# US 5,707,552 A · Zinc antimonate anhydride and method for producing same

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- Number: US 5,707,552 A
- Document ID: US5707552A
- Status: Granted
- Kind: A
- Application number: 08/711,460
- Filed: 1996-09-11
- Granted: 1998-01-13
- Earliest claimed: 1994-06-06
- Assignees: Nissan Chemical Industries, Ltd.
- Inventors: Yoshitane Watanabe; Keitaro Suzuki; Yoshinari Koyama
- Web page: https://patentgrep.com/patent/US5707552A

## CPC

- C01G 30/02: Antimonates; Antimonites {(C01G30/001 takes precedence)}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C08K 3/2279: {of antimony}
- C09K 3/16: Anti-static materials
- C09K 21/02: Inorganic materials
- H01B 1/08: oxides
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/88: by thermal analysis data, e.g. TGA, DTA, DSC
- C01P 2004/03: obtained by SEM
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2004/10: extending in one dimension, e.g. needle-like
- C01P 2004/50: Agglomerated particles
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- 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
- C01P 2006/22: Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
- C01P 2006/40: Electric properties
- C01P 2006/60: Optical properties, e.g. expressed in CIELAB-values
- C01P 2006/82: water content
- 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
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- H01B: CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES (selection for magnetic properties H01F1/00; waveguides H01P {; printed circuits H05K})
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The object of the invention is to provide a zinc antimonate anhydride and a production method thereof. The invention relates to a particle having a ZnO/Sb.sub.2 O.sub.5 molar ratio in a range of from 0.8 to 1.2, a crystal structure of zinc antimonate anhydride (Znsb.sub.2 O.sub.6), and a primary particle size in a range of from 5 to 500 nm. The production method of these particles comprises the steps of mixing a zinc compound with a colloidal antimony oxide at a ZnO/Sb.sub.2 O.sub.5 molar rate in a range of from 0.8 to 1.2, followed by calcining the mixture within a temperature range of from 500.degree. to 680.degree. C. The particles of this invention are applicable as a flame retardant for plastics, a smoke suppressant, antistatic agent for plastics and glasses, and resistor.

## Claims

### Claim 1

A method for producing electroconductive particles having a ZnO/Sb.sub.2 O.sub.5 molar ratio in a range of from 0.8 to 1.2, comprising the steps of:
mixing a zinc compound with a colloidal antimony oxide at a ZnO/Sb.sub.2 O.sub.5 molar ratio in a range of from 0.8 to 1.2; and
thereafter calcining the mixture within a temperature range of from 500.degree. to 680.degree. C.;
wherein said particles are electroconductive, have a crystal structure of zinc antimonate anhydride (ZnSb.sub.2 O.sub.6), a primary particle size in a range of from 5 to 500 nm and a resistivity ranging from 0.1 K.OMEGA. to 1 M.OMEGA..

### Claim 2 (depends on 1)

A method for producing electroconductive particles as claimed in claim 1, wherein the calcining is conducted within a temperature range of from 500.degree. to 680.degree. C. for 2 to 20 hours.

### Claim 3 (depends on 1)

A method for producing electroconductive particles as claimed in claim 1, wherein the zinc compound and an antimony oxide sol are mixed, then the mixture is dried at a temperature of 500.degree. C. or below, and thereafter the dried mixture is calcined at a temperature range of from 500.degree. to 680.degree. C.

### Claim 4 (depends on 1)

A method for producing a stable sol comprising electroconductive particles having a ZnO/Sb.sub.2 O.sub.5 molar ratio in a range of from 0.8 to 1.2, having a crystal structure of zinc antimonate anhydride (ZnSb.sub.2 O.sub.6), and having a primary particle size in a range of from 5 to 500 nm, comprising the step of wet pulverizing in a solvent the particles prepared by the production method described in claim 1.

### Claim 5 (depends on 1)

A method for producing electroconductive particles as claimed in claim 1, wherein the zinc compound is at least one compound selected from the group consisting of zinc hydroxide, zinc oxide, zinc salt of inorganic acid, and zinc salt of organic acid.

### Claim 6 (depends on 1)

A method for producing electroconductive particles as claimed in claim 1, wherein the zinc compound is at least one compound selected from the group consisting of zinc hydroxide, zinc oxide, zinc carbonate, basic zinc carbonate, zinc nitrate, basic zinc nitrate, zinc chloride, basic zinc chloride, zinc sulfate, basic zinc sulfate, zinc formate, zinc acetate, zinc oxalate, and basic zinc oxalate.

### Claim 7 (depends on 1)

A method for producing electroconductive particles as claimed in claim 1, wherein the zinc compound is a material selected from the group consisting of zinc carbonate powder, basic zinc carbonate powder, zinc hydroxide powder or sol having a primary particle size of 500 nm or less, zinc oxide powder or sol having a primary particle size of 500 nm or less, and a mixture thereof.

### Claim 8 (depends on 1)

A method for producing electroconductive particles as claimed in claim 1, wherein the colloidal antimony oxide is an antimony oxide having a primary particle size of 300 nm or less.

### Claim 9 (depends on 1)

A method for producing electroconductive particles as claimed in claim 1, wherein the colloidal antimony oxide is a material selected from the group consisting of diantimony pentoxide sol, diantimony pentoxide powder, diantimony trioxide powder, and a mixture thereof, having a primary particle size in a range of from 2 to 300 nm.

### Claim 10 (depends on 1)

A method for producing electroconductive particles as claimed in claim 1, wherein the colloidal antimony oxide is diantimony pentoxide sol having a primary particle size in a range of from 2 to 300 nm.

### Claim 11 (depends on 1)

A method for producing electroconductive particles as claimed in claim 1, wherein the zinc compound is a material selected from the group consisting of zinc carbonate powder, basic zinc carbonate powder, zinc hydroxide powder or sol having a primary particle size of 500 nm or less, zinc oxide powder or sol having a primary particle size of 500 nm or less, and a mixture thereof and wherein the colloidal antimony oxide is diantimony pentoxide sol having a primary particle size in a range of from 2 to 300 nm.

### Claim 12

A method for producing electroconductive particles having a ZnO/Sb.sub.2 O.sub.5 molar ratio in a range of from 0.8 to 1.2, comprising the steps of:
mixing a zinc compound with a colloidal antimony oxide at a ZnO/Sb.sub.2 O.sub.5 molar ratio in a range of from 0.8 to 1.2 to form a mixture;
drying said mixture at a temperature of 500.degree. C. or below; and
thereafter calcining the dried mixture within a temperature range of from 500.degree. to 680.degree. C.;
wherein said particles are electroconductive, have a crystal structure of zinc antimonate anhydride (ZnSb.sub.2 O.sub.6), a primary particle size in a range of from 5 to 500 nm and a resistivity ranging from 0.1 K.OMEGA. to 1 M.OMEGA..

### Claim 13 (depends on 12)

A method for producing electroconductive particles as claimed in claim 12, further comprising powdering said calcined mixture to provide particles having a primary particle size in a range of from 5 to 500 nm.

### Claim 14 (depends on 12)

A method for producing electroconductive particles as claimed in claim 12, wherein said drying step is conducted at a temperature of 300.degree. C. or below.
