CN102674301A - Method for preparing strontium doped barium ferric phosphate - Google Patents
Method for preparing strontium doped barium ferric phosphate Download PDFInfo
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- CN102674301A CN102674301A CN2012101686508A CN201210168650A CN102674301A CN 102674301 A CN102674301 A CN 102674301A CN 2012101686508 A CN2012101686508 A CN 2012101686508A CN 201210168650 A CN201210168650 A CN 201210168650A CN 102674301 A CN102674301 A CN 102674301A
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- barium
- strontium
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- iron phosphate
- ferric phosphate
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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
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- 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 method for preparing strontium doped barium ferric phosphate. The chemical formula of the barium ferric phosphate is Ba(FePO4)2, and raw materials of a barium source, a ferric source and a phosphate radical source are measured based on a mole ratio of the chemical formula Ba(FePO4)2; a doped element source is calculated and added according to the weight percentage from 0.1% to 5% based on the weight of the barium ferric phosphate which can be generated in theory; and the raw materials and the doped element source are mixed, then are subjected to high-speed ball grinding for 15 to 20 hours in an ethanol medium and are dried at the temperature between 105 DEG C to 120 DEG C to obtain a precursor, and the precursor obtained by drying is placed in a high temperature furnace and is subjected to a high-temperature calcination at the temperature between 300 DEG C to 450 DEG C for 2 to 4 hours in a nitrogen atmosphere so as to obtain a product. The strontium doped barium ferric phosphate is mainly used as a reducing agent, a deoxidier, a food preservation agent, a raw material of electronic elements and batteries, an additive for smelt, alloy and glass production and the like. The barium ferric phosphate has the advantages that the raw materials are sufficient, the cost is low, the barium ferric phosphate is environment-friendly and free of pollution and the like.
Description
Technical field
Strontium doping tertiary iron phosphate 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 strontium doping tertiary iron phosphate barium.
The preparation method of strontium doping tertiary iron phosphate barium of the present invention 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 strontium doping tertiary iron phosphate 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 Preparation of Metallic Strontium, strontium hydroxide (Sr (OH) 2), Strontium carbonate powder SrCO3, etc.; It
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: strontium doping tertiary iron phosphate 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
Strontium doping tertiary iron phosphate 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 strontium doping tertiary iron phosphate 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;
One of said alloying element source: the strontium source is a Preparation of Metallic Strontium, strontium hydroxide (Sr (OH) 2), Strontium carbonate powder SrCO3, 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 alloying element source can generate the weight of tertiary iron phosphate barium by theory, calculates by 1% (weight percent) and adds the alloying element strontium, and the strontium source is Preparation of Metallic Strontium (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 strontium doping tertiary iron phosphate 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 dopant elements strontium, and the strontium source is Preparation of Metallic Strontium (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 strontium doping tertiary iron phosphate 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 strontium, and the strontium source is Preparation of Metallic Strontium (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 strontium doping tertiary iron phosphate 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 strontium, and the strontium source is strontium hydroxide (Sr (OH) 2) (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 strontium doping tertiary iron phosphate 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 strontium, and the strontium source is strontium hydroxide (Sr (OH) 2) (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 strontium doping tertiary iron phosphate 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 strontium, and the strontium source is strontium hydroxide (Sr (OH) 2) (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 strontium doping tertiary iron phosphate 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 strontium, and the strontium source is strontium hydroxide (Sr (OH) 2) (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 strontium doping tertiary iron phosphate 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 strontium, and the strontium source is Strontium carbonate powder SrCO3 (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 strontium doping tertiary iron phosphate 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 strontium, and the strontium source is Strontium carbonate powder SrCO3 (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 strontium doping tertiary iron phosphate 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 the alloying element strontium, and the strontium source is Strontium carbonate powder SrCO3 (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 strontium doping tertiary iron phosphate 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 the alloying element strontium, and the strontium source is Strontium carbonate powder SrCO3 (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 strontium doping tertiary iron phosphate 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.
Strontium doping tertiary iron phosphate 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 strontium doping tertiary iron phosphate 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; Strontium doping tertiary iron phosphate 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 a strontium doping tertiary iron phosphate 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 strontium doping tertiary iron phosphate 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 Preparation of Metallic Strontium, one of strontium hydroxide, Strontium carbonate powder.
2. the preparation method of strontium doping tertiary iron phosphate barium according to claim 1 is characterized in that: said ethanol medium is alkaline.
3. the preparation method of strontium doping tertiary iron phosphate barium according to claim 1 is characterized in that: said ethanol medium is ammoniacal liquor-alcohol mixeding liquid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101686508A CN102674301A (en) | 2012-05-28 | 2012-05-28 | Method for preparing strontium doped barium ferric phosphate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101686508A CN102674301A (en) | 2012-05-28 | 2012-05-28 | Method for preparing strontium doped barium ferric phosphate |
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| CN102674301A true CN102674301A (en) | 2012-09-19 |
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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
- 2012-05-28 CN CN2012101686508A patent/CN102674301A/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 (1)
| 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》 * |
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Application publication date: 20120919 |