mH2O (1)
wherein M2+ indicates at least one divalent metal, M3+ indicates at least one trivalent metal, An− indicates an n-valent anion, n indicates an integer of 1 to 6, and x and m are within respective ranges of 0.1≤x≤0.33 and 0≤m≤10,
the plate-shaped hydrotalcite satisfying (A) to (D) below:
(A) an average width of primary particles as measured using an SEM method is 1 μm or greater;
(B) an average thickness of primary particles as measured using an SEM method is 80 nm or less;
(C) a degree of monodispersity of width expressed by an equation below is 50% or greater:
degree of monodispersity of width (%)=(average width of primary particles as measured using the SEM method/average width of secondary particles as measured using a laser diffraction method)×100; and
(D) a degree of monodispersity of thickness expressed by an equation below is 50% or greater:
degree of monodispersity of thickness (%)=(average thickness of primary particles as measured using the SEM method/average thickness of secondary particles as measured using an SEM method)×100; and
a boehmite content in the plate-shaped hydrotalcite being 0.1 wt. % or less with respect to the plate-shaped hydrotalcite.

### Claim 2 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein (A) the average width of primary particles is 2 μm or greater.

### Claim 3 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein (B) the average thickness of primary particles is 60 nm or less.

### Claim 4 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein (C) the degree of monodispersity of the width is 80% or greater.

### Claim 5 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein (D) the degree of monodispersity of the thickness is 80% or greater.

### Claim 6 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein, in the formula (1), M2+ is at least one divalent metal selected from the group consisting of Mg and Zn, and M3+ is Al.

### Claim 7 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein, in the formula (1), the range of x is 0.15≤x≤0.25.

### Claim 8 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein surfaces of plate-shaped hydrotalcite particles are surface-treated with at least one agent selected from the group consisting of an anionic surfactant, phosphate esters, a silane coupling agent, a titanate coupling agent, an aluminum coupling agent, a silicone-based treatment agent, water glass, silica, and a cationic surfactant.

### Claim 9 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein, in the formula (1), the range of m is 0≤m≤0.05.

### Claim 10 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein the boehmite content in the plate-shaped hydrotalcite is 0.002 to 0.1 wt. % with respect to the plate-shaped hydrotalcite.

### Claim 11 (depends on 1)

The plate-shaped hydrotalcite according to claim 1, wherein the boehmite content in the plate-shaped hydrotalcite is 0.002 to 0.008 wt. % with respect to the plate-shaped hydrotalcite.

### Claim 12

A plate-shaped hydrotalcite represented by a formula (1) below:
(M2+)1−x(M3+)x(OH)2(An−)x/n·mH2O (1)
wherein M2+ indicates at least one divalent metal, M3+ indicates at least one trivalent metal, An− indicates an n-valent anion, n indicates an integer of 1 to 6, and x and m are within respective ranges of 0.1≤x≤0.33 and 0≤m≤10,
the plate-shaped hydrotalcite satisfying (A) to (E) below:
(A) an average width of primary particles as measured using an SEM method is 1 μm or greater;
(B) an average thickness of primary particles as measured using an SEM method is 80 nm or less;
(C) a degree of monodispersity of width expressed by an equation below is 50% or greater:
degree of monodispersity of width (%)=(average width of primary particles as measured using the SEM method/average width of secondary particles as measured using a laser diffraction method)×100;
(D) a degree of monodispersity of thickness expressed by an equation below is 50% or greater:
degree of monodispersity of thickness (%)=(average thickness of primary particles as measured using the SEM method/average thickness of secondary particles as measured using an SEM method)×100; and
(E) an aspect ratio of secondary particles (average width of secondary particles as measured using the laser diffraction method/average thickness of secondary particles as measured using the SEM method) is 10 or greater; and
a boehmite content in the plate-shaped hydrotalcite being 0.1 wt. % or less with respect to the plate-shaped hydrotalcite.

### Claim 13 (depends on 1)

A resin composition which contains the plate-shaped hydrotalcite of claim 1 in an amount of 0.1 to 250 parts by weight with respect to 100 parts by weight of a resin.

### Claim 14 (depends on 13)

A molded product formed of the resin composition according to claim 13.

### Claim 15 (depends on 1)

A method for manufacturing the plate-shaped hydrotalcite according to claim 1, the method comprising:
(i) preparing a slurry by dispersing a plate-shaped hydrotalcite represented by a formula (2) below in water; and (ii) subjecting the slurry to hydrothermal treatment at 200 to 300° C. for 10 to 24 hours,
(M2+)1−x(M3+)x(OH)2(An−)x/n·mH2O (2)
where M2+ indicates at least one divalent metal, M3+ indicates at least one trivalent metal, An− indicates a monovalent anion such as F−, Cl−, Br−, I−, NO3−, or CH3COO−, and x and m are within respective ranges of 0.1≤x≤0.33 and 0≤m≤10.

### Claim 16 (depends on 15)

The method for manufacturing a plate-shaped hydrotalcite according to claim 15, wherein An− of the plate-shaped hydrotalcite represented by the formula (2) is at least one monovalent anion selected from the group consisting of F−, Cl−, Br−, and I−.

### Claim 17 (depends on 15)

The method for manufacturing the plate-shaped hydrotalcite according to claim 15, wherein the method further comprises (iii) the plate-shaped hydrotalcite is obtained by further drying the plate-shaped hydrotalcite at 120° C. to 350° C. for 1 to 24 hours.