CN102674308A - Preparation method of praseodymium doped iron phosphate barium - Google Patents

Preparation method of praseodymium doped iron phosphate barium Download PDF

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CN102674308A
CN102674308A CN2012101845006A CN201210184500A CN102674308A CN 102674308 A CN102674308 A CN 102674308A CN 2012101845006 A CN2012101845006 A CN 2012101845006A CN 201210184500 A CN201210184500 A CN 201210184500A CN 102674308 A CN102674308 A CN 102674308A
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barium
praseodymium
source
phosphoric acid
iron
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张健
吴润秀
王晶
张雅静
李�杰
李安平
李先兰
韦谷林
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韦谷林
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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 praseodymium doped iron phosphate barium. A chemical formula is Ba(FePO4)2, raw materials of a barium source, an iron source and a phosphate radical source are measured according to mol proportion of the chemical formula Ba(FePO4)2. A doped element source is measured according to weight of the iron phosphate barium capable of theoretically generating, and added doped elements are calculated according to the percentage by weight in the scope of 0.1-5%. After being mixed, high-speed ball-milling is carried out in an ethanol medium for 15-20h at the rotation speed of 200-800r/mimn, a precursor is obtained after stoving at 105-120 DEG C, the precursor obtained by stoving is placed in a high temperature furnace, high-temperature calcinations in the nitrogen atmosphere is carried out at 300-450 DEG C for 2-4h to obtain doped iron phosphate barium products. The praseodymium doped iron phosphate barium mainly serves as a reducing agent, a deoxidizing agent and a food deoxygenation preserving agent; serves as production materials for electronic element materials or manufacturing electronic elements and production materials for manufacturing battery positive pole materials and a battery; is used for an annexing agent of smelting, alloy and glass production; has the advantages of being sufficient in raw materials, low in production cost, environmental friendly, free of pollution and the like; and serves as the battery positive pole materials. The electric potential of a charge-discharge platform relative to a barium electrode is about 3.6V, initial discharge capacity exceed 187mAh/g, capacity after 100 times of charge and discharge reduces about 0.2%, compared with the prior art, specific capacity and cycling stability are greatly improved, and production cost is more than tens of times lower than that in the prior art.

Description

The preparation method of praseodymium doping phosphoric acid iron barium
Technical field
Praseodymium 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 praseodymium doping phosphoric acid iron barium.
The preparation method of praseodymium 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 praseodymium 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 one of praseodymium chloride, Praseodymium trioxide.
For making each mixing of materials more even; Said ethanol medium is a tart; Its acidic ethanol liquid, available art methods is regulated acquisition, and preferred organic acid-alcohol mixeding liquid is good; Said organic acid is preferably formic acid or acetate, and said acidic ethanol liquid is preferably the alcohol mixeding liquid that contains 1-5% formic acid or 1-5% acetate.
The present invention's beneficial effect compared with prior art: titanium doped tertiary iron phosphate barium product of the present invention, main 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
Praseodymium 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 praseodymium 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 one of praseodymium chloride, Praseodymium trioxide.
For making each mixing of materials more even; Said ethanol medium is a tart; Its acidic ethanol liquid, available art methods is regulated acquisition, and preferred organic acid-alcohol mixeding liquid is good; Said organic acid is preferably formic acid or acetate, and said acidic ethanol liquid is preferably the alcohol mixeding liquid that contains 1-5% formic acid or 1-5% acetate.
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 praseodymium, and the praseodymium source is praseodymium chloride (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 praseodymium 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 praseodymium, and the praseodymium source is praseodymium chloride (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 praseodymium 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 praseodymium, and the praseodymium source is praseodymium chloride (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 praseodymium 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 praseodymium, and the praseodymium source is praseodymium chloride (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 praseodymium 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 praseodymium, and the praseodymium source is praseodymium chloride (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 praseodymium 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 praseodymium, and the praseodymium source is Praseodymium trioxide (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 praseodymium 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 praseodymium, and the praseodymium source is Praseodymium trioxide (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 praseodymium 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 praseodymium, and the praseodymium source is Praseodymium trioxide (98%); After the mixing, in containing the alcohol mixeding liquid medium of 1-5% acetate, 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 praseodymium 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 praseodymium, and the praseodymium source is Praseodymium trioxide (98%); After the mixing, in containing the alcohol mixeding liquid medium of 1-5% formic acid, 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 praseodymium 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 praseodymium, and the praseodymium source is Praseodymium trioxide (98%); After the mixing, in containing the alcohol mixeding liquid medium of 1-5% formic acid, 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 praseodymium doping phosphoric acid iron barium product of the present invention.
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 praseodymium, and the praseodymium source is Praseodymium trioxide (98%); After the mixing, in containing the alcohol mixeding liquid medium of 1-5% formic acid, 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 praseodymium doping phosphoric acid iron barium product of the present invention.
Praseodymium 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 praseodymium 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; Praseodymium 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 a praseodymium 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 praseodymium 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 one of praseodymium chloride, Praseodymium trioxide.
2. the preparation method of praseodymium doping phosphoric acid iron barium according to claim 1, it is characterized in that: said ethanol medium is a tart.
3. the preparation method of praseodymium doping phosphoric acid iron barium according to claim 1 is characterized in that: said ethanol medium is the alcohol mixeding liquid that contains 1-5% formic acid or 1-5% acetate.
CN2012101845006A 2012-06-06 2012-06-06 Preparation method of praseodymium doped iron phosphate barium Pending CN102674308A (en)

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Application publication date: 20120919