CN102689891A - Method for preparing titanium doped barium iron phosphate - Google Patents
Method for preparing titanium doped barium iron phosphate Download PDFInfo
- Publication number
- CN102689891A CN102689891A CN2012101563122A CN201210156312A CN102689891A CN 102689891 A CN102689891 A CN 102689891A CN 2012101563122 A CN2012101563122 A CN 2012101563122A CN 201210156312 A CN201210156312 A CN 201210156312A CN 102689891 A CN102689891 A CN 102689891A
- Authority
- CN
- China
- Prior art keywords
- barium
- source
- iron phosphate
- titanium
- alloying element
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for preparing titanium doped barium iron phosphate which is represented as a chemical formula: Ba(FePO4)2. The method includes that raw materials of barium source, iron source and phosphate radical source are measured according to a mol (mole) ratio of the formula Ba(FePO4)2; doped element source is measured by weight percentage ranging from 0.1 to 5% according to the weight capable of generating the barium iron phosphate theoretically; after all the sources are doped, the doped sources are subjected to ball milling for 15 to 20 hours at a high speed in an ethanol medium, and then are dried at a temperature ranging from 105 DEG C to 120 DEG C to obtain a precursor; the precursor obtained from drying is disposed in a high temperature furnace, and is roasted for 2 to 4 hours at a temperature ranging from 300 DEG C to 450 DEG C at a nitrogen atmosphere to obtained a finished product. The titanium doped barium iron phosphate can be utilized for reductant, deoxidant and food preservative, or electronic element, raw battery material and additive for smelting, alloying and glass producing, and has the advantages of adequacy in raw materials, low cost, environment-friendliness, no pollution and the like.
Description
Technical field
Titanium doped 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 titanium doped tertiary iron phosphate barium.
The preparation method of titanium doped 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) metering of 2 mol ratio; 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 titanium doped 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 is: the titanium source is, is one of metatitanic acid, titanium oxide, titanium tetrachloride.
The present invention's beneficial effect compared with prior art:
Titanium doped tertiary iron phosphate 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
Titanium doped 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) metering of 2 mol ratio; 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 titanium doped 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, and one of primary ammonium phosphate or Secondary ammonium phosphate,
Said alloying element source is: the titanium source is one of metatitanic acid, titanium oxide, titanium tetrachloride.
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) metering of 2 mol ratio; 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 titanium, and the titanium source is metatitanic 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 titanium doped 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) metering of 2 mol ratio; 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 titanium, and the titanium source is metatitanic 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 titanium doped 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) metering of 2 mol ratio; 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 titanium, and the titanium source is metatitanic 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 titanium doped 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) metering of 2 mol ratio; 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 titanium, and the titanium source is metatitanic 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 titanium doped 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) metering of 2 mol ratio; 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 titanium, and the titanium source is metatitanic 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 titanium doped 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) metering of 2 mol ratio; 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 titanium, and the titanium source is a titanium oxide; 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 titanium doped 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) metering of 2 mol ratio; 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 titanium, and the titanium source is a titanium oxide; 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 titanium doped 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) metering of 2 mol ratio; 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 titanium, and the titanium source is a titanium tetrachloride; 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 titanium doped 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) metering of 2 mol ratio; 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 titanium, and the titanium source is a titanium tetrachloride; 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 titanium doped tertiary iron phosphate 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) metering of 2 mol ratio; 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 titanium, and the titanium source is a titanium tetrachloride; 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 titanium doped tertiary iron phosphate 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) metering of 2 mol ratio; 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 titanium, and the titanium source is a titanium tetrachloride; 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 titanium doped tertiary iron phosphate barium product of the present invention through 300-450 ℃ of high-temperature calcination 2-4h.
Titanium doped 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 titanium doped 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; Titanium doped 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 (1)
1. the preparation method of a titanium doped 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) metering of 2 mol ratio; 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 titanium doped 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 is: be one of metatitanic acid, titanium oxide, titanium tetrachloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101563122A CN102689891A (en) | 2012-05-18 | 2012-05-18 | Method for preparing titanium doped barium iron phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101563122A CN102689891A (en) | 2012-05-18 | 2012-05-18 | Method for preparing titanium doped barium iron phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102689891A true CN102689891A (en) | 2012-09-26 |
Family
ID=46855651
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101563122A Pending CN102689891A (en) | 2012-05-18 | 2012-05-18 | Method for preparing titanium doped barium iron phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102689891A (en) |
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 CN2012101563122A patent/CN102689891A/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.》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102689887A (en) | Method for preparing zinc doped barium iron phosphate | |
| CN102689884A (en) | Method for preparing germanium doped barium iron phosphate | |
| CN102689891A (en) | Method for preparing titanium doped barium iron phosphate | |
| CN102674290B (en) | Preparation method of neodymium-doped barium iron phosphate | |
| CN102674296B (en) | Preparation method for aluminium-doped barium iron phosphate | |
| CN102674288A (en) | Preparation method of boron-doped barium iron phosphate | |
| CN102689889A (en) | Method for preparing vanadium doped barium iron phosphate | |
| CN102701175B (en) | Preparation method of yttrium-doped barium iron phosphate | |
| CN102674306B (en) | Preparation method of lithium doped barium iron phosphate | |
| CN102689890A (en) | Method for preparing copper doped barium iron phosphate | |
| CN102701178B (en) | Preparation method of sulfur-doped barium iron phosphate | |
| CN102701179B (en) | Preparation method of Sc doped barium iron phosphate | |
| CN102689888A (en) | Method for preparing niobium-doped barium ferric phosphate | |
| CN102674293A (en) | Preparation method for calcium-doped barium iron phosphate | |
| CN102689885A (en) | Preparation method for silver doped ferric phosphate barium | |
| CN102674304A (en) | Preparation method for molybdenum-doped barium iron phosphate | |
| CN102674295A (en) | Preparation method of magnesium doped iron barium phosphate | |
| CN102674299A (en) | Preparation method of stibium doped barium ferric phosphate | |
| CN102674289A (en) | Preparation method of nickel-doped barium iron phosphate | |
| CN102674302A (en) | Method for preparing zirconium doped barium iron phosphate | |
| CN102689886A (en) | Method for preparing tin-doped barium iron phosphate | |
| CN102701177A (en) | Preparation method of dysprosium doping Ba(FePO4)2 (iron barium phosphate) | |
| CN102701176A (en) | Preparation method for terbium-doped barium iron phosphate | |
| CN102730660A (en) | Preparation method of europium doped barium iron phosphate | |
| CN102674294A (en) | Method for preparing bismuth-doped ferric barium phosphate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120926 |