CN102674299A - Preparation method of stibium doped barium ferric phosphate - Google Patents

Preparation method of stibium doped barium ferric phosphate Download PDF

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CN102674299A
CN102674299A CN2012101686480A CN201210168648A CN102674299A CN 102674299 A CN102674299 A CN 102674299A CN 2012101686480 A CN2012101686480 A CN 2012101686480A CN 201210168648 A CN201210168648 A CN 201210168648A CN 102674299 A CN102674299 A CN 102674299A
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barium
phosphoric acid
iron
source
antimony
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张健
吴润秀
王晶
张雅静
李�杰
李安平
李先兰
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李安平
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention provides a preparation method of stibium doped barium ferric phosphate. The chemical formula of barium ferric phosphate is Ba(FePO4)2, raw materials of barium sources, iron sources and phosphate sources are calculated according to the mole ratio of the chemical formula of Ba(FePO4)2, doped element sources can be calculated according to weight of the barium ferric phosphate which is possibly generated in theory, and doped elements are added according to 0.1-5% of the weight of the barium ferric phosphate; the barium ferric phosphate and the doped elements are mixed, the mixture is subjected to high-speed ball milling for 15-20 hours in ethanol media and then is dried at the temperature between 105 DEG C and 120 DEG C to obtain precursors, the precursors obtained by drying are placed into a high temperature furnace and then subjected to high-temperature calcination at the temperature between 300 DEG C and 450 DEG C for 2-4 hours in a nitrogen atmosphere, and finally products are obtained. The cobalt doped barium ferric phosphate is mainly used as a reducing agent, a deoxidizing agent and a food preservative, used as a production raw material of electronic components and batteries, and used as an additive for smelting, alloy and glass. The cobalt doped barium ferric phosphate has the advantages of being sufficient in raw materials, low in costs, environment-friendly and pollution-free.

Description

The preparation method of antimony doping phosphoric acid iron barium
Technical field
Antimony doping phosphoric acid iron barium of the present invention belongs to a kind of novel material.
Background technology
At present, still find no the report and the record of ferric phosphate barium compound.Through the retrieval of publication, investigations such as the information of internet and books and periodicals, magazine, market do not have to find the patent documentation identical with technical products of the present invention, do not see report or sale with technology of the present invention or product yet.
Summary of the invention
The objective of the invention is to: the preparation method who proposes a kind of antimony doping phosphoric acid iron barium.
The preparation method of antimony doping phosphoric acid iron barium of the present invention, it is characterized in that: its chemical formula is: Ba (FePO 4) 2, the raw material of its barium source, source of iron, phosphoric acid root is according to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 0.1-5% scope weight percent, adds alloying element; After the mixing, in ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention;
Said barium source is one of barium carbonate, hydrated barta, bariumchloride, nitrate of baryta, barium oxide, barium sulphide; Source of iron is Ferrox, ferrous chloride, iron trichloride, red stone etc.; The phosphoric acid root is: phosphoric acid, sodium phosphate salt, one of primary ammonium phosphate or Secondary ammonium phosphate;
Said alloying element source: be Antimony Trioxide: 99.5Min Sb2O3 etc.
For making each mixing of materials more even, said ethanol medium is alkaline, its alkaline ethanol liquid, and available art methods is regulated acquisition, and preferred ammoniacal liquor-alcohol mixeding liquid is good.
The present invention's beneficial effect compared with prior art: antimony doping phosphoric acid iron barium product of the present invention, mainly as reductive agent, reductor, food deoxidizing antistaling agent; Be used as the raw materials for production of raw materials for production, manufacturing cell positive material and the battery thereof of materials of electronic components or manufacturing electronic component; Be used to smelt, the additive of alloy, glass production; It is very sufficient to have raw material, at the bottom of the production cost, and characteristics such as environment friendly and pollution-free; As cell positive material, the relative barium electropotential of its charge and discharge platform is about 3.6V, and initial discharge capacity surpasses 187mAh/g, and capacity decays about 0.2% approximately after 100 charge and discharge cycles; Specific storage and cyclical stability compared with prior art are greatly improved, and the production cost price is lower more than tens of times than prior art.
Embodiment
Below in conjunction with embodiment the present invention is described further, but embodiment of the present invention is not limited thereto.
Embodiment 1
Antimony doping phosphoric acid iron barium preparation method of the present invention is characterized in that: the raw material of its barium source, source of iron, phosphoric acid root, and according to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, presses 0.1-5% scope weight percent and calculates, and adds alloying element; After the mixing, in ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus; In nitrogen atmosphere,, promptly get antimony doping phosphoric acid iron barium product of the present invention through 300-450 ℃ of high-temperature calcination 2-4h;
Said barium source is one of barium carbonate, hydrated barta, bariumchloride, nitrate of baryta, barium oxide, barium sulphide; Source of iron is Ferrox, ferrous chloride, iron trichloride, red stone etc.; The phosphoric acid root is: phosphoric acid, sodium phosphate salt, one of primary ammonium phosphate or Secondary ammonium phosphate;
Said alloying element source: be Antimony Trioxide: 99.5Min Sb2O3 etc.
For making each mixing of materials more even, said ethanol medium is alkaline, its alkaline ethanol liquid, and available art methods is regulated acquisition, and preferred ammoniacal liquor-alcohol mixeding liquid is good.
Embodiment 2
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The dopant elements source can generate the weight of tertiary iron phosphate barium by theory, calculates by 1% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in anhydrous ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.
Embodiment 3
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 0.5% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in anhydrous ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.
Embodiment 4
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 0.1% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in anhydrous ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.
Embodiment 5
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 4.5% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in anhydrous ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.
Embodiment 6
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 3% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in anhydrous ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.
Embodiment 7
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 1.5% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.
Embodiment 8
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 0.6% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.
Embodiment 9
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 2% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.
Embodiment 10
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 1% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.For making each mixing of materials more even, said ethanol medium is alkaline, its alkaline ethanol liquid, and available art methods is regulated acquisition, and preferred ammoniacal liquor-alcohol mixeding liquid is good.
Embodiment 11
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 5% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus; In nitrogen atmosphere,, promptly get antimony doping phosphoric acid iron barium product of the present invention through 300-450 ℃ of high-temperature calcination 2-4h.For making each mixing of materials more even, said ethanol medium is alkaline, its alkaline ethanol liquid, and available art methods is regulated acquisition, and preferred ammoniacal liquor-alcohol mixeding liquid is good.
Embodiment 12
Select for use: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is a raw material; According to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 0.3% (weight percent) and adds alloying element antimony, and the antimony source is Antimony Trioxide: 99.5Min Sb2O3 (98%); After the mixing, in ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention.For making each mixing of materials more even, said ethanol medium is alkaline, its alkaline ethanol liquid, and available art methods is regulated acquisition, and preferred ammoniacal liquor-alcohol mixeding liquid is good.
Antimony doping phosphoric acid iron barium product of the present invention is mainly as reductive agent, reductor, food deoxidizing antistaling agent; The raw materials for production of materials of electronic components or manufacturing electronic component, the raw materials for production of manufacturing cell positive material and battery thereof; Be used to smelt, the additive of alloy, glass production.
It has extremely strong reducing property antimony doping phosphoric acid iron barium product of the present invention, and it contacts with air, gets final product oxidation by air, becomes brown or yellow by dark color; Can be widely used in reduction, the deoxidation industry production; Because its nontoxic, water insoluble and organic solvent can generally be used for food deoxidizing antistaling agent (non-food product additive), and deixis is arranged.
As cell positive material, can be used as battery material, mainly as cell positive material; Also can be used as materials of electronic components.As cell positive material; Adopt the testing apparatus of prior art and the testing method of prior art; Antimony doping phosphoric acid iron barium product to above embodiment 1-12; Test respectively: the relative barium electropotential of its charge and discharge platform is about 3.6V, and initial discharge capacity surpasses 187mAh/g, and capacity decays about 0.2% approximately after 100 charge and discharge cycles; Specific storage and cyclical stability compared with prior art are greatly improved, and the production cost price is lower more than tens of times than prior art.
Be used to smelt, the additive of alloy, glass production; Be used for smelting, alloy production additive, but the improved products performance; The additive that is used for glass production can obtain required special glass product.

Claims (3)

1. the preparation method of an antimony doping phosphoric acid iron barium, it is characterized in that: its chemical formula is: Ba (FePO 4) 2, the raw material of its barium source, source of iron, phosphoric acid root is according to chemical formula Ba (FePO 4) 2Mol ratio metering; The alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 0.1-5% scope weight percent, adds alloying element; After the mixing, in ethanol medium, rotating speed 200-800r/mimn high speed ball milling 15-20h; With 105-120 ℃ of oven dry; Obtain presoma, the presoma that oven dry is obtained places in the High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get antimony doping phosphoric acid iron barium product of the present invention;
Said barium source is one of barium carbonate, hydrated barta, bariumchloride, nitrate of baryta, barium oxide, barium sulphide; Source of iron is Ferrox, ferrous chloride, iron trichloride, red stone etc.; The phosphoric acid root is: phosphoric acid, sodium phosphate salt, one of primary ammonium phosphate or Secondary ammonium phosphate;
Said alloying element source: be Antimony Trioxide: 99.5Min.
2. the preparation method of antimony doping phosphoric acid iron barium according to claim 1, it is characterized in that: said ethanol medium is alkaline.
3. the preparation method of antimony doping phosphoric acid iron barium according to claim 1 is characterized in that: said ethanol medium is ammoniacal liquor-alcohol mixeding liquid.
CN2012101686480A 2012-05-28 2012-05-28 Preparation method of stibium doped barium ferric phosphate Pending CN102674299A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1800000A (en) * 2004-12-31 2006-07-12 山西超新金属材料有限公司 Barium metaphosphorate production process
CN102347486A (en) * 2011-10-26 2012-02-08 吴润秀 Method for preparing barium-activated lithium iron phosphate cathode material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1800000A (en) * 2004-12-31 2006-07-12 山西超新金属材料有限公司 Barium metaphosphorate production process
CN102347486A (en) * 2011-10-26 2012-02-08 吴润秀 Method for preparing barium-activated lithium iron phosphate cathode material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
ALEXEI A. BELIK ET AL.: "Neutron powder diffraction study of the magnetic and crystal structures of SrFe2(PO4)2", 《JOURNAL OF SOLID STATE CHEMISTRY》 *
ALEXEI A. BELIK ET AL.: "SrFe2(PO4)2: Ab Initio Structure Determination with X-ray Powder Diffraction Data and Unusual Magnetic Properties", 《CHEM. MATER.》 *

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Application publication date: 20120919