CN102701175B - Preparation method of yttrium-doped barium iron phosphate - Google Patents

Preparation method of yttrium-doped barium iron phosphate Download PDF

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CN102701175B
CN102701175B CN201210156321.1A CN201210156321A CN102701175B CN 102701175 B CN102701175 B CN 102701175B CN 201210156321 A CN201210156321 A CN 201210156321A CN 102701175 B CN102701175 B CN 102701175B
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barium
yttrium
source
phosphoric acid
iron
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CN102701175A (en
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张健
吴润秀
王晶
张雅静
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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 preparation method of yttrium-doped barium iron phosphate which has a chemical formula of Ba(FePO4)2. The preparation method comprises the steps of: metering raw materials of a barium source, an iron source and a phosphate radical source according to the mol ratio in the chemical formula Ba(FePO4); adding a doping element from a doping element source at a amount of 0.1-5% the weight of barium iron phosphate generated in theory; and mixing, carrying out high-speed ball milling in ethanol medium for 15-20 h, baking at 105-120 DEG C to obtain a precursor, placing the baked precursor in a high-temperature furnace, and carrying out high-temperature calcination at 300-450 DEG C in nitrogen atmosphere to obtain the product. The obtained product is mainly used as a reducing agent, a deoxidizer and a food preservative, a raw material for electronic components and a battery, an additive for smelting, and alloy and glass production and the like, and has the characteristics of sufficient raw materials, low cost, environmental friendliness, no pollution and the like.

Description

The preparation method of yttrium doping phosphoric acid iron barium
Technical field
Yttrium 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 yttrium doping phosphoric acid iron barium.
The preparation method of yttrium 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, calculate by 0.1-5% scope weight percent, adds doped element; After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 Yttrium trichloride, yttrium oxide.
The present invention's beneficial effect compared with prior art:
Yttrium 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 exceedes 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
Yttrium 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, calculate by 0.1-5% scope weight percent, adds doped element; After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 Yttrium trichloride, yttrium oxide.
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 yttrium, yttrium source is Yttrium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 yttrium, yttrium source is Yttrium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 yttrium, yttrium source is Yttrium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 yttrium, yttrium source is Yttrium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 yttrium, yttrium source is Yttrium trichloride (98%); After mixing, in anhydrous ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 yttrium, yttrium source is Yttrium trichloride (98%); After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 yttrium, yttrium source is yttrium oxide (98%); After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 yttrium, yttrium source is yttrium oxide (98%); After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 dopant elements yttrium, yttrium source is yttrium oxide (98%); After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 yttrium, yttrium source is yttrium oxide (98%); After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium 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 yttrium, yttrium source is yttrium oxide (98%); After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium doping phosphoric acid iron barium product of the present invention.
Yttrium 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 yttrium 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 from dark color; 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, to the yttrium doping phosphoric acid iron barium product of 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 exceedes 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; For the additive of glass production, can obtain required special glass product.

Claims (1)

1. a preparation method for yttrium 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, calculate by 0.1-5% scope weight percent, adds doped element; After mixing, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C 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 DEG C of high-temperature calcination 2-4h, obtain yttrium doping phosphoric acid iron barium product of the present invention;
Described doped element source: be one of Yttrium trichloride, yttrium oxide.
CN201210156321.1A 2012-05-18 2012-05-18 Preparation method of yttrium-doped barium iron phosphate Expired - Fee Related CN102701175B (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系统公司 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系统公司 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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