# US 11,999,857 B2 · Coated particles and methods of making and using the same

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- Number: US 11,999,857 B2
- Document ID: US11999857B2
- Status: Granted
- Kind: B2
- Application number: 16/618,496
- Filed: 2018-06-01
- Published: 2020-04-23
- Granted: 2024-06-04
- Earliest claimed: 2017-06-02
- Assignees: W.R. Grace & Co.-Conn.
- Applicants: W. R. Grace & Co.-Conn.
- Inventors: Feng Gu
- Web page: https://patentgrep.com/patent/US11999857B2

## CPC

- C09C 1/3072: {Treatment with macro-molecular organic compounds}
- C01B 33/14: Colloidal silica, e.g. dispersions, gels, sols
- C08K 9/08: Ingredients agglomerated by treatment with a binding agent
- C08L 1/12: Cellulose acetate
- C08L 9/00: Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L 23/06: Polyethylene
- C08L 23/12: Polypropene
- C08L 33/26: Homopolymers or copolymers of acrylamide or methacrylamide
- C08L 39/06: Homopolymers or copolymers of N-vinyl-pyrrolidones
- C08L 91/00: Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C09C 1/3018: {Grinding}
- C09C 1/3027: {Drying, calcination}
- C09C 1/3063: {Treatment with low-molecular organic compounds}
- C09D 7/42: Gloss-reducing agents
- C09D 7/62: modified by treatment with other compounds
- C09D 15/00: Woodstains
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2006/12: Surface area
- C01P 2006/14: Pore volume
- C01P 2006/60: Optical properties, e.g. expressed in CIELAB-values
- C01P 2006/62: L* (lightness axis)
- C08K 9/04: Ingredients treated with organic substances {(treated with macromolecular compounds C08K9/08)}
- 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}
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- 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)
- 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)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Improved silica based matting agents are disclosed. The matting agents are useful in waterborne coatings composition to provide exceptional properties to a wood based substrate. Films resulting on the coated substrate unexpectedly provide improved chemical resistance, thermal stress resistance, weather resistance, and/or film clarity to the surface of a wood substrate. Methods of making and using the matting agents are also disclosed.

## Claims

### Claim 1

A matting agent comprising coated silica particles, said coated particles consisting of:
silica particles having a particle surface; and
greater than 30.0 weight percent (wt %), based on a total weight of said silica particles, of (i) one or more waxes, (ii) one or more polymers, or (iii) any combination of (i) and (ii) coated on said particle surface;
wherein said one or more polymers comprise polydiene, vulcanized polydiene, polyvinyl polypyrrolidone, cellulose acetate butyrate, or any combination thereof; and
wherein the coated silica particles are solvent-free, free-flowing particles and have an average particles size of from about 3.0 μm to about 12 μm.

### Claim 2 (depends on 1)

The matting agent of claim 1, wherein said silica particles comprise 31.0 wt % to about 50.0 wt %, based on a total weight of said silica particles, of (i) said one or more waxes, (ii) said one or more polymers, or (iii) any combination of (i) and (ii) on said particle surface.

### Claim 3 (depends on 1)

The matting agent of claim 1, wherein said silica particles comprise from about 40.0 wt % to about 50.0 wt %, based on a total weight of said silica particles, of (i) said one or more waxes, (ii) said one or more polymers, or (iii) any combination of (i) and (ii) on said particle surface.

### Claim 4 (depends on 1)

The matting agent of claim 1, wherein said silica particles comprise silica gel, precipitated silica or fumed silica particles.

### Claim 5 (depends on 1)

The matting agent of claim 1, wherein said silica particles have a total pore volume of from about 0.30 cc/gm to about 2.20 cc/gm, as determined by Barrett-Joyner-Halenda (BJH) method, and a BET particle surface area of at least about 100 m2/g up to 1500 m2/g, or greater.

### Claim 6 (depends on 5)

The matting agent of claim 5, wherein said silica particles have a total pore volume of from about 1.8 cc/gm to about 2.0 cc/gm, as determined by BJH method, and a BET particle surface area of at least about 200 m2/g up to 900 m2/g.

### Claim 7 (depends on 1)

The matting agent of claim 1, wherein said coated particles comprise said one or more waxes.

### Claim 8 (depends on 7)

The matting agent of claim 7, wherein said one or more waxes comprise a hydrocarbon wax, a paraffin wax, a polyethylene wax, a polypropylene wax, a plant wax, an animal wax, or any combination thereof.

### Claim 9 (depends on 8)

The matting agent of claim 8, wherein said one or more waxes comprise a polyethylene wax, a polypropylene wax, or a combination thereof.

### Claim 10 (depends on 1)

The matting agent of claim 1, wherein said coated particles consist of silica particles having a particle surface and greater than 30.0 wt. %, based on a total weight of said silica particles, of one or more polymers, wherein said one or more polymers comprise polydiene, vulcanized polydiene, polyvinyl polypyrrolidone, cellulose acetate butyrate, or any combination thereof.

### Claim 11 (depends on 1)

The matting agent of claim 1, when incorporated into a coating composition and applied onto a substrate, enables the coating composition to (i) form a film having a film clarity ΔL* of less than 7.0 units as measured using a portable Spectro-Guide 45/0 colorimeter, and (ii) exhibit a water damage 24 hr ΔL* of less than 5.0 units as measured using a portable Spectro-Guide 45/0 colorimeter.

### Claim 12 (depends on 11)

The matting agent of claim 11, when incorporated into a coating composition and applied onto a substrate, enables the coating composition to exhibit a 50/50 water/ethanol damage 1 hr ΔL* of less than 8.0 units as measured using a portable Spectro-Guide 45/0 colorimeter.

### Claim 13 (depends on 12)

The matting agent of claim 12, when incorporated into a coating composition and applied onto a substrate, enables the coating composition to exhibit a 50/50 water/ethanol damage 4 hr ΔL* of less than 16.0 units as measured using a portable Spectro-Guide 45/0 colorimeter.

### Claim 14 (depends on 1)

The matting agent of claim 1, when incorporated into a coating composition and applied onto a substrate, enables the coating composition to exhibit (i) a film clarity ΔL* of less than 7.0 units, (ii) a water damage 24 hr ΔL* of less than 4.0 units, (iii) a 50/50 water/ethanol damage 1 hr ΔL* of less than 8.0 units, and (iv) a 50/50 water/ethanol damage 4 hr ΔL* of less than 10.0 units, all measured using a portable Spectro-Guide 45/0 colorimeter.

### Claim 15 (depends on 1)

A coating composition comprising the matting agent of claim 1.

### Claim 16 (depends on 15)

The coating composition of claim 15, wherein said composition comprises an aqueous composition.

### Claim 17 (depends on 15)

A substrate coated with the coating composition of claim 15, wherein said substrate comprises a wood substrate.

### Claim 18 (depends on 1)

A method of preparing the matting agent of claim 1, said method comprising:
contacting the porous silica particles with (i) the one or more waxes, (ii) the one or more polymers, or (iii) any combination of (i) and (ii) so as to form coated silica paricles;
heat treating the coated silica particles at an elevated temperature for a heat treatment period of time so as to form heat-treated coated particles;
allowing the heat-treated coated particles to cool; and
milling the heat-treated coated particles so as to result in a final particle size of less than about 100 μm.

### Claim 19 (depends on 18)

The method of claim 18, wherein the coated silica particles are heat treated at elevated temperature ranges from about 90° C. to about 140° C., and the heat treatment period of time ranges from about 1.0 hour (hr) to about 4.0 hr.

### Claim 20 (depends on 1)

A method of improving chemical resistance, thermal stress resistance, weather resistance, film clarity, or any combination thereof, of a waterborne coating composition applied to a wood substrate, said method comprising:
incorporating the matting agent of claim 1 into the coating composition;
applying the coating composition onto at least one surface of a wood substrate to form a coating; and
drying the coating to form a film on at least one surface of the wood substrate.

### Claim 21 (depends on 20)

The method of claim 20, wherein the film exhibits (i) a film clarity ΔL* of less than 7.0 units, (ii) a water damage 24 hr ΔL* of less than 4.0 units, (iii) a 50/50 water/ethanol damage 1 hr ΔL* of less than 8.0 units, and (iv) a 50/50 water/ethanol damage 4 hr ΔL* of less than 10.0 units, all measured using a portable Spectro-Guide 45/0 colorimeter.