# US 9,040,448 B2 · Method of manufacturing spherical mesoporous silica containing dispersed silver nanoparticles, and spherical mesoporous silica manufactured by said method

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- Number: US 9,040,448 B2
- Document ID: US9040448B2
- Status: Granted
- Kind: B2
- Application number: 13/640,953
- Filed: 2010-10-13
- Published: 2013-02-28
- Granted: 2015-05-26
- Earliest claimed: 2010-04-12
- Assignees: Thermolon Korea Co., Ltd.
- Applicants: Chung Kwon Park; Sang Cheol Han
- Inventors: Chung Kwon Park; Sang Cheol Han
- Web page: https://patentgrep.com/patent/US9040448B2

## CPC

- B01J 20/28007: {with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like (carbon nanostructures B01J20/205)}
- B01J 20/0233: {Compounds of Cu, Ag, Au}
- B01J 20/103: {comprising silica}
- B01J 20/28083: {being in the range 2-50 nm, i.e. mesopores}
- B01J 20/28097: {being coated, filled or plugged with specific compounds}
- B01J 20/3057: {Use of a templating or imprinting material (molecularly imprinted polymers B01J20/268); filling pores of a substrate or matrix followed by the removal of the substrate or matrix}
- B01J 20/3085: {Chemical treatments not covered by groups B01J20/3007 - B01J20/3078}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C01B 33/12: Silica; Hydrates thereof, e.g. lepidoic silicic acid
- 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)
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/03: obtained by SEM
- C01P 2004/32: Spheres
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2006/12: Surface area
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present invention relates to a method of preparing a spherical mesoporous silica structure containing silver nanoparticles dispersed therein by adding a silver nitrate solution to an aqueous surfactant solution and performing a sol-gel process and to spherical mesoporous silica prepared thereby. The spherical mesoporous silica is cost-effective compared to a conventional method that uses silver nanoparticles as a raw material, because the silver nitrate solution that is inexpensive compared to silver nanoparticles is used. Also, the spherical mesoporous silica can be with high productivity in large amounts, and thus is easily commercialized. Moreover, because silver nanoparticles are incorporated into the pores of the mesoporous silica, the silver nanoparticles are used stably and do not change color and odor. In addition, the spherical mesoporous silica exhibits various additional effects, including far-infrared ray emission and deodorization, attributable to silica.

## Claims

### Claim 1

A method for preparing spherical mesoporous silica containing silver nanoparticles dispersed therein, the method comprising the steps of:
(P100) adding a template to an aqueous alcohol solution, and then heating and dissolving the template, followed by cooling to room temperature, thereby forming a gel having a micelle structure;
(P200) adding a 5% silver nitrate solution to the gel solution to form an aqueous solution of a silver ion-amine complex compound;
(P300) adding a silica precursor to the gel solution containing the silver ion-amine complex compound formed therein, followed by stirring to form spherical mesoporous silica by a sol-gel process and to attach the silver ion-amine complex compound to the inside of the spherical mesoporous silica;
(P400) adding a reducing agent to convert silver ions in the silver ion-amine complex compound, attached to the inside of the spherical mesoporous silica, to silver nanoparticles; and
(P500) filtering the spherical mesoporous silica using a vacuum system, removing the remaining reducing agent from the filtered spherical mesoporous silica, and removing dodecylamine present in the spherical mesoporous silica with hot ethanol, followed by drying.

### Claim 2 (depends on 1)

The method of claim 1, wherein the aqueous alcohol solution is a mixture of 5-10 wt % of alcohol and 90-95 wt % of purified water.

### Claim 3 (depends on 1)

The method of claim 1, wherein the template is added in an amount of 1.0 mole per 20-24 L to form the micelle structure.

### Claim 4 (depends on 1)

The method of claim 1, wherein the silver nitrate solution is added in an amount of 0.1-0.3 moles per mole of the template.

### Claim 5 (depends on 1)

The method of claim 1, wherein the precursor is added in an amount of 3.6-4.4 moles per mole of the template.

### Claim 6 (depends on 1)

The method of claim 1, wherein the reducing agent is added in an amount of 0.2-0.6 moles per mole of the template.

### Claim 7 (depends on 1)

The method of claim 1, wherein the template is one or more selected from among alkylamines having 1 to 16 carbon atoms.

### Claim 8 (depends on 1)

The method of claim 1, wherein the silica precursor is one selected from among tetraethoxyorthosilicate (TEOS), tetramethoxyorthosilicate (TMOS), tetrapropoxyorthosilicate (TPOS), tetrabutoxyorthosilicate (TBOS), tetrapentoxyorthosilicate (TPEOS), tetra(methylethylketoxime)silane, vinyl oxime silane (VOS), phenyl tris(butanone oxime)sliane (POS), and methyl oxime silane (MOS).

### Claim 9 (depends on 1)

The method of claim 1, wherein the reducing agent is one or more selected from among NaBH4, NH2NH2, NH3, and H2S.

### Claim 10

A method for preparing spherical mesoporous silica containing silver nanoparticles dispersed therein, the method comprising the steps of:
(S100) adding a template to an aqueous alcohol solution, and then heating and dissolving the template, followed by cooling to room temperature, thereby forming a gel having a micelle structure (a gel solution-forming step);
(S200) adding a 5% silver nitrate solution to the gel solution to form an aqueous solution of a silver ion-amine complex compound;
(S300) adding a reducing agent to convert silver ions in the silver ion-amine complex compound to silver nanoparticles;
(S400) adding a silica precursor to the gel solution containing the silver nanoparticles dispersed therein, followed by stirring to form spherical mesoporous silica by a sol-gel process and to attach the silver nanoparticles to the inside of the spherical mesoporous silica; and
(S500) filtering the spherical mesoporous silica using a vacuum system, removing the remaining reducing agent from the filtered spherical mesoporous silica, and removing dodecylamine present in the spherical mesoporous silica with hot ethanol, followed by drying.

### Claim 11 (depends on 10)

The method of claim 10, wherein the aqueous alcohol solution is a mixture of 5-10 wt % of alcohol and 90-95 wt % of purified water.

### Claim 12 (depends on 10)

The method of claim 10, wherein the template is added in an amount of 1.0 mole per 20-24 L to form the micelle structure.

### Claim 13 (depends on 10)

The method of claim 10, wherein the silver nitrate solution is added in an amount of 0.1-0.3 moles per mole of the template.

### Claim 14 (depends on 10)

The method of claim 10, wherein the precursor is added in an amount of 3.6-4.4 moles per mole of the template.

### Claim 15 (depends on 10)

The method of claim 10, wherein the reducing agent is added in an amount of 0.2-0.6 moles per mole of the template.

### Claim 16 (depends on 10)

The method of claim 10, wherein the template is one or more selected from among alkylamines having 1 to 16 carbon atoms.

### Claim 17 (depends on 10)

The method of claim 10, wherein the silica precursor is one selected from among tetraethoxyorthosilicate (TEOS), tetramethoxyorthosilicate (TMOS), tetrapropoxyorthosilicate (TPOS), tetrabutoxyorthosilicate (TBOS), tetrapentoxyorthosilicate (TPEOS), tetra(methylethylketoxime)silane, vinyl oxime silane (VOS), phenyl tris(butanone oxime)sliane (POS), and methyl oxime silane (MOS).

### Claim 18 (depends on 10)

The method of claim 10, wherein the reducing agent is one or more selected from among NaBH4, NH2NH2, NH3, and H2S.