# US 10,869,826 B2 · Particulate metal oxide particles comprising a metal oxide core and a coating layer comprising an inorganic material, a silane coupling agent and/or a hydrophobizing agent

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- Number: US 10,869,826 B2
- Document ID: US10869826B2
- Status: Granted
- Kind: B2
- Application number: 14/418,999
- Filed: 2013-07-19
- Published: 2015-07-30
- Granted: 2020-12-22
- Earliest claimed: 2012-08-06
- Assignees: Croda International PLC
- Applicants: Croda International PLC
- Inventors: Robert Michael Sayer; Ian Robert Tooley; Paul Martin Staniland
- Web page: https://patentgrep.com/patent/US10869826B2

## CPC

- A61K 8/585: {Organosilicon compounds}
- A61K 8/0241: {Containing particulates characterized by their shape and/or structure (see also A61K8/04, A61K8/11, and A61K8/14, further aspects are classified in A61K2800/40 and subcodes)}
- A61K 8/04: Dispersions; Emulsions
- A61K 8/25: Silicon; Compounds thereof
- A61K 8/29: Titanium; Compounds thereof
- A61K 8/361: {Carboxylic acids having more than seven carbon atoms in an unbroken chain; Salts or anhydrides thereof}
- A61Q 17/04: Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C09C 1/043: {Zinc oxide}
- C09C 1/24: Oxides of iron
- C09C 1/3661: {Coating}
- C09C 1/3669: {Treatment with low-molecular organic compounds}
- C09C 1/3676: {Treatment with macro-molecular organic compounds}
- C09C 1/3692: {Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684}
- C09C 3/006: {Combinations of treatments provided for in groups C09C3/04 - C09C3/12}
- C09C 3/063: {Coating}
- C09C 3/08: Treatment with low-molecular-weight {non-polymer} organic compounds {(C09C3/006, C09C3/048 take precedence)}
- C09C 3/12: Treatment with organosilicon compounds {(C09C3/006 takes precedence)}
- A61K 2800/413: Nanosized, i.e. having sizes below 100 nm
- A61K 2800/63: More than one coating
- C01P 2004/51: Particles with a specific particle size distribution
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2004/84: one phase coated with the other
- C01P 2006/12: Surface area
- C01P 2006/60: Optical properties, e.g. expressed in CIELAB-values
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- A61Q: SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- 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}
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A particulate metal oxide has a metal oxide core and a coating layer containing an inorganic material and (i) a quaternary silane coupling agent, and/or (ii) a silane coupling agent and a hydrophobizing agent. Preferred materials are titanium dioxide core particles, an amino organosilane coupling agent and a fatty acid hydrophobizing agent. The particulate metal oxide is suitable for use in forming a dispersion, and the particles and dispersion can be used in an end-use sunscreen composition which is transparent, exhibits effective UV absorption properties, reduced photoactivity, and/or improved skin feel.

## Claims

### Claim 1

Coated metal oxide particles comprising metal oxide core particles each having thereon a coating layer comprising silica, a fatty acid and/or a salt thereof and a silane coupling agent,
wherein
the metal oxide comprises titanium dioxide,
the silane coupling agent comprises at least one hydrolyzable group and an amine group,
the coated metal oxide particles have an E308/E524 ratio of greater than 20, and
the coated metal oxide particles have a BET specific surface area in a range from 75 to 100 m2g−1.

### Claim 2 (depends on 1)

The coated metal oxide particles of claim 1, wherein the fatty acid has 10 to 24 carbon atoms.

### Claim 3 (depends on 1)

The coated metal oxide particles of claim 1, wherein the coating layer comprises 0.5% to 35% by weight of the silica, and/or 0.5 to 20% by weight of silane coupling agent, and/or 0.5% to 20% by weight of fatty acid and/or salt thereof, all based on the weight of the metal oxide core particles.

### Claim 4 (depends on 1)

The coated metal oxide particles of claim 1, comprising 82% to 84% by weight of the metal oxide, 6.5% to 7.5% by weight of the silica, 4% to 5.5% by weight of silane coupling agent, and 4.5% to 6% by weight of fatty acid and/or salt thereof, all based on the total dry weight of the particles.

### Claim 5 (depends on 1)

The coated metal oxide particles of claim 1, having a median volume particle diameter in dispersion of 40 to 55 nm.

### Claim 6 (depends on 1)

The coated metal oxide particles of claim 1, having a BET specific surface area in a range from 85 to 90 m2g−1.

### Claim 7 (depends on 1)

The coated metal oxide particles of claim 1, having a maximum extinction coefficient (Emax) in the range from 50 to 68 l/g/cm.

### Claim 8 (depends on 1)

A dispersion comprising the coated metal oxide particles of claim 1 in a liquid dispersing medium, wherein the liquid dispersing medium is a cosmetically acceptable material.

### Claim 9 (depends on 8)

The dispersion of claim 8, which comprises at least 30% by weight of the coated metal oxide particles.

### Claim 10 (depends on 8)

The dispersion of claim 8, which comprises a dispersing agent.

### Claim 11 (depends on 1)

A method of making the coated metal oxide particles of claim 1, comprising:
(i) forming metal oxide core particles, and
(ii) applying a coating layer to the metal oxide core particles comprising silica, the silane coupling agent, and the fatty acid and/or salt thereof.

### Claim 12 (depends on 11)

The method of claim 11, wherein the coating layer is applied sequentially in the order of (1) silica, (2) silane coupling agent, and (3) fatty acid and/or salt thereof.

### Claim 13 (depends on 1)

A sunscreen composition comprising the coated metal oxide particles of claim 1.

### Claim 14 (depends on 1)

A method of improving skin feel in a sunscreen composition comprising applying to the skin a composition comprising coated metal oxide particles of claim 1.

### Claim 15 (depends on 14)

The method of claim 14, wherein the improved skin feel includes a higher degree of lubricity to the skin.

### Claim 16

A composition comprising:
(i) coated metal oxide particles comprising metal oxide core particles each having thereon a coating layer comprising silica, a fatty acid and/or a salt thereof and a silane coupling agent,
wherein
the metal oxide comprises at least one member selected from the group consisting of titanium dioxide, zinc oxide and iron oxide,
the silane coupling agent comprises at least one hydrolyzable group and an amine group, and
the coated metal oxide particles have a BET specific surface area in a range from 75 to 100 m2g−1; and
(ii) a liquid medium selected from the group consisting of a C12-C15 alkyl benzoate, a fatty acid glyceride and isohexadecane.
