# US 12,215,033 B2 · Silica particles comprising nitrogen element-containing compound containing molybdenum element

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- Number: US 12,215,033 B2
- Document ID: US12215033B2
- Status: Granted
- Kind: B2
- Application number: 17/584,390
- Filed: 2022-01-26
- Published: 2022-10-06
- Granted: 2025-02-04
- Earliest claimed: 2021-03-25
- Assignees: FUJIFILM Business Innovation Corp.
- Applicants: FUJIFILM Business Innovation Corp.
- Inventors: Yuka Zenitani; Sakae Takeuchi; Koji Sasaki; Yoshifumi Eri; Mai Mochida
- Web page: https://patentgrep.com/patent/US12215033B2

## CPC

- C01B 33/18: Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof (preparation of aerogels by dehydrating gels C01B33/158; treatment to enhance the pigmenting or filling properties C09C)
- C01B 33/159: Coating or hydrophobisation
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01P 2004/03: obtained by SEM
- C01P 2004/51: Particles with a specific particle size distribution
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2004/80: Particles consisting of a mixture of two or more inorganic phases
- C01P 2006/14: Pore volume
- C01P 2006/17: Pore diameter distribution
- C01P 2006/80: Compositional purity
- C01P 2006/90: Other properties not specified above
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Silica particles contain a nitrogen element-containing compound containing a molybdenum element, in which a ratio (Mo/Si) of Net intensity of the molybdenum element to Net intensity of a silicon element measured by X-ray fluorescence analysis is 0.035 or more and 0.35 or less.

## Claims

### Claim 1

Silica particles comprising:
silica base particles;
a reaction product of a trifunctional silane coupling agent, the reaction product covers at least a part of a surface of the silica base particles; and
a nitrogen element-containing compound containing a molybdenum element,
wherein an amount of the reaction product is 5.5% by mass or more and 30% by mass or less with respect to an amount of the silica particles, and
a ratio (Mo/Si) of Net intensity of the molybdenum element to Net intensity of a silicon element measured by X-ray fluorescence analysis is 0.035 or more and 0.35 or less.

### Claim 2 (depends on 1)

The silica particles according to claim 1,
wherein the nitrogen element-containing compound is at least one compound selected from the group consisting of a quaternary ammonium salt containing a molybdenum element and a mixture of a quaternary ammonium salt and a metal oxide containing a molybdenum element.

### Claim 3 (depends on 1)

The silica particles according to claim 1,
wherein the silica particles have a number average particle size of 10 nm or more and 200 nm or less.

### Claim 4 (depends on 1)

The silica particles according to claim 1,
wherein the nitrogen element-containing compound is adsorbed onto at least a part of pores of the reaction product.

### Claim 5 (depends on 1)

The silica particles according to claim 1,
wherein the silica particles have a degree of hydrophobicity of 10% or more and 60% or less.

### Claim 6 (depends on 1)

The silica particles according to claim 1,
wherein in a case where A represents a pore volume of pores having a diameter of 1 nm or more and 50 nm or less determined from a pore size distribution curve obtained by a nitrogen adsorption method before baking at 350° C., and B represents a pore volume of pores having a diameter of 1 nm or more and 50 nm or less determined from a pore size distribution curve obtained by a nitrogen adsorption method after baking at 350° C., B/A is 1.2 or more and 5 or less, and B is 0.2 cm3/g or more and 3 cm3/g or less.

### Claim 7 (depends on 1)

The silica particles according to claim 1,
wherein in a case where C represents an integral value of signals observed in a range of chemical shift of −50 ppm or more and −75 ppm or less in a 29Si solid-state nuclear magnetic resonance (NMR) spectrum obtained by a cross-polarization/magic angle spinning (CP/MAS) method, and D represents an integral value of signals observed in a range of chemical shift of −90 ppm or more and −120 ppm or less in the same spectrum, a ratio C/D is 0.10 or more and 0.75 or less.

### Claim 8 (depends on 1)

The silica particles according to claim 1,
wherein an extraction amount X of the nitrogen element-containing compound by a mixed solution of ammonia/methanol is 0.1% by mass or more, and
the extraction amount X of the nitrogen element-containing compound and an extraction amount Y of the nitrogen element-containing compound by water satisfy Expression: Y/X<0.3.

### Claim 9 (depends on 1)

The silica particles according to claim 1,
wherein the silica particles have an average circularity of 0.60 or more and 0.96 or less.

### Claim 10 (depends on 1)

The silica particles according to claim 1,
wherein the silica particles have a number-based particle size distribution index of 1.1 or more and 2.0 or less.