CN102689888A - Method for preparing niobium-doped barium ferric phosphate - Google Patents
Method for preparing niobium-doped barium ferric phosphate Download PDFInfo
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- CN102689888A CN102689888A CN2012101554763A CN201210155476A CN102689888A CN 102689888 A CN102689888 A CN 102689888A CN 2012101554763 A CN2012101554763 A CN 2012101554763A CN 201210155476 A CN201210155476 A CN 201210155476A CN 102689888 A CN102689888 A CN 102689888A
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- barium
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- niobium
- phosphoric acid
- iron
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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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a method for preparing niobium-doped barium ferric phosphate having a chemical formula Ba (FePO4)2. The method comprises: weighting raw materials of a barium source, a ferric source and a phosphate radical source in terms of the mol percent of the elements in the chemical formula Ba (FePO4)2; weighting a doped element source according to a weight of barium ferric phosphate generated in theory and adding the doped element according to a weight percentage in a range of 0.1-5%; after mixing the resources above, ball milling a mixture at a high speed for 15-20 hours in an ethanol medium; drying the mixture at 105-120 DEG C to obtain a precursor; placing the precursor obtained from drying in a high temperature furnace; calcining the precursor at a high temperature of 300-450 DEG C in a nitrogen atmosphere for 2-4 hours to get a product. The product can be used as reductant, deoxidizer, antistaling agent of foodstuff, raw materials of an electronic component and a battery, additive of smelting, alloy and glass production etc., and is advantaged by sufficient raw material, low cost, environmental protection with no pollution, etc.
Description
Technical field
Niobium 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 niobium doping phosphoric acid iron barium.
Another object of the present invention is to: the purposes that proposes a kind of tertiary iron phosphate barium product.
The preparation method of niobium 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, by 0.1-5% scope weight percent, 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; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get niobium 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 sodium columbate (NaNbO3) niobic acid NbO3, Niobium Pentxoxide (Nb2O5) etc.
The present invention's beneficial effect compared with prior art:
Niobium doping phosphoric acid iron barium product of the present invention is 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
Niobium 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, 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 niobium 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 sodium columbate (NaNbO3) niobic acid NbO3, Niobium Pentxoxide (Nb2O5) etc.
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 alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 1% (weight percent) and adds the alloying element niobium, and the niobium source is sodium columbate (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 niobium 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 the alloying element niobium, and the niobium source is sodium columbate (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 niobium 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 the alloying element niobium, and the niobium source is sodium columbate (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 niobium 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 the alloying element niobium, and the niobium source is niobic acid (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 niobium 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 the alloying element niobium, and the niobium source is niobic acid (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 24h, promptly get niobium 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 the alloying element niobium, and the niobium source is niobic acid (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 niobium 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 the alloying element niobium, and the niobium source is niobic acid (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 niobium 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 the alloying element niobium, and the niobium source is a Niobium Pentxoxide (Nb2O5) (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 niobium 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 the alloying element niobium, and the niobium source is a Niobium Pentxoxide (Nb2O5) (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 niobium doping phosphoric acid iron barium product of the present invention.
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 the alloying element niobium, and the niobium source is a Niobium Pentxoxide (Nb2O5) (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 niobium doping phosphoric acid iron barium product of the present invention through 300-450 ℃ of high-temperature calcination 2-4h.
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 the alloying element niobium, and the niobium source is a Niobium Pentxoxide (Nb2O5) (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 niobium doping phosphoric acid iron barium product of the present invention.
Niobium 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 niobium 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; Niobium 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 (1)
1. the preparation method of a niobium 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, by 0.1-5% scope weight percent, 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; Through 300-450 ℃ of high-temperature calcination 2-4h, promptly get niobium 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 is: be sodium columbate, niobic acid, one of Niobium Pentxoxide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101554763A CN102689888A (en) | 2012-05-18 | 2012-05-18 | Method for preparing niobium-doped barium ferric phosphate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101554763A CN102689888A (en) | 2012-05-18 | 2012-05-18 | Method for preparing niobium-doped barium ferric phosphate |
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| CN2012101554763A Pending CN102689888A (en) | 2012-05-18 | 2012-05-18 | Method for preparing niobium-doped barium ferric phosphate |
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Citations (2)
| 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 |
-
2012
- 2012-05-18 CN CN2012101554763A patent/CN102689888A/en active Pending
Patent Citations (2)
| 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)
| 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: 20120926 |