# US 2013/0156684 A1 · Process for preparation of silver oxide

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- Number: US 2013/0156684 A1
- Document ID: US20130156684A1
- Status: Published application
- Kind: A1
- Application number: 13/755,101
- Filed: 2013-01-31
- Published: 2013-06-20
- Earliest claimed: 2007-12-07
- Assignees: Inktec Co., Ltd.
- Inventors: Kwang Choon CHUNG; Hyun Nam CHO; Ji Hoon YOO; Kee In SON
- Web page: https://patentgrep.com/patent/US20130156684A1

## CPC

- C01G 5/00: Compounds of silver
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C01P 2004/03: obtained by SEM
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- 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

A process for preparation of silver oxide with various shape and size using a silver complex compound having a special structure, includes 1) step of preparing a precursor solution including a silver complex compound obtained by reacting a silver compound with one or more mixture selected from the group consisting of an ammonium carbamate-based compound, an ammonium carbonate-based compound or an ammonium bicarbonate-based compound in the presence of a solvent; and 2) step of preparing silver oxide by reacting the precursor solution including the silver complex compound of step 1) with an oxidant. The shape and particle size of the silver oxide prepared according to the preparation process can be changed.

## Claims

### Claim 1

A process for preparation of silver oxide comprising:
preparing a precursor solution including a silver complex compound obtained by reacting a silver compound represented by the formula 1 below with one or more mixture selected from an ammonium carbamate-based compound, an ammonium carbonate-based compound or an ammonium bicarbonate-based compound represented by the formula 2, 3 or 4 below in the presence of a solvent; and preparing silver oxide by reacting the precursor solution including the silver complex compound of step 1) with an oxidant
AgnX [Formula 1]
[In the formula 1, n is an integer from 1 to 4 and X is a substituent selected from the group consisting of oxygen, sulfur, halogen, cyano, cyanate, carbonate, nitrate, nitrite, sulfate, phosphate, thiocyanate, chlorate, perchlorate, tetrafluoroborate, acetylacetonate, carboxylate and derivatives thereof.]
[In the formulas 2 to 4, R1, R2, R3, R4, R5 and R6 is hydrogen, aliphatic or cycloaliphatic (C1-C30)alkyl group, (C6-C20)aryl group, (C6-C20)aryloxy group, (C6-C20) ar (C1-C30)alkyl group, tri(C1-C30)alkylsilyl group, tri(C1-C30)alkoxy silyl group, tri(C6-C20)arylsilyl group, allyl group, or 3-membered to 7-membered heterocyclic compound group, polymer compound group, hydroxyl group, (C1-C30)alkoxy group, (C1-C30)alkylamino group, independently from each other, or R1 and R2 or R4 and R5 may be bonded independently from each other by (C2-C6)alkylene, which includes or does not include hetero atom, to form a ring, the alkyl group or aryl group of R1, R2, R3, R4, R5 and R6 may further be substituted by aliphatic or cycloaliphatic (C1-C30)alkyl, (C1-C30)alkoxy, cyano, hydroxy, amino, (C6-C20)aryl, tri(C1-C30)alkylsilyl, tri(C1-C30)alkoxysilyl, tri(C6-C20)aryl silyl, allyl or carboxylic acid.]

### Claim 2 (depends on 1)

The process for preparation of silver oxide according to claim 1, wherein the silver compound represented by the formula 1 is a mixture of at least one selected from silver oxide, silver thiocyanate, silver cyanide, silver cyanate, silver carbonate, silver nitrate, silver nitrite, silver sulfate, silver phosphate, silver perchlorate, silver tetrafluoroborate, silver acetylacetonate, silver acetate, silver lactate, silver oxalate and derivatives thereof.

### Claim 3 (depends on 1)

The process for preparation of silver oxide according to claim 1, wherein each substituent of R1, R2, R3, R4, R5 and R6 is independently selected from the group consisting of hydrogen, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, amyl, hexyl, ethylhexyl, heptyl, octyl, isooctyl, nonyl, decyl, dodecyl, hexadecyl, octadecyl, docodecyl, cyclopropyl, cyclopentyl, cyclohexyl, allyl, hydroxy, methoxy, hydroxyethyl, methoxyethyl, 2-hydroxypropyl, methoxypropyl, cyanoethyl, ethoxy, butoxy, hexyloxy, methoxyethoxyethyl, methoxyethoxyethoxyethyl, hexamethyleneimine, morpholine, piperidine, piperazine, ethylenediamine, propylenediamine, hexamethylenediamine, triethylenediamine, pyrrole, imidazole, pyridine, carboxymethyl, trimethoxysilylpropyl, triethoxysilylpropyl, phenyl, methoxyphenyl, cyanophenyl, phenoxy, tollyl, benzyl, derivatives thereof, polymer compounds such as polyallylamine and polyethyleneimine and derivatives thereof.

### Claim 4 (depends on 1)

The process for preparation of silver oxide according to claim 1, wherein the ammonium carbamate-based compound represented by the formula 2 are one or more mixture selected from the group consisting of ammonium carbamate, ethylammonium ethylcarbamate, isopropylammonium isopropylcarbamate, n-butylammonium n-butylcarbamate, isobutylammonium isobutylcarbamate, t-butylammonium t-butylcarbamate, 2-ethylhexylammonium 2-ethylhexylcarbamate, octadecylammonium octadecylcarbamate, 2-methoxyethylammonium 2-methoxyethylcarbamate, 2-cyanoethylammonium 2-cyanoethylcarbamate, dibutylammonium dibutylcarbamate, dioctadecylammonium dioctadecylcarbamate, methyldecylammonium methyldecylcarbamate, hexamethyleneiminium hexamethyleneiminecarbamate, morpholinium morpholinecarbamate, pyridinium ethylhexylcarbamate, benzylammonium benzylcarbamate, triethoxysilylpropylammonium triethoxysilylpropylcarbamate and derivatives thereof; the ammonium carbonate-based compound represented by the formula 3 are one or more mixture selected from the group consisting of ammonium carbonate, ethylammonium ethylcarbonate, isopropylammonium isopropylcarbonate, n-butylammonium n-butylcarbonate, isobutylammonium isobutylcarbonate, t-butylammonium t-butylcarbonate, 2-ethylhexylammonium 2-ethylhexylcarbonate, 2-methoxyethylammonium 2-methoxyethylcarbonate, 2-cyanoethylammonium 2-cyanoethylcarbonate, octadecylammonium octadecylcarbonate, dibutylammonium dibutylcarbonate, dioctadecylammonium dioctadecylcarbonate, methyldecylammonium methyldecylcarbonate, hexamethyleneiminium hexamethyleneiminecarbonate, morpholinium morpholinecarbonate, benzylammonium benzylcarbonate, triethoxysilylpropylammonium triethoxysilylpropylcarbonate, triethylenediaminium isopropylcarbonate and derivatives thereof; and the ammonium bicarbonate-based compound represented by the formula 4 are one or more mixture selected from the group consisting of ammonium bicarbonate, isopropylammonium bicarbonate, t-butylammonium bicarbonate, 2-ethylhexylammonium bicarbonate, 2-methoxyethylammonium bicarbonate, 2-cyanoethylammonium bicarbonate, dioctadecylammonium bicarbonate, pyridinium bicarbonate, triethylenediaminium bicarbonate and derivatives thereof.

### Claim 5 (depends on 1)

The process for preparation of silver oxide according to claim 1, wherein the solvent of step 1) is at least one selected from the group consisting of water, alcohols, glycols, acetates, ethers, ketones, aliphatic hydrocarbons, aromatic solvents, and halogen-substituted solvents

### Claim 6 (depends on 5)

The process for preparation of silver oxide according to claim 5, wherein the solvent is one or more mixture solvent selected from the group consisting of water, methanol, ethanol, isopropanol, butanol, ethylene glycol, glycerine, ethyl acetate, butyl acetate, carbitol acetate, diethyl ether, tetrahydrofuran, dioxane, methyl ethyl ketone, acetone, hexane, heptane, benzene, toluene, chloroform, methylene chloride and carbon tetrachloride.

### Claim 7 (depends on 1)

The process for preparation of silver oxide according to claim 1, wherein the precursor solution including the silver complex compound of step 1) further includes a dispersing agent.

### Claim 8 (depends on 7)

The process for preparation of silver oxide according to claim 7, wherein the dispersing agent is a mixture of at least one selected from the group consisting of resin; surfactant; an amine compound selected from a primary amine, a secondary amine or a tertiary amine; the ammonium carbamate-based compound represented by the formula 2; the ammonium carbonate-based compound represented by the formula 3; the ammonium bicarbonate-based compound represented by the formula 4; a phosphorus compounds; a sulfur compound; and fatty acid.
[In the formulas 2 to 4, R1, R2, R3, R4, R5 and R6 is hydrogen, aliphatic or cycloaliphatic (C1-C30)alkyl group, (C6-C20)aryl group, (C6-C20)aryloxy group, (C6-C20) ar (C1-C30)alkyl group, tri(C1-C30)alkylsilyl group, tri(C1-C30)alkoxy silyl group, tri(C6-C20)arylsilyl group, allyl group, or 3-membered to 7-membered heterocyclic compound group, polymer compound group, hydroxyl group, (C1-C30)alkoxy group, (C1-C30)alkylamino group, independently from each other, or R1 and R2 or R4 and R5 may be bonded independently from each other by (C2-C6)alkylene, which includes or does not include hetero atom, to form a ring, the alkyl group or aryl group of R1, R2, R3, R4, R5 and R6 may further be substituted by aliphatic or cycloaliphatic (C1-C30)alkyl, (C1-C30)alkoxy, cyano, hydroxy, amino, (C6-C20)aryl, tri(C1-C30)alkylsilyl, tri(C1-C30)alkoxysilyl, tri(C6-C20)aryl silyl, allyl or carboxylic acid.]

### Claim 9 (depends on 8)

The process for preparation of silver oxide according to claim 8, wherein the resin is at least one of an acryl resin, a cellulose resin, a polyester resin, a polyamide resin, a polyether resin, a vinyl resin, a polyurethane resin, a urea resin, an alkyd resin, a silicone resin, a fluorine resin, an olefin resin, petroleum, rosin, an epoxy resin, an unsaturated or vinyl polyester resin, a diallylphthalate resin, a phenol resin, an oxetane resin, an oxazine resin, a bismaleimide resin, a modified silicone resin melamine, an acryl resin, a styrene-butadiene rubber (SBR) or a natural polymer,

### Claim 10 (depends on 8)

The process for preparation of silver oxide according to claim 8, wherein the phosphorus compound is one represented by the formulas 6 to 8 below.
R3P [Formula 6]
(RO)3P [Formula 7]
(RO)3PO [Formula 8]
[wherein R is a linear or branched (C1-C20)alkyl group or a (C6-C20)aryl group.]

### Claim 11 (depends on 8)

The process for preparation of silver oxide according to claim 8, wherein the sulfur compound is selected from butanethiol, n-hexanethiol, diethyl sulfide or tetrahydrothiophene.

### Claim 12 (depends on 8)

The process for preparation of silver oxide according to claim 8, wherein the fatty acid is selected from palmitic acid, stearic acid, oleic acid or linoleic acid.

### Claim 13 (depends on 1)

The process for preparation of silver oxide according to claim 1, wherein the oxidant applied in the step 2) is at least one selected from the group consisting of an oxidative gas, a peroxide, a peroxy acid, an oxidative inorganic acid, an oxidative metal compound, and an oxidative nonmetal compound.

### Claim 14 (depends on 13)

The process for preparation of silver oxide according to claim 13, wherein the oxidant has an equivalent of 0.1 to 10, by mole number of silver in the precursor solution including the silver complex compound of step 1).

### Claim 15 (depends on 13)

The process for preparation of silver oxide according to claim 13, wherein the oxidant is at least one selected from the group consisting of oxygen, ozone, NaOH, KOH, Ca(OH2)H2O2, K2S2O8, NaBO3, KO2, Na2O2, (NH4)2S2O8, Na2S2O8, KHSO5, H2SO5, (CH3)3CO2H, (C6H5CO2)2, HCO3H, CH3CO3H, CF3CO3H, C6H5CO3H, m-ClC6H5CO3H, NaOCH3, NaOCH2CH3, nitric acid, sulfuric acid, I2, FeCl3, Fe (NO3)3, Fe2(SO4)3, K3Fe(CN)6, (NH4)2Fe(SO4)2, Ce(NH4)4(SO4)4, NaIO4, KMnO4, and K2CrO4.

### Claim 16 (depends on 13)

The process for preparation of silver oxide according to claim 13, wherein the oxidant is diluted using at least one solvent selected from the group consisting of water, an alcohol, a glycol, an acetate, an ether, a ketone, a hydrocarbon, an aromatic solvent, and a halogen hydrocarbon.

### Claim 17 (depends on 16)

The process for preparation of silver oxide according to claim 16, wherein the solvent is at least one selected from the group consisting of water, methanol, ethanol, isopropanol, 1-methoxypropanol, butanol, ethylhexyl alcohol, terpineol, ethylene glycol, glycerine, ethyl acetate, butyl acetate, methoxypropyl acetate, carbitol acetate, ethylcarbitol acetate, methylcellosolve, butylcellosolve, diethyl ether, tetrahydrofuran, dioxane, methyl ethyl ketone, acetone, dimethylformamide, 1-methyl-2-pyrrolidone, hexane, heptane, dodecane, paraffin oil, benzene, toluene, xylene, chloroform, methylene chloride, carbon tetrachloride, acetonitrile and dimethylsulfoxide.