# US 10,501,637 B2 · Silane-treated forsterite fine particles and production method therefor, and organic solvent dispersion of silane-treated forsterite fine particles and production method therefor

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- Number: US 10,501,637 B2
- Document ID: US10501637B2
- Status: Granted
- Kind: B2
- Application number: 15/315,286
- Filed: 2015-08-06
- Published: 2017-07-06
- Granted: 2019-12-10
- Earliest claimed: 2014-08-07
- Assignees: Nissan Chemical Industries, Ltd.
- Applicants: Nissan Chemical Industries, Ltd.
- Inventors: Tadayuki Isaji; Masahiro Hida
- Web page: https://patentgrep.com/patent/US10501637B2

## CPC

- C09C 3/12: Treatment with organosilicon compounds {(C09C3/006 takes precedence)}
- C01B 33/22: Magnesium silicates
- C09C 1/28: Compounds of silicon {(C09C1/0009, C09C1/0015, C09C1/0078 take precedence)}
- C09C 3/006: {Combinations of treatments provided for in groups C09C3/04 - C09C3/12}
- C09D 17/00: Pigment pastes, e.g. for mixing in paints (artists' paints C09D5/06)
- 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}
- 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)

## Abstract

The invention provides silane-treated forsterite microparticles having a specific surface area of 5 to 100 m2/g, wherein 1 to 5 silyl groups are bound to 1 nm2 of the surface area thereof.

## Claims

### Claim 1

An organic solvent dispersion of silane-treated forsterite microparticles, the dispersion comprising:
silane-treated forsterite microparticles having a specific surface area of 5 to 100 m2/g, and having 1 to 5 silyl groups bound to 1 nm2 of the surface area thereof; and
a dispersion medium containing an organic solvent,
wherein the silyl groups are represented by the following formula (1):
—Si(R1)n(X)3-n (1)
wherein:
R1 represents at least one member selected from the group consisting of an alkyl group, an aryl group, a halo-alkyl group, a halo-aryl group, an alkenyl group, an epoxy group, a (meth)acryloyl group, a mercapto group, an amino group, and a cyano group, each of which is substituted or unsubstituted and has a solubility parameter (SP), estimated through the Fedors method, of 5.5 to 11.5;
X represents at least one of a hydroxyl group and a C1 to C4 alkoxy group; and
n is an integer of 0 to 3.

### Claim 2 (depends on 1)

An organic solvent dispersion of silane-treated forsterite microparticles according to claim 1, wherein the dispersion medium containing an organic solvent has a solubility parameter (SP) of 8 to 15.

### Claim 3 (depends on 1)

An organic solvent dispersion of silane-treated forsterite microparticles according to claim 1, wherein the organic solvent is at least one member selected from the group consisting of methyl alcohol (SP=14.5), ethyl alcohol (SP=12.7), isopropyl alcohol (SP=11.5), dimethylformamide (SP=12.0), methylcellosolve (SP=11.4), ethylcellosolve (SP=9.9), butylcellosolve (SP=8.9), ethylene glycol (SP=14.6), propylene glycol monomethyl ether (SP=10.5), propylene glycol monomethyl ether acetate (SP=8.7), 1-pentanol (SP=11.0), methyl ethyl ketone (SP=9.3), methyl isobutyl ketone (SP=8.3), cyclohexanone (SP=9.8), ethyl acetate (SP=9.1), butyl acetate (SP=8.5), toluene (SP=8.9), methyl methacrylate (SP=9.9), pentaerythritol triacrylate (SP=10.0), dipentaerythritol hexaacrylate (SP=9.1), bisphenol A epoxy resin (SP=10.4), and bisphenol F epoxy resin (SP=10.8).

### Claim 4 (depends on 1)

An organic solvent dispersion of silane-treated forsterite microparticles according to claim 1, wherein the organic solvent dispersion has a water content of 5 mass % or less.

### Claim 5 (depends on 1)

An electric wire coating material formed from the organic solvent dispersion of silane-treated forsterite microparticles as recited in claim 1.

### Claim 6 (depends on 1)

An insulating coating material formed from the organic solvent dispersion of silane-treated forsterite microparticles as recited in claim 1.

### Claim 7 (depends on 1)

An insulator formed from the organic solvent dispersion of silane-treated forsterite microparticles as recited in claim 1.

### Claim 8 (depends on 1)

An electron tube part formed from the organic solvent dispersion of silane-treated forsterite microparticles as recited in claim 1.

### Claim 9 (depends on 1)

A circuit component substrate formed from the organic solvent dispersion of silane-treated forsterite microparticles as recited in claim 1.

### Claim 10 (depends on 1)

A semiconductor package formed from the organic solvent dispersion of silane-treated forsterite microparticles as recited in claim 1.

### Claim 11 (depends on 1)

A method for producing the organic solvent dispersion of silane-treated forsterite microparticles according to claim 1, the method comprising the following steps (a) and (b):
step (a): a step of wet-crushing forsterite microparticles having a specific surface area of 5 to 100 m2/g in a dispersion medium containing an organic solvent by means of a bead mill, to thereby prepare an organic solvent dispersion; and
step (b): a step of adding, to the organic solvent dispersion prepared in step (a), an organic silicon compound represented by the following formula (2):
Si(R1)n(X)4-n (2)
(wherein R1 represents at least one member selected from the group consisting of an alkyl group, an aryl group, a halo-alkyl group, a halo-aryl group, an alkenyl group, an epoxy group, a (meth)acryloyl group, a mercapto group, an amino group, and a cyano group, each of which is substituted or unsubstituted and has a solubility parameter (SP), estimated through the Fedors method, of 5.5 to 11.5; X represents at least one of a hydroxyl group and a C1 to C4 alkoxy group; and n is an integer of 0 to 3) and/or a hydrolyzate thereof, so that the ratio by mass of organic silicon compound to forsterite microparticles (organic silicon compound/forsterite microparticles) is adjusted to 0.01 to 0.50, to thereby bind the silyl groups represented by the formula (1) onto the surfaces of the forsterite microparticles.

### Claim 12 (depends on 11)

A method for producing an organic solvent dispersion of silane-treated forsterite microparticles according to claim 11, wherein the dispersion medium containing an organic solvent has a solubility parameter (SP) of 8 to 15.

### Claim 13 (depends on 11)

A method for producing an organic solvent dispersion of silane-treated forsterite microparticles according to claim 11, wherein the organic solvent is at least one member selected from the group consisting of methyl alcohol (SP=14.5), ethyl alcohol (SP=12.7), isopropyl alcohol (SP=11.5), dimethylformamide (SP=12.0), methylcellosolve (SP=11.4), ethylcellosolve (SP=9.9), butylcellosolve (SP=8.9), ethylene glycol (SP=14.6), propylene glycol monomethyl ether (SP=10.5), propylene glycol monomethyl ether acetate (SP=8.7), 1-pentanol (SP=11.0), methyl ethyl ketone (SP=9.3), methyl isobutyl ketone (SP=8.3), cyclohexanone (SP=9.8), ethyl acetate (SP=9.1), butyl acetate (SP=8.5), toluene (SP=8.9), methyl methacrylate (SP=9.9), pentaerythritol triacrylate (SP=10.0), dipentaerythritol hexaacrylate (SP=9.1), bisphenol A epoxy resin (SP=10.4), and bisphenol F epoxy resin (SP=10.8).

### Claim 14 (depends on 11)

A method for producing an organic solvent dispersion of silane-treated forsterite microparticles according to claim 11, wherein the production method further includes the following step (c):
step (c): a step of substituting at least a part of the dispersion medium in the organic solvent dispersion produced in step (b), by another organic solvent.

### Claim 15 (depends on 11)

A method for producing an organic solvent dispersion of silane-treated forsterite microparticles according to claim 11, wherein the organic solvent dispersion has a water content of 5 mass % or less.

### Claim 16 (depends on 11)

A method for producing silane-treated forsterite microparticles, the method comprising the following steps (A) and (B):
step (A): a step of producing an organic solvent dispersion of silane-treated forsterite through a production method as recited in claim 11; and
step (B): a step of removing the dispersion medium contained in the organic solvent dispersion.
