CN102701179B - Preparation method of Sc doped barium iron phosphate - Google Patents

Preparation method of Sc doped barium iron phosphate Download PDF

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CN102701179B
CN102701179B CN201210184498.2A CN201210184498A CN102701179B CN 102701179 B CN102701179 B CN 102701179B CN 201210184498 A CN201210184498 A CN 201210184498A CN 102701179 B CN102701179 B CN 102701179B
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barium
source
phosphoric acid
scandium
iron phosphate
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CN102701179A (en
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张健
吴润秀
王晶
张雅静
李�杰
李安平
李先兰
曾令城
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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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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention provides a preparation method of Sc doped barium iron phosphate. The chemical formula of barium iron phosphate is Ba(FePO4)2, raw materials of the barium source, the iron source and the phosphate source are metered according to the mol proportion of the chemical formula Ba(FePO4)2, an element source is doped, and the added doped element is metered according the weight of barium iron phosphate generated in theory and the weight percent within the 0.1 to 5% range; after the sources are mixed, is ball-ground for 15 to 20 hours in an ethanol medium at a high speed, and dried at the temperature of 105 to 120 DEG C to obtain a precursor; the precursor obtained through drying is put in a high-temperature furnace, is calcinated for 2 to 4 hours at a high temperature of 300 to 450 DEG C under the nitrogen atmosphere to obtain the Sc doped barium iron phosphate, the Sc doped barium iron phosphate is used as a reducing and deoxidizing agent, a food fresh-keeping agent, a battery raw material, metallurgy, alloy and glass production additives and the like, and has the characteristics of abundant raw material, low cost, environmental protection, no pollution and the like.

Description

The preparation method of scandium doping phosphoric acid iron barium
Technical field
Scandium doping phosphoric acid iron barium of the present invention, belongs to a kind of novel material.
Background technology
At present, not yet find that there is report and the record of tertiary iron phosphate barium compound.Through the retrieval of publication, the 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, have no report or sale with technology of the present invention or product yet.
Summary of the invention
The object of the invention is to: the preparation method who proposes a kind of scandium doping phosphoric acid iron barium.
The preparation method of scandium doping phosphoric acid iron 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, according to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium by theory, by 0.1-5% scope weight percent, calculate, and adds doped element; After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention;
Described 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, ferric oxide etc.; Phosphoric acid root is: phosphoric acid, sodium phosphate salt, one of primary ammonium phosphate or Secondary ammonium phosphate;
Described doped element source: be one of Scium trichloride, Scium trioxide.
For making each mixing of materials more even, described ethanol medium is acid, its acidic ethanol liquid, available art methods regulates acquisition, preferably organic acid-alcohol mixeding liquid is good, described organic acid is preferably formic acid or acetic acid, and described acidic ethanol liquid is preferably the alcohol mixeding liquid containing 1-5% formic acid or 1-5% acetic acid.
The present invention's beneficial effect compared with prior art: scandium 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, manufacture cell positive material and the battery thereof of materials of electronic components or manufacture electronic component; For smelting, the additive of alloy, glass production; There is raw material very sufficient, at the bottom of production cost, the feature such as environment friendly and pollution-free; As cell positive material, the relative barium electropotential of its charge and discharge platform is 3.6V left and right, and initial discharge capacity surpasses 187mAh/g, capacity 0.2% left and right of approximately decaying after 100 charge and discharge cycles; Specific storage and cyclical stability compared with prior art, are greatly improved, and production cost price is than more than the low decades of times of prior art.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but embodiments of the present invention are not limited to this.
Embodiment 1
Scandium 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; Doped element source, can generate the weighing scale of tertiary iron phosphate barium by theory, by 0.1-5% scope weight percent, calculate, and adds doped element; After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention;
Described 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, ferric oxide etc.; Phosphoric acid root is: phosphoric acid, sodium phosphate salt, one of primary ammonium phosphate or Secondary ammonium phosphate;
Described doped element source: be one of Scium trichloride, Scium trioxide.
For making each mixing of materials more even, described ethanol medium is acid, its acidic ethanol liquid, available art methods regulates acquisition, preferably organic acid-alcohol mixeding liquid is good, described organic acid is preferably formic acid or acetic acid, and described acidic ethanol liquid is preferably the alcohol mixeding liquid containing 1-5% formic acid or 1-5% acetic acid.
Embodiment 2
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 1%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Embodiment 3
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 0.5%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Embodiment 4
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 0.1%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Embodiment 5
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 4.5%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain doping phosphoric acid iron barium product of the present invention.
Embodiment 6
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 3%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Embodiment 7
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 1.5%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trichloride (98%); After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Embodiment 8
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 0.6%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trioxide (98%); After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Embodiment 9
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 2%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trioxide (98%); After mixing, in containing the alcohol mixeding liquid medium of 1-5% acetic acid, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Embodiment 10
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 1%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trioxide (98%); After mixing, in containing the alcohol mixeding liquid medium of 1-5% formic acid, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Embodiment 11
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 5%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trioxide (98%); After mixing, in containing the alcohol mixeding liquid medium of 1-5% formic acid, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Embodiment 12
Select: barium carbonate (BaCO3) (99.8%), Ferrox (FeC2O4.2H2O) (99.06%), Secondary ammonium phosphate (NH4H2PO4) (98%) is raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium, by 0.3%(weight percent by theory) to calculate and add doped element scandium, scandium source is Scium trioxide (98%); After mixing, in containing the alcohol mixeding liquid medium of 1-5% formic acid, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention.
Scandium doping phosphoric acid iron barium product of the present invention, mainly as reductive agent, reductor, food deoxidizing antistaling agent; The raw materials for production of materials of electronic components or manufacture electronic component, the raw materials for production of manufacture cell positive material and battery thereof; For smelting, the additive of alloy, glass production.
It has extremely strong reducing property scandium doping phosphoric acid iron barium product of the present invention, and it contacts with air, gets final product oxidation by air, from dark color, becomes brown or yellow; Can be widely used in reduction, deoxidation industry production; Because it is nontoxic, water insoluble and organic solvent, can be general for food deoxidizing antistaling agent (non-food product additive), and have deixis.
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, scandium doping phosphoric acid iron barium product to above embodiment 1-12, test respectively: the relative barium electropotential of its charge and discharge platform is 3.6V left and right, initial discharge capacity surpasses 187mAh/g, capacity 0.2% left and right of approximately decaying after 100 charge and discharge cycles; Specific storage and cyclical stability compared with prior art, are greatly improved, and production cost price is than more than the low decades of times of prior art.
For smelting, the additive of alloy, glass production; For smelting, alloy production additive, can improved products performance; Additive for glass production, can obtain required special glass product.

Claims (3)

1. a preparation method for scandium doping phosphoric acid iron barium, its chemical formula is: Ba (FePO 4) 2, it is characterized in that: the raw material of its barium source, source of iron, phosphoric acid root, select: barium carbonate (BaCO 3), Ferrox (FeC 2o 4.2H 2o), Secondary ammonium phosphate (NH 4h 2pO 4) be raw material; According to chemical formula Ba (FePO 4) 2mol ratio metering; Doped element source, can generate the weighing scale of tertiary iron phosphate barium by theory, by 0.1-5% scope weight percent, calculate, and adds doped element; After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 ℃ of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in High Temperature Furnaces Heating Apparatus, in nitrogen atmosphere, through 300-450 ℃ of high-temperature calcination 2-4h, obtain scandium doping phosphoric acid iron barium product of the present invention;
Described doped element source: be one of Scium trichloride, Scium trioxide.
2. the preparation method of scandium doping phosphoric acid iron barium according to claim 1, is characterized in that: described ethanol medium is acid.
3. the preparation method of scandium doping phosphoric acid iron barium according to claim 1, is characterized in that: described ethanol medium is the alcohol mixeding liquid containing 1-5% formic acid or 1-5% acetic acid.
CN201210184498.2A 2012-06-06 2012-06-06 Preparation method of Sc doped barium iron phosphate Expired - Fee Related CN102701179B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1754275A (en) * 2002-12-23 2006-03-29 A123***公司 High energy and power density electrochemical cells
CN1772604A (en) * 2005-10-11 2006-05-17 清华大学 Prepn process of oxygen place doped lithium ferric phosphate powder
CN1785823A (en) * 2005-12-23 2006-06-14 清华大学 Preparation method of phosphorus position partly substituted iron lithium phosphate powder
CN101339994A (en) * 2008-09-01 2009-01-07 罗绍华 Preparation of multi-position doped lithium iron phosphate positive electrode material and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1754275A (en) * 2002-12-23 2006-03-29 A123***公司 High energy and power density electrochemical cells
CN1772604A (en) * 2005-10-11 2006-05-17 清华大学 Prepn process of oxygen place doped lithium ferric phosphate powder
CN1785823A (en) * 2005-12-23 2006-06-14 清华大学 Preparation method of phosphorus position partly substituted iron lithium phosphate powder
CN101339994A (en) * 2008-09-01 2009-01-07 罗绍华 Preparation of multi-position doped lithium iron phosphate positive electrode material and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Alexei A. Belilk etal.Neutron powder diffraction study of the magnetic and crystal structures of SrFe2(PO4)2.《Journal of Solid State Chmistry》.2008, *
Neutron powder diffraction study of the magnetic and crystal structures of SrFe2(PO4)2;Alexei A. Belilk etal;《Journal of Solid State Chmistry》;20080528;参见第2292页左栏第2段至第2293页右栏第4段 *

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